EPA/540/2-89/049
      SUPERFUNDTREATABILITY
             CLEARINGHOUSE
                Document Reference:
EBASCO Services inc. "Litigation Technical Support and Services, Rocky Mountain
Arsenal (Basis F Wastes)." Six-part technical report with a total of approximately 600
 pp. prepared for U.S. Army Program Manager's Office for Rocky Mountain Arsenal
   Cleanup during April and September 1986 and March, April, and May 1987.
              EPA LIBRARY NUMBER:

            Superfund Treatability Clearinghouse - FDBP

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                SUPERFUND TREATABILITY CLEARINGHOUSE ABSTRACT
 Treatment Process:

 Media:

 Document Reference:
 Document  Type:

 Contact:
Thermal Treatment - Incineration

Soil/Generic

EBASCO Services Inc.  "Litigation Technical Support
and Services, Rocky Mountain Arsenal (Basis F
Wastes)."  Six-part technical report with a total
of approximately 600 pp. prepared for U.S. Army
Program Manager's Office for Rocky Mountain Arsenal
Cleanup during April and September 1986 and March,
April, and May 1987.

Contractor/Vendor Treatability Study
Bruce Huenfeld
U.S. DOD/USATHAMA
Aberdeen Proving Ground,
301-617-3446
                                                 MD   21010-5401
 Site  Name:
 Location  of  Test:
Rocky Mountain Arsenal,  CO (NPL - Federal facility)

Rocky Mountain, CO
BACKGROUND;  This  report  consists of 5 documents which cover  incineration
tests at  the Rocky Mountain Arsenal (RMA), Denver, CO, ranging  from a  labor-
atory test plan and  bench-scale  test to  full-scale testing.   This abstract
reports only on the  results of bench-scale incineration  tests of contaminants
from Basin F of the  RMA.   Objectives of  the study were to:  1)  Gather  infor-
mation on properties of the wastes, 2) provide a bench-scale  apparatus to
determine incinerability  characteristics of the wastes,  3) demonstrate 99.99%
destruction removal  efficiency (DRE), and 4) determine gas residence time,
temperature and excess 0«  necessary for  99.99% DRE.
OPERATIONAL INFORMATION;   The types of waste discharged  into  the Basin F
lagoon included sodium salts of  chloride, fluoride, hydroxide,  methyl
phosphate, acetate,  sulfate and  pesticides.
    Bench-scale tests were conducted on  pure compounds and field samples.   The
technical approach involved using equipment to simulate  three of the major
incineration mechanisms—pyrolysis, primary incinerator  postflame, and
afterburner postflame.
    The laboratory bench-scale unit was  designed to evaluate  thermal destruc-
tion efficiency up to 1200 F and residence times from 2  to 5 seconds.  The
unit utilized a batch load system with two furnaces and a blended carrier gas.
The first furnace  volatilized the constituents while the carrier gas moved  the
constituents to the  secondary furnace which added ()„ and simulated an  after-
burner in a full-scale unit.
    Residence times  in the afterburner were 1 second or  5 seconds.  Residence
time in the primary  burner was one hour.  Temperature parameters for the pri-
mary and secondary chambers were based on the current limitations of
operational practices for waste  incineration.  Primary burner operating tem-
peratures were 650°, 800° and 900o C.   Secondary afterburner  operating
3/89-22                                              Document Number:   FDBP

   NOTE:  Quality assurance of data nay not be appropriate for all uses.

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 temperatures were 650°, 900° and 1200° C.
            0« concentrations were 5%  to 7%.
 Sixteen successful runs were performed.
      The combustion products in the gases were collected by a sampling train
 for subsequent analysis.  A detailed sampling plan is contained in this study.
 An outline of QA/QC measures that will be taken are reported in the "Draft
 Laboratory Test Plan for Incineration of Basin F Wastes  at  Rocky Mountain
 Arsenal, April 1986."  Samples for analysis were collected  from soils,  sludge
 and liquid.  GC/MS was employed to analyze for ten semivolatile compounds in
 the feed stock.  GS/MS selective ion monitoring was used for contaminant
 residue and off gas analysis.
 PERFORMANCE:  In all but a few instances, a 99.99% ORE was  demonstrated for
 the ten principal hazardous organic constituents.   Residues were tested for EP
 Toxicity to determine the leachability of heavy metals contained in the
 Basin F wastes.  No heavy metals exceeded the EP Toxicity limit.   In summary,
 Basin F wastes are incinerable and ORE levels were 99.99% under almost  all the
 conditions investigated.
 CONTAMINANTS;

 Analytical data is provided in the treatability
 of the contaminants by treatability group  is:
 Treatability Group

 WOl-Halogenated  Non-Polar
      Aromatic Compounds
 V03-Halogenated  Phenols
      Cresols and Thiols
WOA-Halogenated Aliphatic
     Solvents
W05-Halogenated Cyclic
     Aliphatics/Ethers/
     Esters/Ketones

W07-Hetercyclics and Simple
     Aromatics
W09-0ther Polar Organic
     Compounds

W13-0ther Organics
CAS Number

108-90-7


CPMS

CPMS02

CPMSO

470-90-6

96-12-8


309-00-2
72-20-8
465-73-6
60-57-1

108-88-3
1330-20-7
ABC

109-92-2
110-71-4
T119-36-8

142-82-5
77-73-6
                 study report.  The breakdown
Contaminants

Chlorobenzene

P-Chlorophenylme thyl
 Sulfide
P-Chlorophenylme thyl
 Sulfone
P-Chlorophenylmethyl
 Sulfoxide
Supona
1,2-Dibromo-3-chloropropane

Aldrin
Endrin
Isodrin
Dieldrin
Toluene
Xylenes
Alkyl Benzene
Ethoxyethylene
Dimethoxyethane
Benzoic Acid
Heptane
Dicyclopentadiene
Note:  This is a partial listing of data.  Refer to  the document  for  more
       information.
3/89-22                                              Document Number:   FDBP

   NOTE:  Quality assurance of data nay not be appropriate  for all  uses.

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                                                               TABLE  1
                                                    REMOVAL EFFICIOKT OF TKM PKIBKriPAL HAZARDOUS
                                                    C COKSn^RJKRS  Mt OWKMHUMO
Tanp Degrees C in
Secondary Burner

Teap Degrees C in
Primary Burner

Gas Residence Ti»e
in Second Burner
(in seconds)

Oxygen Level in
off-gas (%)
                    650     650
                    6SO
                            699
                                    650
                                    650
                                            900     900     900      900      900      900      900      1200    1200    1200    1200
                                            650     800     800      900      900      900
                                                                                             900
                                                                                                      650     900     900     900
                     5.4
                                            5.4
                                                                     5.4
                                                                                     5.4
                                                                                                      5.4     5.4
Run Rumbtc
14 11 6
17
18 20 18 12 3 9 7 8 10 2
13
5

ALDRIN
CPUS
CPMSO
CPMSO2
DBCP
DIELDRIN
ENDRIN
ISODRIN
SUPONA
100
100
100
100
100
100
100
100
99
100
100
100
100
100
100
100
99
100
.00 100.00 100.00
.00
.00 100.00 100.00
.00
.00 100.00 100.00
.00
.00 100.00 100.00
.00
.00 100.00 100.00
.00
.00 100.00 100.00
.00
.00 100.00 100.00
.00
.00 100.00 100.00
.00
.74 99.38 100.00
.00
100.00 100.00 100.00 100.00 99.94 100.00 100.00 100.00 100
100
100.00 100.00 100.00 100.00 99.99 100.00 100.00 100.00 100
100
100.00 100.00 100.00 100.00 99.41 100.00 100.00 100.00 100
100
100.00 99.99 100.00 100.00 100.00 100.00 100.00 100.00 100
100
100.00 100.00 100.00 100.00 100.00 100.00 100.00 100.00 100
100
100.00 100.00 100.00 100.00 99.97 100.00 100.00 100.00 100
100
100.00 100.00 100.00 100.00 100.00 100.00 100.00 100.00 100
100
100.00 100.00 100.00 100.00 99.99 100.00 100.00 100.00 100
100
100.00 100.00 100.00 100.00 100.00 100.00 100.00 100.00 100
, 100
.00 100.00
.00
.00 100.00
.00
.00 100.00
.00
.00 100.00
.00
.00 100.00
.00
.00 100.00
.00
.00 100.00
.00
.00 100.00
.00
.00 100.00
.00
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
3/89-22
                                                                                                         Document Number:  FDBP
                            ROTE:  Quality assurance  of  data  «ay not be appropriate for all uses.

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                                                              '  KT-
                                    DRAFT
                      BENCH-SCALE LABORATORY INCINERATION
                                      OF
                                BASIN F WASTES
                            ROCKY MOUNTAIN ARSENAL
                                   MAY 1987
                                 TASK  NO.  17
                         CONTRACT NO. DAAK11-84-D-0017
THE VIEWS,  OPINIONS,  AND/OR FINDINGS CONTAINED  IN  THIS REPORT ARE THOSE  OF
THE AUTHOR(S) AND  SHOULD  NOT BE CONSTRUED AS AN OFFICIAL  DEPARTMENT  OF ARMY
POSITION, POLICY, OR DECISIONS, UNLESS SO DESIGNATED BY OTHER DOCUMENTATION.
THE  USE OF TRADE  NAMES   IN THIS  REPORT DOES  NOT  CONSTITUTE  AN OFFICIAL
ENDORSEMENT OR APPROVAL OF THE USE  OF SUCH COMMERCIAL PRODUCTS.   THIS REPORT
MAY NOT BE CITED FOR PURPOSES OF ADVERTISEMENT.
2306E

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                      BENCH-SCALE LABORATORY INCINERATION
                                      OF
                                BASIN F WASTES
                                                                    PAGE
 1.0   INTRODUCTION                                                    1-1
      1.1  PURPOSE                                                    1-1
      1.2  STUDY CONSTRAINTS                                          1-2
      1.3  STUDY APPROACH                                             1-2

 2.0   CHARACTERISTICS OF BASIN F WASTES                               2-1
      2.1  INTRODUCTION                                               2-1
      2.2  BACKGROUND                                                 2-1
          2.2.1  Basin F History                                     2-1
          2.2.2  Basin F Waste Characteristics                       2-2
      2.3  SAMPLING                                                   2-4
      2.4  LABORATORY ANALYSIS                                        2-4
          2.4.1  Objectives                                          2-4
          2.4.2  Analytical Parameters and Methods                   2-5
          2.4.3  Basin F Liquid                                      2-5
          2.4.4  Basin F Overburden                                  2-6

3.0   BENCH-SCALE INCINERATION SYSTEM                                 3-1
      3.1  RATIONAL FOR A BENCH-SCALE SYSTEM                          3-1
      3.2  SYSTEM DESCRIPTION                                         3-1
          3.2.1  Primary Furnace                                     3-2
          3.2.2  Fly Ash Trap                                        3-2
          3.2.3  Secondary Combustor Gas                             3-2
          3.2.4  Secondary Furnace                                   3-2
          3.2.5  Cooling Section                                     3-3
          3.2.6  Sample Collection                                   3-3
     3.3  SAMPLING                                                   3-3
          3.3.1  Introduction                                        3-3
          3.3.2  Particulate and Residue Collection                  3-4
     3.4  OPERATING PROCEDURES                                       3-5
          3.4.1  Soil Tests                                          3-5
77C16F

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                              TABLE OF CONTENTS
                                 (continued)
                                                                  PAGE

4.0  BENCH-SCALE INCINERATION TEST CONDITIONS                     4-1
     4.1   SELECTED VARIABLES                                     4-1
           4.1.1  Time Parameters                                 4-1
           4.1.2  Temperature Parameters                          4-1
           4.1.3  Oxygen Concentration                            4-3
     4.2   ANALYTICAL PARAMETERS MONITORED                        4-3

5.0  TEST RESULTS                                                  5-1
     5.1   SUMMARY                                                 5-1
     5.2   FEED SAMPLE ANALYSES                                    5-1
     5.3   RESIDUE ANALYSES                                        5-2
     5.4   OFF-GAS ANALYSES                                        5-2
     5.5   DETERMINATION OF ORE                                    5-3
     5.6   ANALYSIS OF COMBUSTION RESULTS                          5-4
     5.7   ANALYSIS OF PRODUCTS OF INCOMPLETE COMBUSTION           5-8
     5.8   DETERMINATION OF OPTIMUM COMBUSTION CONDITIONS          5-14
     5.9   OPTIMIZATION RUNS                                       5-15
     5.10  EP TOXICITY OF RESIDUE                                  5-15
     5.11  LIQUID TEST BURN RESULTS                                5-15

6.0  SUMMARY AND CONCLUSIONS                                       6-1

APPENDICES
     APPENDIX A   ANALYTICAL RESULTS OF FEED, RESIDUE AND OFF-GAS SAMPLES
     APPENDIX B   CHEMICAL  STRUCTURES  OF  22 SEMI-VOLATILE  ORGANIC  TARGET
                  COMPOUNDS
     APPENDIX C   CHEMICAL STRUCTURES OF IDENTIFIED PRODUCTS OF INCOMPLETE
                  COMBUSTION IN OFF-GASES FROM RUN NOS. 12, 13 AND 14
     APPENDIX D   REFERENCES
                                      ii

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                                LIST  OF  FIGURES
Figure 2.2-1
Figure 2.2-2
Location of Boring Sites Within Basin F
Contaminants Identified in the SWLP
  Extracts of the Soils in Basin F
                                                                   Following
                                                                      Page
2-2

2-3
Figure 3.2-1
Figure 3.2-2
Figure 3.2-3
Figure 3.3-1
Figure 3.3-2
Figure 3.3-3
Laboratory Scale Incineration Unit                      3-1
Rotating Tube Furnace Arrangement                       3-2
Rotating Tube Unit                                      3-2
Sampling Train                                          3-4
Solid Residue Collection Flow Chart                     3-4
Modified Sampling Train for High Moisture Samples       3-5
Figure 4.1-1   Exhaust CO and Total Hydrocarbons and Fraction
                 of Test Compound Remaining in Exhaust as a
                 Function of Theoretical Air
                                                        4-3
Figure 5.7.1

Figure 5.7-2

Figure 5.7-3

Figure 5.8-1
Figure 5.8-2
Figure 5.8-3
Figure 5.9-1

Figure 5.9-2
Reconstructed Ion Chromatograph for Products of
  Incompete Combustion in Off-Gases of Run No. 12       5-9
Reconstructed Ion Chromatograph for Products of
  Incomplete Combustion if Off-Gases of Run No. 13      5-9
Reconstructed Ion Chromatograph for Products of
  Incomplete Combustion if Off-Gases of Run No. 14      5-9
Concentration of CO in Off-Gases of Run No. 12         5-14
Concentration of CO in Off-Gases of Run No. 13         5-14
Concentration of CO in Off-Gases of Run No. 14         5-14
Reconstructed Ion Chromatograph for Products of
  Incompete Combustion in Off-Gases of the
  Optimization Run No. 1                               5-15
Reconstructed Ion Chromatograph for Products of
  Incompete Combustion in Off-Gases of the
  Optimization Run No. 2                               5-15
                                      iii

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                                LIST OF TABLES
 Table  2.2-1
 Table  2.2-2

 Table  2.4-1
 Table  2.4-2
 Table  2.4-3
 Table  2.4-4
Chemical Characterization of Basin F Liquid
Concentrations of Contaminants in Soil
  Samples Underlying Basin F Liner
Summary of Laboratory Analyses
Physical, Chemical, and Thermodynamic Test
  Results of Basin F Liquid and Overburden
Analytical Results of Basin F Liquid Sample
Analytical Results of the Overburden Sample
Table 3.3-1    Gas Sample Collection Matrix
                                                                   Following
                                                                      Page
2-2

2-4
2-5

2-5
2-5
2-6

3-5
Table 5.1-1
Table 5.2-1
Table 5.3-1
Table 5.4-1
Table 5.5-1

Table 5.7-1

Table 5.7-2

Table 5.7-3

Table 5.7-4

Table 5.9-1
Test Matrix
Feed Sample
Residue Analyses
Contaminants Remaining in Off-Gases
Destruction and Removal Efficiency of
  Principal Organic Hazardous Constituents
Library Search Results of Products of
  Incomplete Combustion in Off-Gas Sample
  From Run No. 12
Library Search Results of Products of
  Incomplete Combustion in Off-Gas Sample
  from Run No. 13
Library Search Results of Products of
  Incomplete Combustion in Off-Gas Sample
  from Run No. 14
Summary of Observed Toxic Products
  of Incomplete Combustion
Summary of Identified Products of Incomplete
  Combustion in Off-Gas Samples of
  Two Optimization Runs
Table 5.10-1   EP Toxicity Results
5-1
5-1
5-2
5-2

5-4

5-9

5-9

5-9

5-9

5-15
5-15
                                      iv

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                              TEXT ABBREVIATIONS
A        Frequency Factor
°C       Degree Celsius
DRE      Destruction and Removal Efficiency
E        Activation Energy
EP       Extraction Procedure
FID      Flame lonization Detector
GC-MS    Gas Chromatography - Mass Spectrometry
MM5      Modified Method 5
PCT      Physical, Chemical and Thermodynamic
PIC      Products of Incomplete Combustion
PMO      Program  Manager's Office  for Rocky Mountain  Arsenal Contamination
         Cleanup
POHCs  :  Principal Organic Hazardous Constituents
RCRA   :  Resource Conservation and Recovery Act
SIM    :  Selective Ion Monitoring
SWLP   :  Solid Waste Leaching Procedures
T      :  Temperature
cm
ft
gm
kcal
kg
1
Ib
mg
mm
ppb
ppm
s
fr
ug
centimeter
foot or feet
gram
Kilocalorie
kilogram
liter
pound
milligram
millimeter
parts per billion
parts per million
second
gas residence time
microgram

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                             CHEMICAL ABBREVIATIONS
 Ag
 As
 Ba
 BCHO
 Ca
 Cd
 CHClj
 co2
 COD
 CPMS
 CPMSO
 CPMSO,
      A
 Cr
 Cu
 DBCP
 DCPD
 DOE
 DDT
 DIMP
 DMDS
 DMMP
 H
 H20
 HBr
 HCB
 HC1
 HCCPD
 Hg
 K
 Mg
MIBK
N2
Na
 Silver
 Arsenic
 Barium
 Bicycloheptadiene
 Calcium
 Cadmium
 Chloroform
 Carbon Dioxide
 Chemical  Oxygen  Demand
 P-Chlorophenylmethyl Sulfide
 P-Chlorophenylmethyl Sulfoxide
 P-Chlorophenylmethyl Sulfone
 Chromium
 Copper
 Nemagon (Dibromo Chloropropane)
 Dicyclopentadiene
 l,l-dichloro-2,  2-bis-(p-chlorophenyl) ethylene
 Dichloro  diphenyl trichloroethane
 Diisopropylmethyl Phosphonate
 Dimethyl  Disulfide
 Dimethymethyl Phosphate
 Hydrogen
 Water
 Hydrogen  Bromide
 Hexachloro-1, 3-butadiene
 Hydrogen  Chloride
 Hexachlorocyclopentadiene
Mercury
Potassium
Magnesium
Methyl  Isobutyl  Ketone
Nitrogen
Sodium
2306E
                                      vi

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                             CHEMICAL flRRRFVTflTTnK|<;
                                   (Continued)
 NaOH

 °2
 OH
 Pb
 PERC
 PNA
 Se:
 TOC
 Zn
Sodium Hydroxide
Oxygen
Hydroxyl
Lead
Tetrachloroethene
Polynuclear Aromatic
Selenium
Total Organic Carbon
Zinc
                                      vii
2306E

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                               1.0   INTRODUCTION
1.1  PURPOSE

The  Program  Manager's  Office  for  Rocky  Mountain  Arsenal  Contamination
Cleanup  (PMO)  is currently  in the process  of gathering information on  the
technical and  economic  aspects of incineration/thermal treatment of Basin  F
wastes.  This  information gathering  process  is one  aspect  of developing  a
broad  remedial  action  alternative  for Basin  F.   The  PMO  has  taken  this
action in accordance with the  National  Contingency Plan,  50  Federal Register
47912  (1985).   Accordingly,  the  PMO  has contracted  Ebasco  to conduct  this
work effort under Task Order 17.

Task Order  17 comprises  several  distinctly separate work elements (Ebasco,
1986a).  One  of these  work elements  consists of laboratory investigations
for determining  the incinerability  characteristics of Basin  F wastes.   Under
this work element,  Ebasco has designed and executed a laboratory test program
(Ebasco,  1986b).  This report  describes  the  rationale,  performance,  and
results of that undertaking.

The objectives of the laboratory test program were to:

    o  Gather  information  on  the  physical,  chemical,  and  thermodynamic
       properties of Basin F wastes (both liquid and contaminated soils) to
       ensure reasonable success in designing an incineration program;

    o  Provide a bench-scale  apparatus that  can  be  used  to  determine the
       incinerability characteristics of Basin F wastes;

    o  Demonstrate that  99.99 percent  destruction  and removal  efficiency
       (ORE) is  achievable for the hazardous organic constituents  associated
       with Basin F wastes;
                                      1-1

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     o  Determine what  residence times, temperatures,  and levels of excess
        oxygen  (02)  will   achieve  99.99  percent  ORE  within  the  most
        cost-effective incinerator technology framework; and

     o  Provide guidance for selecting  the  final  incineration  technology  and
        optimizing  the   transition  from  a  bench-scale  system  to  a  pilot
        plant, or from a bench-scale system to a full-scale operation.

1.2  STUDY CONSTRAINTS

The  laboratory test  program was  designed  within  the available  resources.
The  basic  objective  of the program  was to determine and demonstrate  that
contaminants associated with Basin F soils and liquids could be  decomposed
through thermal  treatment.   To  that  extent, the  program was delineated by
the following factors:

     o  The  bench-scale  thermal   destruction   device  was   constructed  to
        determine  the  thermal  decomposition  characteristics  of  Basin  F
        contaminants in a nonflame mode environment;

     o  Testing  of  Basin  F  wastes  was   limited  to  contaminated  solids
        (overburden) overlying the  basin's  asphalt liner and liquid from the
        main impoundment;

     o  Maximum  temperatures at  which  the bench-scale  Incineration system
        was  operated were  900°C  at  the  primary burner  and 1200°C  at the
        secondary burner;

     o  Secondary burner residence times were 2 and 5  seconds; and

     o  Maximum primary burner sample sizes were  limited to 500 grains.

1.3  STUDY APPROACH

The  technical  approach  developed  for  this program  recognizes  the  inherent
limitations of investigations within  a  laboratory environment as well  as the
lack of precise data concerning the feedstocks to be  incinerated.

                                      1-2

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The  technical approach  Involves using  equipment  to  simulate  three  of  the
major  incineration  mechanisms:   (1) pyrolysis;  (2) primary incinerator post-
flame; and (3) afterburner postflame.

The  technical  approach  was designed to  focus on and evaluate the impacts of
incinerating  Basin  F contaminated  soil.   Initially,  this approach  did  not
designate one  or more principal  organic  hazardous  constituents (POHCs) to be
incinerated,   but   rather  evaluated   the  impact   of  incineration  on  all
compounds identified in the soil samples.

The  technical  approach  began  with   limited   characterization  of  selected
compounds  in  terms of  physical,  chemical, and  thermodynamlc  properties.
Following this characterization, the  contaminated soil  compounds  were then
tested for determining  the impacts  from  incineration  at  two residence times
(in  the  afterburner),   two   temperatures,   and two  levels  of  excess  02.
Multiple runs  were  used to ensure that  the ORE associated with any compound
would  not  be  masked,   regardless  of  the concentration of  the  incoming
material to be incinerated.
                                      1-3

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                     2.0   CHARACTERISTICS OF BASIN F WASTES

 2.1  INTRODUCTION

 Waste characterization  is  a major  factor in  assessing the  feasibility of
 destroying hazardous waste material  by  incineration.   This characterization
 affects  the design  of the  incinerator and its  emission control system, and
 aids in  determining  incinerator operating conditions for complete destruction
 of a specific  organic compound.

 This chapter discusses physical, chemical, and thermodynamic (PCT) properties
 of  Basin   F   wastes that  are  important  in  evaluating  the  incineration
 technology as  well  as  designing a  full-scale  incineration system  based on
 the selected   incineration  technology.   The discussion  of  PCT properties of
 Basin F  wastes are  based on past studies and  limited sampling and analyses
 performed  under this program (Task 17).

 2.2  BACKGROUND

 2.2.1 Basin F History

 Basin F  is located  in  the northwest  part  of the Rocky Mountain Arsenal in
 Section  26.  This asphalt-lined basin had been used  for total retention of
 chemical  wastes   generated  from Army  and Shell  operations.   The  basin was
 used  from 1956 to  1982.  The types  of chemical wastes discharged into the
 basin consisted mainly of aqueous solutions of various  sodium  salts  including
 chloride,  fluoride,  hydroxide,  methyl  phosphonate,  acetate,  sulfate, and
 pesticides.  The  potential for industrial  waste discharge into Basin F was
 eliminated  in  1982  when the  chemical  sewer   line  feeding  the  basin was
 excavated.  The  remaining  Basin  F  liquid has  been evaporating  since  that
 time.  A comprehensive  study conducted in  1982  revealed that the overburden
 and  soil  underneath the  liner of  the  basin   have  been  contaminated  with
various  chemicals that  had accumulated  in Basin  F during  its operational
period.
                                      2-1

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 2.2.2  Basin F Waste  Characteristics

 In addition  to the  actual  liquid  wastes contained  within Basin  F,  three
 other categories  of  materials  are present  which may  be  considered  waste
 materials.   These  are the basin liner itself, the overburden above the liner
 (including  precipitates), and  any  contaminated soil adjoining the  basin or
 beneath   the  liner.   Overburden,  liner,  and  contaminated  soils  can  be
 considered together for treatment and disposal.

 Numerous  analyses  have been  conducted  on Basin F  liquid  through the years.
 A  comprehensive review of  the  previous analytical results  was  conducted in
 1977  (Buhts  et  al.,  1977).  The  results of  this effort are  summarized in
 Table 2.2-1.  Contaminant  concentrations in the liquid have likely increased
 since 1977 due to the evaporation of water within the basin.

 A  comprehensive study  of Basin  F was  conducted in  1982 to  determine the
 distribution  of contaminants in  the overburden  and  in the  soil underlying
 the  liner,   and  to assess the  condition of the  liner  (Myers  & Thompson,
 1982).  This  study  involved 16  shallow  borings in the exposed portion of the
 basin as  indicated in Figure  2.2-1.

 The sample cores and  samples  of the overburden were subjected to a series of
 analytic  extraction  procedures.   Among  those  initially  considered  were
 extraction procedure  (EP) toxicity, solid waste  leaching procedures (SWLP),
 and total extraction (bulk  analysis).   The  EP toxicity  procedure  yields  a
 determination  of whether the waste  would be  considered hazardous under the
 Resource  Conservation and Recovery Act  (RCRA).   The SWLP is  similar to the
 EP toxicity  test with the  exception that a  neutral  pH water  is used as an
 extract to  more accurately  simulate leachate migration  potential  (Myers  &
 Thompson,  1982).   Bulk  analyses  utilize  a   solvent  rinse to  determine the
 gross  amount  of  contaminant held  within the  waste matrix  that  could be
 potentially released.

The extracts  from  the SWLP  tests  conducted  on subsamples of the cores  were
analyzed  for  a select  group   of  contaminants   that  had  been identified
previously  in  the Basin  F  liquid.   The  concentrations  of  many  of the
                                      2-2

-------
                              TABLE 2.2-1

               CHEMICAL CHARACTERIZATION OF BASIN F LIQUID
Compound or Parameter
PH
Aldrin
Isodrin
Dieldrin
Endrin
Dithiane
DIMP
DMMP
Sulfoxide
Sulfone
Chloride
Sulfate
Copper
Iron
Nitrogen
Phosphorus (total)
Hardness
Fluoride
Arsenic
Magnesium
Mercury
Cyanide
COO
TOC
Units
-
PPb
ppb
PPb
ppb
Ppb
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
PPb
ppm
ppm
ppm
Concentration Ranged
6.9
50.0
2.0
5.0
5.0
30.0
10.0
500.0
4.0
25.0
48,000.0
21,000.0
700.0
5.0
120.0
2,050.0
2,100.0
110.0
1.0
35.0
26.0
1.45
24,500.0
20,500.0
- 7.2
- 400
- 15
- 110
- 40
- 100
- 20
- 2,000
- 10
- 60
- 56,000
- 25,000
- 750
- 6
- 145
- 2,150
- 2,800
- 117
- 1.3
- 40
- 29
- 1.55
- 26,000
- 22,500
I/  Based on analysis of various samples from different locations and
    depths in the basin (Bunts et al., 1977).
2306E

-------
  ^-APPROXIMATE
     WATER LEVEL
         1882
       LIQUID
       BORING LOCATIONS
                                   FIGURE 2.2-1
                        LOCATION OF BORING SITES WITHIN BASIN F
SOURCE: MYERS AND THOMPSON. 1982

-------
 contaminants  in the SWLP  extracts  were very low  or  beiow detectable limits
 (Myers  & Thompson, 1982).   A map summarizing the  SWLP cores is presented in
 Figure  2.2-2.

 The  contaminants  found  above their  respective action  level concentrations
 included Aldrin, Dieldrin, Endrin, Isodrin, organo-sulfur compounds, dibromo-
 chloropropane  (DBCP),  arsenic,  and fluoride.   Borings 01 and  02  were found
 to  have the greatest  number  of contaminants in the  extracts for  all depths
 intervals.   Also,   the concentrations  of the  contaminants   in  the extracts
 from these two  borings were generally higher than those associated with other
 borings.

 The  SWLP tests,  conducted  on  the  overburden  samples  collected  from five
 boring  sites,  resulted in  much higher  concentrations of contaminants in the
 extracts  than  in those associated  with the soils  underlying the  liner.  In
 addition  to the contaminants  identified in the  SWLP extracts from the cores,
 concentrations  of   diisopropylmethyl  phosphate  (DIMP)  and  dicyclopentadiene
 (DCPD)  were found in some of the extracts  from the overburden.

 Only the  extracts  from the cores collected at Boring 02 from the 0 to 1 foot
 (ft)  and 1 to  2 ft  intervals  exhibited  concentrations  exceeding 100 times
 their respective water quality  levels (see Figure 2.2-2).   For the 0 to 1 ft
 interval, the concentrations  of Aldrin, Dieldrin,  Endrin, and  Isodrin in the
 extract  exceeded  the  criteria.   In  the  1  to  2  ft  interval,  only the
 concentration of Dieldrin  in the extract  exceeded  the criteria.

 As discussed previously, Boring 02  was the only boring  location in the  study
 where the liner was  found to  be in  poor condition.   Contamination in the
 overburden  or  liquid  (when  this area  was innundated)  probably was able to
 migrate  in  high  concentrations  into  the  soil  due  to  the deteriorated
 condition of the liner.  In other areas of the basin  evaluated  in  this study,
 the liner appeared to have maintained sufficient integrity to prevent the
migration of large  amounts of contaminants into the underlying  soils.

Recent  investigation  (ESE, 1986)  at Basin  F revealed  that subsurface  soil
contamination has  occurred only in locations where integrity  of  the asphalt
                                      2-3

-------
                                                                        A ALDRIN
                                                                        B DIELORIN
                                                                        C ARSENIC
                                                                        O ENORIN
                                                                        E ISODRIN
                                                                        F FLUORIDE
                                                                        G SULFURS
                                                                        H DBCP
                                                                        X ACTION LEVELS NOT EXCEEDED
                                                                      NO SAMPLE NOT ANALYZED
                                                                        • INDICATES CONCENTRATION
                                                                          EXCEEDS 100X THE ACTION LEVEL
                                                                            NOTE: NUMBERS IN PARENTHESIS
                                                                                 DENOTE INTERVALS BELOW
                                                                                 LINER AS FOLLOWS:
                                                                                 (1)- 0.0 -1.0 FT
                                                                                 (2) -1.0 -2.0 FT
                                                                                 (3) - 2.0 - 3.0 FT
                                                                                 (4) - 3.0 • 4.0 FT
APPROXIMATE
WATER LEVEL
     1982
                                                                   A, B, D (2)
                                                                  31   F(3)
                   X(2)
                 acoi
                  NO (4)
                                                                            AD(1)
                                                                             X(2)
                                                                            NO (3)
                                                                            NO (4)
                                              X(2)
                                              X(3)
                                             NO (4)
                                       C(2)
                                      A, 0(3)
                                       X(4)
                                                                             A.B.C.D. E(1)
                                                                               A, C, D. F (2)
                                                                             A. B, C. D, F (3)
                                                                             A,B,C. D, F(4)
                                                             X(2)
                                                             X(3)
                                                           NO (4)
                                                                          A«B*C. D«E*F. G.
                                                                           A. B*C, 0. E, F. G (2) 02
                                                                             A. B. C. D, F. G (3)
                                                                               A. C, D, F. G (4)
                                                                     X(2)
                                                                     X(3)
                                                                    NO (4)
                                        C(2)
                                       NO (3)
                                       NO (4)
LIQUID
BORING LOCATIONS
                                           FIGURE  2.2-2
                          CONTAMINANTS IDENTIFIED IN THE SWLP EXTRACTS
                                       OF THE SOILS IN BASIN F
OURCE MYERS AND THOMPSON. 1982

-------
 liner is questionable.   Analytical data collected from this investigation is
 presented in Table  2.2-2.   The study  concluded that the  highest  levels of
 contaminants  (a variety of volatile organics, organochlorine pesticides, and
 elevated levels  of  metals) were  found in  the  boreholes  located  along the
 eastern  boundary of  the basin  and/or in areas where liner  integrity was poor
 (ESE,  1986).  Deepest contamination  (35 ft) was  found along the east boundary
 and  in the southernmost area of Basin F.

 2.3  SAMPLING

 The  purpose  of  the  sampling program was to  collect  Basin  F waste materials
 in  sufficient  quantities for  bench-scale  thermal destruction testing.   The
 sampling  program was not  designed to collect representative samples,  i.e.,
 samples  that  represent the average  spectrum of  contaminants associated with
 Basin  F.

 Grab  samples  from the north end of  the  basin were collected using a bucket-
 type  sampler.   Approximately  15 gallons  of liquid was  collected during the
 liquid sampling  program.

 Soil sampling was limited to collecting overburden from the most  contaminated
 area of  the basin.   It  was determined that the  source contamination problems
 should be tested explicitly.   For that reason,  overburden  from  the Borehole
 01  was  collected by  using a hand auger.   Borehole  01  was  selected for
 sampling  because past  study has indicated highest concentrations of contami-
 nants  in this  borehole than any  other boreholes studied.   Approximately 30
 kilograms  of  overburden  sample   were  collected during  the  soil sampling
 program.

 2.4  LABORATORY ANALYSIS

 2.4.1  Objectives

The  Basin  F   wastes  characterization   program  was  designed  to   gather
information on  physical,  chemical,  and  thermodynamic  properties that  are
essential  in  understanding   the  performance   of  the  bench-scale   thermal
                                      2-4

-------
                                    CONCENTRATIONS OF CONTAMINANTS  IN  SOIL SAMPLES UNDERLYING BASIN F LINER
Constituents
Volatile* (N-40)T
Chlorobenzene
CHCIj
1.2-Dichloroe thane
BCHO
BCHD
Ethyl benzene
Tetrachl oroethene
Tetrachloroethene
Toluene
Toluene
1,1,1-Trichloroe thane
m.xylene*
MIBK
DMOS
Benzene
o,p-xy1ene
Semi-Volatiles (N-401
Aldrin
Dieldrin
Endrin
DIMP
Isodrin
OCPD
DBCP
PCPMS
PCPMSO
DMMP
PCPMS02
Hetalt (N-40)
Cadmium
Chromium
Copper
Lead
Zinc
Arsenic
Mercury
Number
of
Detections*

2
3
1
5
1
2
7
1
7
_
1
2
2
3
3
1

9
7
7
2
7
7
7
3
5
6
14

1
36
40
4
35
20
1
Concentrations (ua/om)
Range

0.8-5
0.3-70
1
2-30
25
1-8
1-40
25
1-1000
25
0.4
0.4-5
0.4-1
2-60
1-3
10

0.7-4000
100-2000
90-900
0.5-0.8
100-3000
30-4000
0.044-8.1
6-700
4-70
3-70
0.5-300

2.0
11-34
5.0-2300
18-35
33-320
4.8-18
0.08-0.08
Mean

3
30
9
_
5
10
_
400
__
—
2
0.7
30
2
—

1000
500
500
0.6
1000
1000
2.4
400
20
20
30

19
85
24
68
9.6
0.08
Median

3
4
5
—
5
10
—
300
—
—
2
0.7
10
2
— -

1000
400
400
0.7
1000
600
0.86
400
5
7
5

18
16
21
57
9.2
0.08
Standard
Deviation

3
40
10
_
5
10
—
400
—
—
3
0.4
30
1
~~

1000
500
300
0.2
1000
1000
3.0
400
30
30
70

5.6
370
7.7
49
3.6
0.08
ESE
Detection
Limit
(ug/gm)

0.3
0.3
0.3
0.3
__
0.3
0.3
—
0.3
—
0.3
0.3
0.5
0.3
0.3
0.5

0.9
0.3
0.7
0.5
0.3
0.3
0.005
0.3
0.4
2
0.3

0.9
7.2
4.8
17
16
4.7
0.05
MRI
Detection
Limit
(ug/gm)

0.3
0.7
0.4
0.8
«
0.4
0.5
__
0.3
—
0.5
—
0.4
4.0
1.0
0.5

0.5
0.6
4.0
3.0
0.6
6.0
0.005
0.3
1.0
3.0
0.4

0.5
7.4
4.9
16
28
5.2
0.07
•  Number of samples in which constituent was detected.
T  N • Number of samples analyzed.

Source:  ESE (1986).

-------
 destruction unit and also in designing a  full-scale incineration system.  It
 should be recognized that the  sampling and analytical programs were  limited
 in  scope, and as such, the  results  derived from these  programs  may not be
 representative of the entire  spectrum of  wastes  associated with Basin  F.

 2.4.2  Analytical Parameters

 The physical, chemical, and  thermodynamic parameters  that were analyzed  for
 Basin F liquid and overburden samples are identified in Table  2.4-1.

 2.4.3  Basin F Liquid

 The Basin F liquid sample was  described  to have a motor  oil-like  appearance
 and a fairly  homogeneous  composition.  The pH  of  the sample was  6.02.   The
 analytical  results of  the Basin F  liquid sample are shown  in Tables 2.4-2
 and  2.4-3.    Only  parameters  found  in  concentrations  higher  than their
 detection limits  are  reported  in   Tables  2.4-2  and  2.4-3.  Table 2.4-2
 presents  the results  of proximate,  heating value, and ash fusion temperature
 analyses  of  Basin  F liquid and  overburden samples.

 Basin  F  liquid  is highly corrosive  (corrosivity 50  millimeters   per year).
 It  is  neither  ignitable nor  reactive.  The heating value  of the liquid waste
 was  found  to  be 4  Btu/lb.   Table  2.4-3  presents  analytical  results of
 organic,  inorganic,  and  metal  constituents  that were  detected in  Basin  F
 liquid.

 The  concentration of sodium (Na) was  found to be 2300  parts per million (ppm)
 while  calcium (Ca),  magnesium  (Mg)  and  potassium (K)  ranged from  5 to 30
 ppm.   Among  the inorganic constituents,  chloride concentration was found to
 be  the highest  (120,000 ppm) which  is almost  2.5 times  more than what  was
 found in  1977  (See Table 2.2-1).

Among the trace  metals, copper concentration was found to be high (210  ppm)
while  cadmium  (Cd),  lead  (Pb),  and  mercury   (Hg)  were  in the  parts  per
billion (ppb) range (74 to 140  ppb).
                                      2-5

-------
                                  TABLE  2.4-1

                        SUMMARY OF LABORATORY ANALYSES
Overburden (One Sample)

       Volatlles by GC/MS
       Semi-Volatiles by GC/MS
       ICP Metals
       Arsenic
       Mercury
       3 RCRA Tests (ignitability, reactivity, corrosivity)
       Proximate and Ultimate Analysis
       Elemental Composition
       Heating Value

Liquid (One Sample')

       Volatile Aromatics
       Volatile Halocarbons
       Organo Chlorine Pesticides
       DCPD/BCHPD/MIBK
       Organo Sulfur Compounds
       DIMP/DMMP
       ON/OP Pesticides
       Arsenic
       Mercury
       ICP Metals
       3 RCRA Tests
       Elemental Composition
       Heating Value
2306E

-------
                                  TABLE  2.4-2

              PHYSICAL, CHEMICAL, AND THERMODYNAMIC TEST RESULTS
                      OF BASIN F LIQUID  AND OVERBURDEN iX
       Parameter                             Liquid          Overburden
Proximate Analysis (percent weight, wet)
    Moisture                                                   23.93
    Volatiles                                                  14.47
    Fixed Carbon                                                2.33
    Ash                                                        59.20
                                                              100.01
Higher Heating Value (Btu/lb)
    Wet Basis                                 4                37
Ash Fusion Temperature ("F)!/
    Initial Deformation                                      2242 - 2253
    Softening                                                2329 - 2377
    Hemispheric Lump                                         2512 - 2622
    Fluid                                                    2784 - 3000
Reactivity (mg/gm)
    Cyanide                                  <0.02              3.6
    Sulfide                                  <0.02             <0.02
Corrosivity
    Millimeters/year                         50                 1.1
Other
    Bulk Density (lbs/ft3)                                    100
    Specific Heat Dry (Btu/lb-°F)                               0.25  -  0.30
    Thermal Conductivity (Btu/hr-ft-eF)                         0.32

II Tests were conducted by UBTL in Salt Lake City under Task 17.
21 On one of the ash fusion analyses, a eutectic effect was indicated.
2306E

-------
                                  TABLE 2.4-3
                  ANALYTICAL RESULTS OF BASIN F LIQUID SAMPLE
Organics
Aldrin (ppb)
Oieldrin (ppb)
Endrin (ppb)
Isodrin (ppb)
ppDDE (ppb)
ppDOT (ppb)
DIMP (ppb)
CPMSO (ppb)
CPMS02 (ppb)
Hexachlorocylopentadiene (ppb)
Atrazine (ppb)
Malathion (ppb)
Parathion (ppb)
Supona (ppb)
Vapona (ppb)
Benzene (ppb)

2,300
459
596
1,980
109
340
400
1,000
1,000
1,850
220
810
110
340
890
7.7
Inorganics
Calcium (ppm)
Magnesium (ppm)
Potassium (ppm)
Sodium (ppm)
Chloride (ppm)
Fluoride (ppm)

METALS
Arsenic (ppm)
Cadmium (ppb)
Chromium (ppb)
Copper (ppm)
Lead (ppb)
Mercury (ppb)
Zinc (ppb)


6.8
5.6
30
2,300
120,000
21


3.0
8.4
85
210
74
140
950

2306E

-------
 The  Basin  F  liquid  analysis  for  selected  organic  compounds  indicated  no
 volatile  halogenated  organics  present  above  the  limits  of  analytical
 detection.   Of the volatile  aromatic organics, benzene was  found to be 7.7
 ppb.

 Among the  organochlorine pesticides,  Aldrin,  Isodrin,  and hexachlorocylo-
 pentadiene  were found to be  2300 ppb,  1980 ppb,  and 1850 ppb, respectively.
 The remaining chlorinated pesticides  ranged from 109 to 596 ppb.

 The organophosphate pesticides ranged  from 110 to 890 micrograms per liter
 (ug/1) or  ppb,  with highest  concentration being attributed  to Vapona (890
 PPb).

 The  concentration  of DIMP,  CPMSO,   and  CMPS02 were  found  to be  400 ppb,
 1000 ppb, and 1000  ppb, respectively.

 2.4.4 Basin  F Overburden

 The analytical results of  the overburden  sample  are shown  in Tables 2.4-2
 and 2.4-4.   The proximate analysis  showed that the  sample contained  almost
 24  percent  moisture and  15  percent  volatile matters.  The ash content  of the
 sample  was  found  to  be  59 percent.   The heating  value of  the  sample was
 measured to be 37 Btu/lb.

 Analyses  on   reactivity,   corrosivity,   and  ignitability   indicated  the
 overburden  sample  to  be  nonignitable,  corrosive  (corrosivity 1.1 millimeter
 per year), and reactive due to cyanide content  (3.6 milligrams per gram).

 Concentrations  of  sodium and chloride were  found to  be 4500  ppm  and 1700
 ppm,  respectively.  Among the trace metals,  the concentration of copper was
 found to be the highest  (5900 ppm),  followed by zinc (430 ppm)  and  lead (270
The  organic analyses  indicated  an absence  of  any volatile  species.   The
chlorinated pesticides  present in the  sample  were Aldrin, Dieldrin,  Endrin,
                                      2-6

-------
                                 TABLE
                  ANALYTICAL RESULTS OF THE OVERBURDEN SAMPLE
     Organics
                            Inorganics
Aldrin (ppm)
Dieldrin (ppm)
Endrin (ppm)
Isodrin (ppm)
Supona (ppm)
DCPD (ppm)
DBCP (ppm)
CPMS (ppm)
CPMSO (ppm)
CPMS02 (ppm)
2480
1300
 165
 100
   6.7
  69.7
  13.7
 216
  34.7
 180
Sodium (ppm)
Chloride (ppm)

METALS

Arsenic (ppm)
Cadmium (ppm)
Chromium (ppm)
Copper (ppm)
Lead (ppm)
Mercury (ppm)
Zinc (ppm)
4500
1700
   3.9
   1.4
  83
5900
 270
   3.5
 430
2306E

-------
 and Isodrin.   Concentrations  of Aldrin and  Dieldrin were found  to  2480 ppm
 and 1300 ppm, respectively.

 The other  organic  compounds  found in  the  sample  were  DCPD,   DBCP,  CPMS,
 CPMSO, and CPMS02 with concentrations ranging from 13 to 216 ppm.
                                      2-7
2306E

-------
                     3.0  BENCH-SCALE INCINERATION SYSTEM
 3.1  RATIONALE FOR A BENCH-SCALE TEST SYSTEM

 Thermal  decomposition  laboratory  tests  have  been  performed  on both  pure
 compounds  and field samples to  determine  incineration  parameters,  including
 residence  time,  temperature, and  excess  oxygen required to  decompose  toxic
 chemicals.   These  laboratory  tests  have  been  performed  primarily  using
 milligram-to-gram size  samples.  These  small sample  sizes have been adequate
 to characterize  incineration parameters for pure compounds and compounds in
 high concentrations.   For chemicals that  are present in low  concentrations,
 these  small  sample  sizes  have not  been adequate to demonstrate 99.99 percent
 destruction  due  to  the analytical limits  of  detection  of the off-gases.  It
 is  of  interest  to demonstrate  99.99  percent  destruction   for all  toxic
 constituents  in  a  feed sample regardless  of  whether or not that constituent
 is chosen as  a  POHC.  Although  there are  substantial data  on  the thermal
 destruction  of individual compounds,  incineration tests on field samples are
 necessary  to adequately simulate the interaction  of various  constituents at
 high temperatures  and  the production  of  products  of  incomplete combustion
 (PIC).  The  bench-scale test unit  for Task 17 was designed to measure ORE up
 to 99.99  percent for  constituents of  concern  at Basin  F  for soil, sludge,
 and liquid samples.

 3.2  SYSTEM DESCRIPTION

 The laboratory bench-scale unit  was designed to evaluate thermal destruction
 efficiency  at temperatures  up  to  1200°C  and  residence times  from 2  to  5
 seconds.   The unit  utilizes a  batch-load  system  with two   furnaces  and  a
 blended carrier  gas to simulate  combustion gases (Figure  3.2-1).  The  first
 furnace  volatilizes  the   constituents  while  the   carrier  gas  moves   these
 constituents  into  the  secondary furnace  which simulates  afterburners in  a
 full-scale incineration plant.   In the secondary furnace, additional blended
gases  with  0_  are added and  temperature  is increased  to  decompose  the
hazardous  constituents.   The  combustion  products  in  the off-gas  are  then
 collected in various sorbents in the  sampling train.
                                      3-1

-------
          ROTATING
          FURNACE
  "-TFlD
         INCINERATION
           FURNACE
         (AFTERBURNER)
   GAS
 SUPPLY
CONTROLS
AA A
                    FLY ASH
                   SEPARATOR
                  _ COOLING
                  r- SECTION
SAMPLING
 TRAIN

                                   EXHAUST
                                     PUMP
SECONDARY
  GAS
PREHEATER
                        FIGURE 3.2-1
       LABORATORY SCALE INCINERATION  UNIT

-------
 3.2.1  Primary Furnace

 The  primary  furnace  (Figure  3.2-2)  was   an   electric  furnace  with  a
 programmable temperature controller  capable  of maintaining  1000°C with gas
 flows up to 20  liters  per  minute.  A gas supply  system  was  used to provide
 blends  of  nitrogen  (N2),  carbon  dioxide   (C02),   and  02  to  simulate
 various combustion processes  in fuels.   The  primary  furnace barrel (Figure
 3.2-3) was  130  millimeters (mm)  in  diameter  and 200 mm in  length.  During
 test  conditions  the maximum  temperature  rise  of the  primary  furnace was
 about 5.5°C per minute  and  the carrier gas velocity was  maintained between 6
 and 8 centimeters  (cm) per  second.

 3.2.2  Fly  Ash Trap

 A  fly ash  separator  was installed between  the primary and secondary furnace.
 The purpose of this separator was  to remove  ash  from the carrier gas and to
 prevent plugging of  the  secondary furnace.   The ash separator was  a cyclone-
 type  design capable of  removing  particulates  as small  as  100 microns.  It
 was constructed  of  stainless  steel and  insulated  to  prevent  heat  loss
 between the  primary and secondary  furnaces.

 3.2.3   Secondary Combustion Gas

 Additional  gases were introduced  between the  primary and secondary furnaces
 to  simulate  secondary combustion gases.  The  composition of this gas was the
 same  as that of the primary  carrier gas which increases the total gas flow
 rate  by 50  percent.   The carrier  gas was  preheated to near (± 50°C) that of
 the primary  carrier gas temperature.

 3.2.A   Secondary Furnace

 The  secondary  furnace  was designed to  heat  gases  up  to  1200°C from the
primary  furnace  along  with the  secondary  airflow  and  to maintain the  gases
at  this temperature for  between 2  and  5  seconds.   To  have fully developed
flow while avoiding high  pressure losses in the furnace,  a velocity range of
20  cm/sec  to 500  cm/sec was  established.   For this velocity range and the
                                      3-2

-------
 fins Supply
ODD
oo o
        Filter
                On/
                Off
Temperature
Controllers
                                        Temperature
                                        Recorder
                                        Programmer
                  FIGURE 3.2-2
 ROTATING TUBE FURNACE  ARRANGEMENT

-------
      RIDING
       RING
                               130 mm DIA.
       RIDING
        RING
150 mm DIA.
                                                             GAS
                                                            JNI.GT
                                                              TYPE
                                                          THERMOCOUPLE
DRIVE
CHAIN
SPROCKET
              SLIP
              SF.AL
                        FIGURE  3.2-3
                ROTATING TUBE  UNIT

-------
 desired gas flow rate,  the furnace tube diameter was approximately 2-1/2 cm.
 To maintain  a  residence  time  of  5  seconds,  the furnace  tube was  built
 approximately  10 meters long.   The secondary furnace tube was constructed of
 fused quartz to provide a nonreactive environment  at  high temperature.  Two
 furnace tube lengths were used to  provide  2 and 5 second residence times in
 the secondary  burner.

 3.2.5  Cooling Section

 The  cooling section consisted  of a  straight 2.5  cm diameter  quartz tube
 approximately  3 feet long.   Exit temperature  from the  cooling  section was
 monitored  to  insure  that  temperature  was  maintained   between  200°C  and
 300°C.   Insulation was applied to the tube to adjust the exit temperature.

 3.2.6   Sample  Collection

 All  off-gases  from  the secondary  furnace  entered  the  sample  collection
 system  that was  designed  to  remove organic  and inorganic  constituents of
 concern.   A pump  was  used  downstream  of  the  sample collection  system to
 maintain  near-atmospheric  pressure  in  the entire  flow  train.   The  sample
 collection system is described in detail in Section 3.3.

 3.3  SAMPLING

 3.3.1   Introduction

Gases generated  from all test incineration  runs  require  a collection  system
of  nonparticulate  and  particulate  fractions.   In  general,  the   sampling
apparatus for collecting off-gas effluents includes three major components:

       o  One  or more thermostatically  controlled compartments  to  maintain
          the  gas  at a  temperature consistent with  the collection medium,
          usually hot (200°C)  for  particulate collection  and cool (20°C) for
          sorbent collection of the more volatile constituents;

       o  Sample collectors,  such as filters and sorbents;  and
                                      3-3

-------
       o  Vacuum pump and gas meter.

The sampling train used is shown  in  Figure  3.3-1.   This  device  is  physically
similar to the Modified Method 5 (MM5) sampling train.

3.3.2  Particulate and Residue Collection

Bottom residue  left  in the kiln  from the test burn was removed by the most
efficient means available to the lab which was consistent with:

       o  Complete removal (>99 percent);
       o  Prevention of outside contamination; and
       o  Prevention of damage to the kiln.

Residue removal and cleaning of the  kiln were made to  assure subsequent test
burns were  not  cross-contaminated.  Bottom residue was  stored at  about  4°C
in glass bottles with Teflon-lined caps until combined  with the fly ash.

The fly  ash separator retained the  larger  particulates carried through  the
primary furnace tube.  The fly ash was removed and stored at about  4°C.

Filter cassettes were  used to trap particulates which were not separated as
fly ash and may vary in size  from 1 to 100 microns.  The  filter  used was a
glass  fiber-type  and  was  stored   at  4°C.   in  a  glass  bottle  with  a
Teflon-lined cap.

Figure 3.3-2 illustrates  the flow of the residue  sample into the analytical
system.  The three  solid  fractions from the  test  burns  were weighed and the
weight summed to estimate the percentage of  sample volatilized:

                                              Wp   WF   Wp
            Percent Sample Volatilized = (1 -  p *  ^       ) x  100
                                                    WS
                 Where     WB = Weight of bottom residue
                           Wp = Weight of fly  ash
                           Wp = Weight of filter particulates
                           W. = Weight of original  sample
                                      3-4

-------
                      HEATED AREA
TEMPERATURE SENSOR
                 RECIRCULATION PUMP

                          THERMOMETERS
                       ORIFICE
  THERMOMETER

L_ ^FILTER HOLDER
         SORBENT
          TRAP
                                          IMPINGERS  'ICE BATH

                                        PAS9_ VALVE
                                              MAIN VALVE
THERMOMETER

    CHECK VALVE
                                DRY GAS   AIR-TIGHT
                                 METER      PUMP
                                                                 VACUUM LINE
                                  FIGURE 3.3-1
                              SAMPLE TRAIN

-------
PHYSICAL
 TESTS
INORGANIC
  TESTS
                                  1
ORGANIC
 TESTS
                                                  PARTICULATES
                                                      i
                                                   WEIGHTED
                                                    COMBINE
                                                     WITH
                                                     XAD-2
                                                    EXTRACT
                                                      I
                                                    ANALYZE
                        Figure 3.3-2
         SOLID  RESIDUE  COLLECTION  FLOW CHART

-------
The  bottom  ash and fly ash were combined and  homogenized.  Allquots  of  this
residue were  taken for the various  chemical and physical analyses  required
to determine the distinction efficiency of the POHCs.

The  particulate filter was  weighed and  combined with  the  XAD-2 resin  for
extraction and analysis.

Table 3.3-1 describes  the  types of sorbent and  impinger solutions that  were
used to  trap  organic and  inorganic  products from the  incineration.   Figure
3.3-3 depicts the sampling train.

After  a test  run,  the sorbents  and  impinger  fractions,  as  well as  the
condensate  when   applicable,   were   transferred  to   glass   bottles   with
Teflon-lined caps for storage at about 4°C.

3.A  OPERATING PROCEDURES

The  following  sections outline  operational  considerations  for the  soil,
sludge, and liquid tests.

3.A.I  Soil Tests

The typical operation sequence  for the bench-scale  soil sample testing is as
follows:
       o  Weigh out appropriate sample size (200-500 grams ±0.5 grams).

       o  Place the  sample  in  the  kiln  barrel  and  bolt the  barrel halves
          together.

       o  Place the kiln barrel into the  furnace and attach the thermocouple
          and gas connections.

       o  Set the  secondary  furnace temperature  and allow it  to reach test
          condition temperature before proceeding.
                                      3-5

-------
                                  TABLE 3.3-1
                         GAS SAMPLE COLLECTION MATRIX
Compound
 Class
   Sorbent
Impinger
Water
 Trap*
Volatile Organics
Tenax/Charcoal
                      Test
Semivolatile Organics   XAD-2


Volatile Metals




Acid Compounds


Cyanide


Basic Compounds
                    Silver Catalyzed

                    Ammonia Persulfate


                    0.1 NaOH


                    0.1 NaOH


                    0.1 HC1
                      Test


                      Test




                      Test


                      Test


                      Test
*A water trap will be utilized when the test sample is sludge or liquid.
 (See text.)
2306E

-------
GAS FLOW.
         FILTER
                        CONDENSER
                   CONDENSATE
                     TRAP
TENAX/CHARCOAL
    TRAP
                                  IMPINGERS
                                   XAO-2
                   FIGURE 3.3-3
          MODIFIED SAMPLING TRAIN
        FOR HIGH  MOISTURE SAMPLES
                                           VACUUM
                                            PUMP

-------
o  Switch on the evacuation exhaust pump.

o  Establish carrier gas flow at the desired blend and  flow  rate.

o  Start temperature ramp on primary furnace.

o  After  reaching  the  desired   test  temperature  on   the   primary
   furnace,   maintain  desired  test  conditions  for  one  hour  before
   starting shutdown procedures.

o  Turn  primary  furnace off  and  stop  barrel  rotation,   but  continue
   gas flow.

o  After  primary furnace  has  cooled  to  400°C,  turn off  secondary
   furnace.

o  Divert gas from sampling train and remove collected samples.

o  After primary  furnace has cooled to near room temperature, remove
   kiln barrel and disassemble.

o  Remove residual sample from barrel.

o  Disassemble fly ash collection system and remove fly ash.

o  During   the   course  of   the  system   operation,   the  following
   parameters were monitored and recorded:  N2, CO,,, and  02 flow
   rates of primary and  secondary gasses,  temperature of the  rotating
   kiln  gas,  fly ash separation  system  exit gas,  secondary  furnace
   and cooling  section  exit  gas, particulate sample  isothermal box,
   and impinger  isothermal box. The  sample train flow meter  pressure
   differential also was monitored.
                               3-6

-------
                 4.0  BENCH-SCALE INCINERATION TEST  CONDITIONS
 4.1  SELECTED VARIABLES

 The  bench-scale test matrix was developed recognizing  the  typical operating
 parameters  for  hazardous waste  incinerators capable of  handling  chemically
 contaminated  solids.   These parameters are  residence time,  temperature,  and
 oxygen  level  necessary in the  combustion  process for complete destruction of
 organics.

 4.1.1   Time Parameters

 The  residence time  of  the waste  materials in the primary burner was selected
 on  the  assumption  that  a  full-scale  incineration  system should  be  able to
 vaporize all  organics  associated with Basin F  soils or overburden materials
 within  an  hour.  Therefore,  the residence  time for the primary  burner was
 limited to  a  maximum  of  one  hour  operation  at  the  selected  operating
 temperature(s).

 The  variation in residence  time in the secondary burner, however, was based
 upon values  in  hazardous waste  incineration literature.   The minimum value
 of 2 seconds appears in virtually all scientific and engineering publications
 concerning  hazardous waste  incineration, and  was  consistent  with  the  data
 presented (Frankel  et al., 1983) for commercially operated afterburners.

 The  5-second  value  appears near the  upper end  of  the  scale (Bonner et  al.,
 1981).

4.1.2   Temperature  Parameters

The  temperature  parameters  in  the   primary  and  secondary  chambers  were
selected based  on the limitation  of  the available laboratory equipment  and
the general operating practices  for the incineration of hazardous  wastes.
                                      4-1

-------
 The primary  chamber  (Linder  furnace)  used in  the  bench-scale setup  can
 operate  at the maximum temperature of  1000°C.  The  typical operating ranges
 for the  rotary kiln, fluid bed, and multiple hearth furnace are:

       Rotary kiln          820°C - 1600°C
       Fluidized bed        450°C -  980°C
       Multiple hearth      660°C - 1000°C

 Based  on the above assumptions, the operating  temperatures selected for the
 primary  burner were:   650°C,  800°C, and 900°C.   (Note:   For safety reasons,
 the  Linder furnace was not operated at the peak value of 1000°C).

 The  first temperature  in the  secondary burner at 900°C  which is consistent
 with   the minimum   afterburner  temperature  (Frankel  et  al.,  1984)  for
 afterburners associated with rotary kilns.

 The  maximum  temperature  in  the afterburner,  1,200°C, represented a practical
 upper  limit  of  the  bench-scale  equipment.   Further,   it  is  a  midrange
 temperature for afterburners as (Frankel et al., 1984).

 A  third  temperature,  650°C,  has  been chosen  as a  minimum  value  for test
 purposes.  This  temperature is consistent with the  low  end of values shown
 for  afterburners.    Further,  it  is at the  low  end of  temperatures where
 99.99 percent  ORE  for hazardous  organics  is  achieved  (Dellinger  et al.,
 1984).

The third  temperature  provided a matrix of  six points for the establishment
of  time  and temperature  requirements  to  incinerate the  soils.   The  matrix
appears as:

                      	Temperature
       Time

       2 seconds
       5 seconds
Minimum
650°C
650°C
Intermediate
900°C
900°C
Maximum
1,200°C
1,200°C
                                      4-2

-------
 4.1.3  Oxygen Concentration

 Oxygen concentration determines the  level  of excess air  that  is optimal in
 firing the  supplementary  fuel.   Oxygen  concentration  was  varied in  the
 carrier gas as a  means  of making the  bench-scale  tests most representative
 of the postflame oxidation regions as  well  as  the  pyrolysis region.  Oxygen
 concentration influences  not  only  the temperatures  achieved  in  the  flame
 (see,   for  example,  Babcock  and  Wilcox,  1978,  for  a correlation  between
 excess CL  and  flame  temperature),  but  also  influences  the  degree  of
 combustion completeness and the minimization of PIC formation.

 The  research  previously  cited  demonstrates  (Kramlich et al., 1984) that PICs
 are  minimized and  DREs are maximized with excess air in the 30 to 40 percent
 range.  Below and  above  that  range,  PICs increase in dramatic quantities, as
 is shown in Figure 4.1-1.

 The  minimum   concentration  of  0_   in  the  exhaust  gas  was   selected  at
 5.4  percent,   corresponding  to   the  apparent  optimal  value   shown  in
 Figure  4.1-1.  This  level was set for the carrier gas in the experiment.

 The  maximum  concentration of 0.  in  the exhaust gas was  set at 7.0 percent,
 corresponding  to  common  firing  practices  of  many  combustion  systems.
 Further, this  representation of 50 percent excess air represented a practical
 upper  limit  beyond which  ORE  levels of 99.99  percent  could not be expected
 (see,  for example, Figure 4.1-1).

 4.2  ANALYTICAL PARAMETERS MONITORED

 The  analytical parameters monitored  to measure the destruction efficiency of
 each test bum were  twenty-two (22)  semivolatile organic compounds that are
 target  compounds for all RMA field  investigation  programs (Ebasco, 1986b).
 However, only  ten  semivolatile compounds (Aldrin, Dieldrin, Endrin, Isodrin,
DCPO, DBCP, CPMS,  CPMSO,  CPMS02 and  Supona)  were detected in the  overburden
 sample  through baseline  analyses  (see Table  2.4-4).  These  ten  compounds
were selected  as  PHOCs.   The analytical method employed for feed  sample was
                                      4-3

-------
     ^2000
ft
o
I/t
0)

5 1500

S
o
       1000
     
-------
gas chromatography-mass  spectrometry (GC/MS) at full  scan,  while for better
sensitivity GC/MS  Selective Ion Monitoring  (SIM)  mode was  used  for residue
and off-gas samples.

-------
                               5.0  TEST RESULTS
 5.1  SUMMARY

 Initially, 25 test burns were conducted on overburden and surrogate samples.
 Six  test  burns  were  aborted due to equipment malfunction.  Three of the test
 burns were conducted on  surrogate  compounds  to demonstrate the efficiency of
 the  sampling trains.  The  remaining test burns were successfully completed;
 Table 5.1-1 presents the test matrix for these 16 successful runs.

 Analyses  for  the 10  selected  POHCs  indicated  complete  (more that  99.99
 percent)  destruction of  organics associated  with  Basin F overburden material
 at  most  of  the test  conditions.   Further  evaluation of selected  runs for
 PICs resulted  in the  selection  of preliminary optimum combustion conditions
 for  the  complete  destruction  of  organics.   Two additional  test  burns of
 overburden  sample  were  conducted  at  these  optimum  conditions   and  upon
 evaluation of  identified PICs in  off-gases  from  these two optimization test
 runs,  the  optimum  combustion   conditions  were  selected  for  a full-scale
 incineration system  concept design.

 5.2  FEED SAMPLE ANALYSES

 The  feed  sample  (overburden  from  Basin F)  for each  test  burn was analyzed
 for 22  semi-volatile organic  compounds (target compounds) by GC/MS  full  scan
 analytical  method  as  certified  by  USATHAMA.   Appendix  A   contains  the
 analytical  results  as reported by the  laboratory  (Hittman-Ebasco),  while
 Appendix B contains the chemical structure of each of  the 22 compounds.

 A summary of results of the feed sample analyses  is presented  in Table 5.2-1.
 The  table identifies  parameters  that were  reported  to have  concentrations
 higher  than their respective  analytical detection   limit.   The parameters
 identified in Table  5.2-1  are Aldrin,  Dieldrin, Endrin, Isodrin, DCPD,  DBCP,
CPMSO,  CPMSO- and Supona.
                                      5-1
2306E

-------
TABLE 5.1-1
TEST MATRIX
Test
Run
2
3
5
6
7
8
9
10
11
12
13
14
17
18
19
20
Temp «C
in
Primary
Burner
900
900
900
650
900
650
900
900
650
900
900
650
650
650
800
800
Tenp *C
in
Secondary
Burner
1200
900
1200
650
900
1200
900
1200
650
900
1200
650
650
900
900
900
Detention
Time (min)
in Primary
Burner
At Operating
Temo.
60
60
60
60
60
60
60
60
60
60
60
60
30
60
30
15
Detention
Time (sec)
in Secondary
Burner
2
2
5
5
5
5
5
2
2
2
2
2
2
2
5
2
0? Level
in
Secondary
Burner
7X
7X
7X
7X
7X
5.4X
5.4X
5.4X
7X
5.4X
5.4X
5.4X
5.4X
5.4X
7X
7X
Type of
Feed in
Primary
Burner
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Remarks
Good
Good
Good
Good
Repeat of Run 4; Good
Good
Good
Good
Good
Good
Good
Good
Good
Good
Test conditions for a
fluidized bed
Test conditions for a
fluidized bed

-------
    TABLE 5.2-1




FEED SAHPLE (ug/gm)
Ttst Run
1
2
3
5
6
7
8
9
10
11
12
13
14
17
18
19
20
Aldrin
AborUd
2200
2100
1700
2400
2300
1900
2300
1700
3600
3700
2300
3600
3100
3500
3900
3700
Dltldrln

1800
1600
1200
1600
1800
1400
1800
1000
1800
1800
1100
1600
1500
1600
1800
2800
Endrin

310
350
240
310
330
260
340
170
300
320
200
390
370
400
500
610
Isodrin

240
300
200
110
130
100
130
89
190
180
110
220
180
190
210
180
DCPD

160
170
120
150
110
110
110
59
100
93
70
88
85
140
160
240
DBCP

41
47
33
36
31
28
29
13
23
22
15
20
12
42
48
49
CPUS

2000
1900
1500
2300
2100
2100
2100
1400
2100
2000
1600
1700
2100
2600
2700
2600
CPNSO

120
140
95
51
57
47
47
31
53
53
46
84
100
99
110
91
CPMS02

490
460
360
200
200
170
160
150
270
250
190
310
330
330
360
280
Supona

13
14
13
19
19
15
22
7.8
17
16
11
20
21
22
26
34

-------
 As  can be  seen  from this  table,  the samples used  for test burns were  not
 homogeneous.  The concentration of Aldrin  ranged  from  1700  to  3900 ppm while
 Oleldrin  ranged  from 1000 to 2800 ppm. Among  Endrin,  Isodrin,  and DCPD,  the
 concentrations ranged from  170 to 610 ppm, 89  to  300 ppm, and 59 to 240 ppm,
 respectively.  Among the chlorophenylmethyl sulfur  compounds, CPMS had  the
 highest concentration for each  test  burn  from 1400  to 2700 ppm.   Concentra-
 tions  of  OBCP  and  Supona were  found  in the  range  of  7.8 to 49  ppm,
 respectively.

 5.3  RESIDUE ANALYSES

 Residue remaining  after each test burn  was analyzed  for all  target  organic
 compounds  to  determine the completeness  of organic volatilization from the
 feed  samples.    The  GC/MS-SIM  mode   was   employed  for  analyses   of  organic
 compounds.   Results  of analyses  of  residue  samples,  as  reported  by  the
 laboratory, are presented in Appendix A.

 A summary of results of  these  analyses is presented  in Table 5.3-1.   Table
 5.3-1  shows those 10 parameters  that were detected  in  feed  samples,  i.e.,
 Aldrin,  Dieldrin,  Endrin,   Isodrin,  DCPO,  DBCP,  CPMS, CPMSO,   CPMS02  and
 Supona.  As can  be seen from this  table,  almost all organics associated with
 the  overburden  samples  were volatilized under  test  conditions (650°C  -
 900°C).

 5.4  OFF-GAS ANALYSES

 Off-gases  from the combustion process  was collected  in  the sampling train.
 Off-gas samples  comprised condensates, accumulated  materials  on the filter,
 and materials  absorbed on  carbon  and  XAD-2  resins.   The  analytical method
 employed  for  off-gas samples was  GC/MS-SIM.  Results of  these  analyses as
 reported  by  the  laboratory,  are shown in  Appendix  A.  A summary  of results
 of analyses  of off-gas  samples, identifying ten  principal organic compounds
 (i.e., Aldrin,  Dieldrin,  Endrin,  Isodrin, DCPO,  DBCP, CPMSO,  CPMS02, and
Supona) is presented in Table 5.4-1 and Appendix A.
                                      5-2

-------
      TABLE 5.3-1




RESIDUE ANALYSES (ug/gm)
est Run
2
3
5
6
7
8
9
10
11
12
13
14
17
18
19
20
Aldrin
<.05
<.05
<.03
<.03
0.03
0.18
0.05
0.23
3.0
0.05
<0.03
0.07
0.25
0.81
<0.03
<0.03
Dieldrin
0.15
<0.02
0.20
<0.01
<0.01
0.10
<0.01
0.10
2.8
0.03
<0.02
0.04
0.06
0.93
<0.02
<0.02
Endrin
<0.08
<0.08
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
Isodrin
<0.08
<0.08
<0.01
<0.05
<0.05
<0.01
<0.01
<0.01
0.04
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
DCPD
<0.008
<0.008
33
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
DBCP
<0.008
<0.02
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
CPUS
<0.08
<0.08
<0.05
<0.05
<0.05
<0.05
<0.05
0.08
<0.05
<0.05
<0.05
1.1
<0.05
<0.05
<0.05
0.06
CPHSO
<0.08
<0.08
<0.05
<0.05
<0.05
0.06
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
CPHS02
0.25
<0.08
<0.05
<0.05
<0.05
<0.05
<0.05
0.05
4.0
0.87
<0.05
0.10
<0.05
<0.05
<0.05
<0.05
Supona
<0.08
<0.08
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05

-------
                                                                          TABLE  5.4-1





                                                            CONTAMINANTS  REMAINING  IN OFF-GASES (ug)
Test Run
2
3
5
6
7
8
9
10
11
12
13
14
17
18
19
20
Aldrin
21
480
<0.03
<0.03
0.14
<0.03
<0.03
<0.03
<0.03
<0.03
<0.03
0.07
2.0
0.49
0.30
<0.03
DitldHn
23
190
<0.01
<0.01
0.11
<0.01
25
0.36
3.5
<0.01
<0.01
1.2
<0.01
0.25
0.94
0.55
Endrin
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
0.20
3.7
4.6
Isodrin
0.50
8.8
<0.01
<0.01
<0.01
<0.01
0.85
<0.01
<0.01
<0.01
<0.01
0.39
0.39
<0.01
<0.01
<0.01
DCPD
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
08CP
1.1
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
1.8
<0.005
<0.005
CPMS
27
57
<0.05
<0.05
0.13
<0.05
6.44
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
3.8
<0.05
2.0
CPMSO
<0.05
290
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
CPMS02
3.2
<0.05
<0.05
<0.05
<0.05
<0.05
1.94
<0.05
<0.05
<0.05
<0.05
1.4
<0.05
<0.05
<0.15
12
Supona
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
37
<0.05
<0.05
18
<0.05
<0.05
<0.05
<0.05
2306E

-------
As can be seen  from  this  table,  the  organic  species  remaining in  the  off -gas
samples were below the analytical detection  limits most of  the time.   It can
be concluded that  the  original organic compounds present in  the  feed sample
can be transformed into some other species if  not  completely  oxidized to CO,
CCL, and H_0 in the specified test conditions.

5.5  DETERMINATION OF ORE

The  Resource   Conservation  and Recovery   Act  regulation  designates the
destruction  and removal  efficiency  (ORE)  of  principal  organic  hazardous
constituents  (POHC)  as  the  requirement  for   incinerator  design  (Federal
Register, 1981).  The DRE of an incinerator system is defined as:
                          * "out
                         win

where     DRE    =  destruction and removal efficiency, %
          W.     =  mass  feed  rate   of  the  principal  organic  hazardous
                    const ituent(s) to the incinerator
          W  .    =  mass  emission rate  of the  principal  organic  hazardous
           out
                    constituent (s)  to  the  atmosphere  (as  measured  in  the
                    stack prior to discharge).

Thus,  destruction  and removal   efficiency  calculations  are  based  on  the
combined efficiencies of destruction  in  the  incinerator and removal from the
gas  stream  in  the air  pollution  control system.   The potential presence of
principal  organic  hazardous  constituents  in  incinerator  bottom   ash  or
solid/ liquid discharges  from air pollution control devices is not accounted
for  in  the destruction  and  removal  efficiency  calculation  as  currently
defined by regulations.

The  regulations  require  a  DRE  of 99.99  percent   for  all principal  organic
hazardous constituents of  a waste,  unless  it can  be demonstrated  that  a
higher or lower destruction  and  removal efficiency is more appropriate based
on human health criteria.
                                      5-3

-------
Based  on the  concept  described above,  the ORE  of each of  the 10 organic
compounds found  in the  feed  sample was determined.  The mass feed rate of
each organic  compound  was determined by multiplying concentration times the
mass of  feed  sample  used in each test burn. • The total  weight in micrograms
of  each  organic  species  present in  each  feed  sample,  as  reported by the
laboratory,  is included in Appendix A.

Table  5.5-1 presents the  ORE  of 10 principal hazardous  organic constituents
at  all test conditions.   As can be seen from this table, a ORE of more than
99.99  percent was achieved for each POHC at most of the test conditions.

5.6  ANALYSIS OF COMBUSTION RESULTS

To  understand the  observed thermal  decomposition or  stability of organic
species  detected  in  feed  samples,  a  discussion  on the  expected  thermal
stability of detected organic species is presented below.
Aldrin
Aldrin  is  a bridged  chlorinated hydrocarbon.  This  molecule can  undergo  a
very low energy concerted  four-center  elimination of hydrogen chloride (HC1)
(see rxn 1).
                                                                      (rxn 1)
The resulting olefin will have  strained bonds at the site of HC1 elimination
and  be expected  to undergo  further  decomposition.   Four  center concerted
eliminations of HC1 have activation energies  (Efl) on the order of 45-50 kcal/
mole  and  frequency  factors  (A)  of  1013'5  -  1014  s"1  (Benson,  1976).
This  means  that  >99.99  percent  destruction  efficiency  is  expected   for
temperatures  around  600-650°C  at  2.0  seconds  gas  phase  residence  time
(tp).  Since  the reaction is  unimolecular,  the rate will not depend on  the
oxygen  concentration or  the  concentration   of  any  other component  of  the
waste feed.
                                      5-4
2306E

-------
                         TABLE 5.5-1

DESTRUCTION AND REMOVAL EFFICIENCY OF TEN PRINCIPAL HAZARDOUS
          ORGANIC CONSTITUENTS IN OVERBURDEN SAMPLE
Temp Degrees C in
Secondary Burner 650
Temp Degrees C in
Primary Burner 650
Gas Residence Tine in
Second Burner 2
(In Seconds)
Oxygen Level in
Off-Gas (X) 5.4
Run Number 14
17
ALDRIN 100.00
100.00
CPMS 100.00
100.00
CPHSO 100.00
mono
CPMSOo 100.00
100.00
OBCP 100.00
100.00
DCPO 99.99
100.00
OIELDRIN 100.00
100.00
ENDRIN 100.00
100.00
ISODRIN 100.00
100.00
SUPONA 99.74
100. DQ

7
11
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
99.38

5
7
6
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
900
650
2
5.4
18
100.00
100.00
100.00
100.00
99.99
100.00
100.00
100.00
100.00
100.00
800
2
7
20
100.00
100.00
100.00
99.99
100.00
100.00
100.00
100.00
100.00
100.00
5
7
19
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
900
2
5.4
12
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
7
3
99.94
99.99
99.41
100.00
100.00
100.00
99.97
100.00
99.99
100.00
5
5.4
9
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
7
7
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
1200
650
5
5.4
8
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
900
2
5.4
10
13
100.00
IQQ.OO
100.00
IQQ.OO |
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
7
2
100.00
100.00
100.00
100.00
99.99
100.00
100.00
100.00
100.00
100.00
5
7
5
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00

-------
 Dieldrin
 This molecule can also undergo  a  low energy elimination of HC1 (rxn 2).  In
 addition,  the  epoxide linking  is weak  and will  undergo homo lysis  at low
                                                      
-------
 kcal/mole  (Benson  & O'Neal,  1970).   CPMS02  could  undergo the  same  bond
 homolysis although the carbon-sulfur bond would be much stronger in CPMSO-.

 Attack  by radical  species  (hydroxyl  [OH]  in an  oxidative environment  or
 hydrogen  [H]  in  a  pyrolytic  environment)  may  be  the  primary  mode  of
 destruction  through  abstraction of  a  H  on  the methyl  substituent.   The
 authors  are  not  aware  of kinetic  or  mechanistic studies  of attack  on the
 sulfone  group itself.   Destruction at  temperature below  800°C  and 2.0  s
 residence time seem reasonable.
CPMSO (Chlorophenylmethylsulfoxide)
The  authors  are not  aware of  directly  relevant studies  in  the literature.
The same general comments made for CPMSO. would apply to CPMSO.

DBCP CDibromochloropropane)

This  molecule may  undergo a  four  center elimination  of HC1  and hydrogen
bromide  (HBr).   Eliminations of  HBr are  an  even lower  energy  pathway than
HC1  (E   = 40-45  kcal/mole (Benson,  1976).   Consequently, this  molecule is
expected to  be  very unstable forming  several  possible inhalogenated olefins
at temperatures below 600°C.
CPMS (p-Chlorophenylmethylsulfone)

The  sulfur   linkage  in   this   molecule  is   isoelectronic   with  oxygen;
consequently, its behavior  under  thermal  stressing is expected to be similar
to that of an ether linkage.  There  are  no low energy concerted pathways or
weak bonds which would  readily  break upon heating.   Electrophilic addition
of OH  to  the  ring  or abstraction  of H  from  the methyl group  are the most
likely  pathways of  destruction.   This  compound may  be  moderately stable
although it  should  not  be  particularly  difficult to destroy by controlled
incineration.
                                      5-6

-------
Supona

Supona  Is  a relatively complex molecule  with  a number of  functional  groups
that can decompose by various mechanisms.  The  dichlorophenyl  group  would  be
expected to be quite  stable.   The phosphate  ester may  undergo  a  6  center
elimination in analogy to those observed  for normal esters  (Benson & O'Neal,
1970).  The latter type of reaction  can  be quite  rapid  (E. = 47 kcal/mole
            17-1
and  A «  10    s   ),  resulting  in  the  formation   of  the  carboxylic  acid
and an  olefin.   Bond homo lysis may  also  occur at  the  carbon-oxygen linkage
in  Supona.   As a  result Supona may  not be very  stable,  decomposing  below
750°C and 2.0 seconds residence time.

Other Low Level Chlorinated Pesticides (Chlordane.  DDT.  DOE. HCCPD)

Chlordane  and DOT can  undergo low  energy  elimination of  HC1.   DOE  is the
elimination product of DOT and should be considerably more stable (rxn 3).
                                                                      (rxn 3)
DOE will  be  degraded by radical attack  and  probably require temperatures in
excess of 750°C at 2.0 s residence time.

HCCPD  is  a   perchlorinated molecule  and  consequently  cannot  undergo HC1
elimination.    However,  the five  membered  ring is  strained  and  would be
expected  to  break at relatively  low temperatures.   It  should be noted  that
this molecule may react to form the very stable molecule, hexachlorobenzene,
in significant yields.

Other Low Level Phosohonated Pesticides  (Malathion and Parathion)

Parathion may decompose by loss of the nitro group at temperatures  of around
700°C and residence  time  of 2.0 s.  Malathion will likely undergo a 6 center
                                      5-7

-------
elimination at the ester functional group to  form the  corresponding  acid  and
ethylene.  The Malathion decomposition may occur at  less than 700°C.

Other  Low  Level  Contaminants   CDIMP.  DMMP.  Vapona.  Atrazine.  Oxathiane.
Dithiane)

With  the exception of  Atrazine,  each of  these molecules is a  phosphonate.
DIMP  may undergo a 6  center elimination  at  low temperatures;  however,  the
pathway  is  not possible in  DMMP and  Vapona.  Consequently, the  latter  two
compounds may be more stable, although still not extremely stable.

In  Atrazine,   the amine  groups  may   be  susceptible  to  radical  attack  at
intermediate  temperatures  through hydrogen  abstraction or  radical  addition
followed by elimination of the  amine.  Atrazine may be expected to decompose
between 700 and 800°C at 2.0 seconds residence time.

Oxathiane  and Dithiane  are  isoelectronic.   Neither  molecule  contains  any
weak  bonds  which would readily break under  thermal  stressing.   Abstraction
of  H by OH  is   the  most  likely mode  of  destruction.   Both species  are
expected  to be  fairly stable,  although  they  should  represent  no special
problems for the incineration of Basin F wastes.

5.7  ANALYSIS OF PRODUCTS OF INCOMPLETE COMBUSTION

Evaluation of  initial  results of test burns  indicated that the ORE of 99.99
percent  for organic  compounds could  be  achieved  at  all  test conditions.
Since the objective  of multiple  test burns is to determine  the optimum
combustion  conditions  for complete  destruction of organics present  in the
feed  sample,  the  following   assumptions  were   postulated  for  further
evaluation.

     o  Organic  compounds  present  in  the  feed sample  can be  destroyed to
        99.99 percent at test conditions;

     o  Test burns performed  with a 2-second  residence time in  the  secondary
        burner would most  likely fail to destroy  organics  at 99.99 percent
        level; and
                                      5-8

-------
      o  The  most  complete destruction  of organics  shouid produce  minimum
        numbers  and  quantities  of  toxic  PICs.   Therefore,  the  test burn that
        produced the  ieast  number  and  quantities  of toxic PICs  in  the
        off-gas  sample  should  be selected  as  the  run   with  the  optimum
        combustion conditions.

 Based on  these  postulations,  the  off-gas samples  from Runs 12,  13,  and 14
 were  selected for the  analyses of PICs.  GC/MS-SIM mode  was used  for PICs
 analyses  (see Figures  5.7-1  to 5.7-3).   The  results of  these  analyses are
 presented  in  Tables   5.7-1  to   5.7-3.   The  chemical  structures  of  the
 identified PICs  are  provided  in Appendix C.   The compounds (PICs) identified
 were  screened for toxicity characteristics.   Some  compounds were identified
 as  toxic  compounds  (irrespective of  dose or concentration) in accordance
 with  the  Registry of  Toxic  Effects  of  Chemical Substances.   The  greatest
 number  and  yield  were  observed  from  Run  No.  14  with  the   primary  and
 secondary  burners at  only  650°C, while  the  least number  and  yield were
 observed for  Run No. 13 with the  primary  and  secondary burners  at 900°C and
 1200°C,  respectively.   The resulting  toxic  PICs   for  all  three runs  are
 summarized  in  Table 5.7-4.    To  understand  pathways  of  PICs, a  general
 discussion  of  the  mechanism  of  formation of  each  class  of   compound is
 presented.   Specific compounds are discussed when  they  are of particular
 interest.  Non-toxic products are  not addressed.

 Aliphatics and Substituted AliDhatics

 Although not  typically  reported in combustion  studies, simple straight chain
 and cyclic aliphatics (e.g.,  hexane and  methylcyclopentane) may be formed by
 a variety  of radical molecule interactions involving smaller hydrocarbons.
 They  may  also  result  from the  thermal  decomposition of  higher molecular
 weight  hydrocarbons.   The  observed   alcohols,  carbonyls,  and  esters are
 typical partial  oxidation  products for  hydrocarbons  for  temperatures below
450°C.  It is  suspected that the  observed oxidation products may be  forming
 in cool regions  of the  transfer line  in the laboratory combustor.  However,
the authors  cannot absolutely  rule out  the possibility that these products
are formed in the "cool" soil and  escape destruction in the  gas phase.
                                      5-9

-------
           >C017835.8-500.8 *»u. HEfll »4755
400000-


368888-


328888-


288888-


240000-


200900-


160000-


120089-


 600R8-


 40000-


    8-
                        400
                                   680
                                       1208
                                                          1688
                          Jl
                     12     16    28    24     28    32
1 I- "I
36
                                                     48
 067
data file header from :  iC0170
                           Operator: CHUCK
                                        MS
    10/19/86 20:49
    BTL* 2
nple:  HEAI  #4755
be   :
s.  #:     2   MS model:   96  SU/HUi rev.: IA  ALS # :   0
lethod file:  HE9501     Tuning file:  MT9501   No. of extra records:  1
)urce  temp.:   190   Analyzer temp.:   200      Transfer line temp.  : 250
   Chromatographic temperatures :   45.   300.     0.
   Chromat ograph ic times, mm.  :   4.0   10.0    0.0
   Chromatographic rate, deg/min:  10.0    0.0    0.0
                                                  0.      0.
                                                 0.0     0.0
                                                 0.0     0.0
                             Figure  5.7-1
             RECONSTRUCTED ION CHROMATOGRAPH  FOR
             PRODUCTS OF  INCOMPLETE COMBUSTION IN
                     OFF-GASES OF RUN NO. 12

-------
ll« >C ii. . - . »">u. T1C
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data file  header from
>C0223
                          Operator:  CHUCK
                      MS
10x27x86
BTL* 2
•nple:  HEAI #4765
ic   :  Compo; i t e
s.  #:     2   MS model:  96  SLJxHU rev. :  I A  ALS * :  0
Method file: HE9501    Tuning file:  MT9501   No. of extra records:
surce  temp.:  190   Analyzer temp.:   200     Transfer line temp.  :
                                                                 1
                                                                250
   Chromatcgraph ic temperatures :   45.    300.     0.     0.     0.
   Chroma tograph ic times, min.   :   4.0    10.0    0.0    0.0    0.0
   Chromatograph ic rate, deg
-------
       Fii« >coi?i 3s.e-see.e

                                  see
                                             izee
          1606
data file  header  from : >C0171
                          Operator:  CHUCK
MS
rople:  HEAI  #4787
sc   :
5.  *:     2  MS model:  96  SU/HU rev.:  IA   ALS *  :  0
Method file: HE9501    Tuning file:  MT9501    No.  of extra records:
Durce  temp.:  190   Analyzer temp.:   200      Transfer line temp. :
10/19/86  21:39
BTL* 3
                                                                 1
                                                                250
   Chromatographic temperatures :
   Chroma tograph ic times, mm.   :
   Chromatographic rate, deg/min:
45.
4.0
10.0
300.
10.0
0.0
0.
0.0
0.0
0.
0.0
0.0
0.
0.0
0.0
                            Figure  5.7-3
            RECONSTRUCTED ION CHROMATOGRAPH FOR
            PRODUCTS  OF INCOMPLETE  COMBUSTION  IN
                     OFF-GASES OF RUN NO. 14

-------
                                  TABLE 5.7-1

          LIBRARY SEARCH RESULTS OF PRODUCTS OF INCOMPLETE COMBUSTION
                       IN OFF-GAS SAMPLE FROM RUN NO.  12
                                                                Estimated
                                                              Total Amount
    Compound                                                        (ug)
Cyclohexane                                                        1500
Methyl Cyclopentane                                                 620
3-Methyl-2-Butanone                                                 160
Benzene                                                            1200
Hexane                                                             3800
2,2-Dimethyl Hexane                                                 420
Chlorobenzene                                                       250
Hexamethyl Cyclotrisiloxane                                        4700
Octamethyl-Cyclotetrasiloxane                                      5000
Decamethyl-Cyclopentasiloxane                                      4500
Unknown (scan #306 voa) Primary m/z 285                             330
Naphthalene                                                         170
Dodecamethyl-Cyclohexasiloxane                                     1800
Unknown (scan #430 voa) Primary m/z 73                              280
2-Pentadecyl-l, 3-Dioxolane                                         720
Unknown (scan #632 voa) Primary m/z 73                              190
o,o,o-Tris-Trimethyl epinephrine                                    160
Unknown (scan #717 voa) Primary m/z 73                              210
Unknown (scan #795 voa) Primary m/z 73                              180
Sulfur, mol. (S8)                                                   430
Hexanedioic acid, dioctyl ester                                     240
2306E

-------
                                 TABLE 5.7-2


          LIBRARY SEARCH RESULTS OF PRODUCTS OF INCOMPLETE COMBUSTION

                       IN OFF-GAS SAMPLE FROM RUN NO. 13
                                                                Estimated
                                                              Total Amount
   Compound                                                       (ug)
2-Methyl Benzofuran                                                470
Octamethyl Cyclotetrasiloxane                                    13000
Unknown (scan #301) Primary m/z 73                                 160
Oecamethyl Cyclopentasiloxane                                    12000
Unknown (scan #339) Primary m/z 285                               2200
Unknown (scan #355) Primary m/z 293                                160
Unknown (scan #388) Primary m/z 73                                 170
Unknown (scan #401) Primary m/z 73                                 130
Unknown (scan #412) Primary m/z 327                                170
Unknown (scan #423) Primary m/z 73                                 240
Dodecamethyl-Cyclohexasiloxane                                    6500
12-methyl Tetradecanol                                            1200
Unknown (scan #496) Primary m/z 73                                 260
12-methyl-l-Tetradecanol                                          1900
Unknown (scan #569) Primary m/z 64                                 230
N-methyl-5-nitro-2-Pyridinamine                                    260
12-methyl-l-Tetradecanol                                           700
0,0,0-Tris Trimethylsilyl Epinephrine                              360
Unknown (scan #742 voa) Primary m/z 73                             540
3,4-bis[(Trimethylsilyl) oxyl]-Estratrienone                       210
Unknown (scan #820) Primary m/z 73                                 480
Sulfur, mol. (S8)                                                  510
Unknown (scan #891) Primary m/z 73                                 400
Unknown (scan #957) Primary m/z 73                                 360
Silicate anion tetramer                                            330
Silicate anion tetramer                                            260
Unknown (scan #1131) Primary m/z 73                                220
Unknown (scan #1182) Primary m/z 73                                180
3,5-bis (l,l-dimethylethyl)-l,2-Benzenediol                        140
2306E

-------
                                 TABUE 5.7-3


          LIBRARY  SEARCH RESULTS OF PRODUCTS OF INCOMPLETE COMBUSTION

                       IN OFF-GAS SAMPLE FROM RUN NO. 14
                                                                Estimated
                                                              Total Amount
   Compound                                                        (ug)
Cyclohexane                                                        1000
3-Chloro-2-Propenenitrile                                           780
Benzene                                                            1600
Hexane                                                             2800
Unknown (scan #158 voa) Primary m/z 93                              700
Unknown (scan #168 voa) Primary m/z 86                             2200
Tetrachloroethene                                                  5000
Methylbenzene                                                       940
Chlorobenzene                                                      4300
N-ethyl-Cyclohexanamine                                             900
Bromobenzene                                                        570
Hexachloro-1, 3-Butadiene                                          1700
1,4-Dichlorobenzene                                                6600
1,2-Dichlorobenzene                                                3 500
Octamethyl Cyclotetrasiloxane                                       850
l-Bromo-2-Chlorobenzene                                            2400
4-Chloro-Benzonitrile                                              6500
1,3,5-Trichlorobenzene                                             8100
1,2,3-Trichlorobenzene                                             3300
2,6-Dichloro Benzonitrile                                           940
1,2,4,5-Tetrachlorobenzene                                         6000
2,4,6-Trichloro Benzenamine                                         240
5-Bromo-6-methyl-3-(l-methylpropyl)-Pyrimidinedione                 250
2,5-Dichloro-Thiazolopyrimidine                                     790
5,7-Dichloro-Thiazolopyrimidine                                     560
Pentachlorobenzene                                                 1500
4,7-Dichloro-benzo-2,1,3-Thiadiazole                                220
3-Chloro-l,lt-Biphenyl-4-01                                         370
Unknown (scan #611 semi-vol) Primary m/z 241                        300
Hexachlorobenzene                                                   220
Hexachlorodifluoro-Pentadiene                                       270
2306E

-------
                                  TABLE 5.7-4

                      SUMMARY OF OBSERVED TOXIC PRODUCTS
                           OF INCOMPLETE COMBUSTION
Compound
T Primary (°C)
T Secondary (°C)
Run No.

Aliphatics and Substituted Aliphatics
Hexane
Cyciohexane
Methyl cyclopentane
2,2 Dimethyl hexane
Hexanedioc acid, dioctyl ester
12-Methyl-l-tetradecanol
3 Methyl-2-butanone
Olefins
Tetrachloroethene
Hexachloro-1 , 3-butadiene
Aroma tics and Substituted Aromatics
Benzene
Toluene
Benzonitrile
3,5-bis (1,1-dimethyl ethyl) -
1,2 benzenediol
2-Methyl benzofuran
Total Amount
650
650
14


2800
1000
NO
ND
ND
ND
ND

5000
1700

1600
2200
1700

ND
ND
900
900
12


3800
1500
620
420
240
ND
160

ND
ND

1200
NO
ND

ND
ND
fUQ)
900
1200
13


ND
ND
ND
ND
ND
700
ND

ND
ND

ND
ND
ND

140
470
2306E

-------
TABLE 5
.7-4


(Continued)
Compound
T Primary (°C)
T Secondary (°C)
Run No.

Halogenated Aroma tics
Chlorobenzene
1,2 Dichlorobenzene
1,4 Dichlorobenzene
1,3,5 Trichlorobenzene
1,2,4,5 Tetrachlorobenzene
Pentachlorobenzene
Hexachlorobenzene
3-chloro-l,!1 biphenyl-4-ol
4-chlorobenzonitrile
2,6-Dichlorobenzonitrile
Heterocyclics
N-Methyl-5 nitro-2-Pyridinamine
5-Bromo-6-methyl-3-(l-methylpropyl)
pyrimidinedione
Polvnuclear Aromatics
Naphthalene
Other
Sulfur, Mol. (S0)
o

650
650
14


4300
3500
6600
8100
6000
1500
220
370
6500
940

NO
250


NO

NO
Total Amount
900
900
12


420
NO
NO
NO
NO
NO
NO
NO
NO
NO

NO
NO


170

430
fua)
900
1200
13


NO
NO
NO
NO
NO
NO
NO
NO
NO
NO

260
NO


NO

510
2306E

-------
 In either case, none of  these  compounds  are on the EPA's Appendix VIII list
 and represent little cause  for  practical  concern.

 Olefins

 Tetrachloroethene  (PERC)  and hexachloro-l,3-butadiene (HCB) were observed in
 the 640°C run (Run  No.  14).  These  results are  not surprising,  as these
 compounds  have been observed in a number of other laboratory studies  (Taylor
 it Oellinger;  Graham, et  al.,  1986)   Both  PICs  are  expected to  be quite
 stable,  especially PERC.   HCB can easily be formed from the fragmentation of
 Aldrin,  Endrin,  Dieldrin,  Isodrin,  or Supona.  PERC could be formed from the
 fragmentation of essentially any of the  chlorinated  pesticides in the feed.
 Both  compounds have  also been observed  to be  formed  from radical molecule
 reactions  involving  chlorinated  C^  and C2  species  (see  rxn  for example)
 (Taylor  &  Dellinger;  Frenklack  et al., 1983).
 •CC13  (or  -CHC12) + CHC13 (or CC14) -»  C^Cls  +  -Cl                   (rxn 4a)
                                        * HCI
                 C2C13 + C2C1^ -» C^C16  +  Cl                          (rxn Ac)

The  suspected  stability  of PERC  suggests  it  could  be one  of  the more
significant  emissions of chlorinated  compound from the incineration  of Basin
F wastes.
Aromatics and Substituted Aromatics

Benzene  and toluene  (as  well as  other substituted  benzenes  such as  ethyl-
benzene  and styrene)  are frequently observed  major PICs, resulting from  the
combustion  or  pyrolysis  of  most  organics.   They may  be formed  from  the
dechlorination  and  loss of other  functional groups from the ring  structures
of most  of  the chlorinated pesticides  in  the  Basin F waste.  However,  it is
more  likely that they  are formed by  radical molecule  addition and  dispro-
portions! ion reactions  similar to  those shown in rxn 4  (without  the  chlorine
                                      c._ -i n

-------
 substituents)   with   an   additional   reaction  involving   acetylene   or
 methylacetylene (see rxn 5).
                        •C H + C H  -» C H  + H                        (rxn 5a)
                         A 5   22    6 6
                        •CH + CH  -» C H  +  -H                       (rxn 5b)
                         45   34    7 8
 Benzonitrile  can be  formed  by addition  of the nitrile radical  to benzene,
 the  nitrile radical resulting from any number  of  fragmentation reactions of
 nitrogen  containing material  in  the waste feed.  Atmospheric nitrogen is not
 expected  to play a role as  temperatures are  not  high enough to  result in
 degradation of N^.

 The  benzedediol would  seem  to be  the  result of a  low temperature reaction
 either  in a transfer line (or the  soil).  2-Methyl benzofuran, on the other
 hand,  may  result  from either  high temperature gas phase  reactions  or, at
 lower  temperatures, via pathways similar to that proposed  for alcohols and
 carboxylic  acid.   Benzofuran and  methyl benzofuran  have  been  observed in
 significant yields  from  other high  temperature  flow  reactor  oxidations of
 organic waste materials (Graham et  al., 1986).

 Halogenated Aromatics

 A  variety of  halogenated benzenes  were observed  for the low temperature run
 (Run No.  14).   This is not surprising  since chlorinated aromatics have  been
 observed  from pyrolysis and  oxidation of  a number  of chlorinated organics
 (Frenklack, et  al., 1986; Graham,  et al.,  1986).   In fact, the presence of
 chlorine  has  been   shown  to effectively   increase  the  yield  of aromatic
 products  and chlorinated aromatics  (Taylor & Del linger).

 The  lower chlorinated  aromatics  may be  a  result of  bond homolysis of  more
 complex chlorinated species  (e.g.,  CPMSO monochlorobenzene); however, it is
more  likely  that  they  form   by  a  complex  series  of  radical molecule
 reactions similar to  that already  illustrated  for the formation of benzene.
 Chlorine  atom  addition reactions to already chlorinated aromatic  structures
may also  contribute to the  formation of the higher chlorinated aromatics.

                                      5-11

-------
 The  formation  of  chlorinated  benzonitriles  may  proceed through  nitrile
 radical attack on  chlorobenzenes or  chlorine atom attack on benzonitrile.
 The observation  of a  chlorobiphenyl-ol  is  puzzling  since  the chlorinated
 biphenyl is  expected  to  be very  resistant  to  radical attack  and partial
 oxidation  (to  form the  phenol)  without  further fragmentation  to smaller
 species.

 The formation of  chlorobenzenes is important because they have been shown to
 be very stable, especially under pyrolytic conditions, and may be one of the
 most difficult PICs (or  POHCs) to  destroy (Graham et  al.,  1986; Dellinger
 et al.,  1984).

 Heterocyclics

 Two nitrogen containing heterocyclics  were observed,  a substituted pyridlne
 and an  pyrimidinedione.   The formation of the latter species is  puzzling for
 two reasons.   First of all,  it  would  not appear to be  very  stable and is  a
 very complex  species  to  be  formed   requiring  a  very  complex  series  of
 reactions.   The  observed pyrimidinedione  also has a nitro substituent which
 is  expected  to be easily fragmented.   This molecule may have been  formed in
 the transfer line after  the secondary chamber.   In any case,   it should be
 readily destroyed in a full-scale incinerator.

 Pyridine  is  a relatively   stable  aromatic,  expected  to  be  slightly more
 stable than  benzene  (Dellinger  et al., 1984).  No possible direct  precursors
 were identified  in the  waste  feed.   Consequently,  it  is  felt  that this
 molecule was formed through a  radical molecule  addition reaction  involving
 possibly HCN and  butadienyl radical in a manner analogous to that  shown  for
 the  formation of benzene  (rxn 6).
                       •C H + HCN -» C  H N + -H                        (rxn 6)
Polynuclear Aromatics
A polynuclear  aromatic hydrocarbon  such as naphthalene  may be formed  as an
extension of mechanism responsible  for  benzene.   A possible mechanism  would
                                      5-12

-------
 be through a  styrene intermediate  formed from the  reaction of  butadienyl
 radical  and vinyl acetylene radical (see rxn 7).
              CH,- CH - CH - CH. + CH - C - CH - CH
    U
&
                       CH . CH.

                             4 CH . CH
                                                                     (rxn 7b)
 It  is not  difficult  to envision  a  continuation of this  process (involving
 another  vinyl  acetylene  instead  of  acetylene)  to  form higher  molecular
 weight PNAs.

 In  fact,  it  is  surprising  that  other  PNAs  were  not  reported.   Other
 laboratory  studies have  shown  that PNAs  can be  the major  PIC  at  higher
 temperatures  even under  oxidative  conditions (Graham, et  al.,  1986)   The
 observation  of chlorinated benzenes without the  observation  of chlorinated
 PNAs  is  also quite puzzling.  In  fact,  as  already discussed,  chlorine atoms
 are implicated in catalyzing the  formation  of aromatics,  PNAs,  and soot due
 to  their  ability to abstract  hydrogen  atoms  and  initiate  the  reaction
 sequences shown  in reactions 3, 4,  5, and  6 (Taylor & Dellinger; Frenklack,
 et al., 1983).

 Other Emissions

Elemental  sulfur  (S_)  was  observed  under all  of  the  conditions tested.
                    o
These species have also been observed from the thermal degradation of sulfur-
containing materials  (Taylor &  Dellinger).  Elemental  sulfur is apparently
stable enough to  resist  oxidation  at  the temperatures  and  oxygen levels
studied.   The authors are not aware  of any concern by EPA over its emission.
                                     5-13

-------
5.8  OPTIMUM COMBUSTION CONDITIONS

Conditions at which Run No.  13  was  conducted have been chosen as the optimum
combustion  conditions  for  achieving  ORE   of  99.99  percent  for  Basin  F
contaminated soils.  Run No. 13 was conducted at the following conditions:

        Temperature in the Primary Burner           900°C
        Temperature in the Secondary Burner        1200°C
        Gas Residence Time in the Secondary Burner    2 seconds
        Oxygen Level in Off-Gases                   5.4 percent

Reasons  for  selecting  the  above  conditions  as  the  optimum  combustion
conditions are discussed in previous subsections.  Primarily, these operating
conditions are  chosen because  in Run  No.  13 ORE  of  99.99  percent  for all
detected organic  compounds and  least numbers and  quantities of  toxic PICs
were observed  amongst the  test runs that  were considered  to  represent the
failure (i.e., not achieving appropriate ORE) conditions.

Furthermore,   the  measurements   of  the  carbon  monoxide  (CO)  concentration
levels  in  the off-gases  indicated  the most complete combustion  of organic
contaminants.  The concentration of  CO in  the  incinerator  off-gases  is an
indicator  for  PIC and  POHC emissions  (Lee & Huffman,  1984).  That  is, if
significant CO emissions are not present,  the presence of other carbon-based
pollutants would be highly unlikely.  Conversely, the presence of  significant
levels  of  CO in the  combustion products would  indicate that the conditions
in  the  incinerator   are  improper  and  may  result in  POHC  and  other PIC
emissions.

Figures 5.8-1, 5.8-2  and 5.8-3  represent  the CO levels observed in  off-gases
for Run Nos. 12, 13,  and  14.   The graphs were plotted CO  levels in  off-gases
versus  temperatures   in  the  primary burner.   The  least  amount  of  CO was
observed during Run No. 13 test  burn period.
                                     5-14

-------
RUN  #  12  TASK  17
       CSI 1001 - 017
coo -
soo -
30O -
200 -
100 -

o -
«.
1
1









I


^
"L^ ^ 	 	 - - 	 	 
-------
C
 1


0.9 -


o.e -


0.7 -


0.6 -


0.5 -


0.4 -


0.3 -


0.2 -


0.1  -


 o
                    RUN  #   13  TASK  #17
                             ESI 1001-107
              0.2
                              I
                             0.4        % 0,6
                                 (7he»w sends.'
                          P.*. k'ART  TtM^fctTURE (C)
0.6
                          Figure 5.8-2
                   CONCENTRATION OF CO IN
                   OFF-GASES OF RUN NO. 13

-------
0.5 -
               RUN  #  14  TASK #17
                           1001-1O7
                  200
 i
400
                                                     II

                                                     (I
600
                    HtVAHT 7EK«*E«:iTUK£ (C)
                         Figure 5.8-3
                  CONCENTRATION OF CO IN
                  OFF-GASES OF  RUN NO. 14

-------
 5.9  OPTIMIZATION RUNS

 Two additional test burns  were  conducted at these  optimum  conditions,  with
 the exception of Run No.  2 which utilized 50 percent  excess  air (7 percent
 0- in  the  off-gases)  for  the  purpose of  determining  the effect  of excess
 oxygen  on the formation of products  of  incomplete  combustion.  It was found
 in the  literature  that  the yield  and  stability  of  PICs  increase  with
 decreased oxygen concentration  (Graham,  et  al.,  1986).  Figures  5.9-1  and
 5.9-2 depict reconstructed ion  chromatograms of observed PICs  in off-gases
 of the  optimization  test   runs.   Table  5.9-1  presents  the  comparative
 evaluation  of these two PIC  analyses.   It can be seen  from  this table that
 the test run  with 7  percent oxygen  level produced the least  numbers  and
 quantities  of products  of  incomplete combustion.   Off-gas samples were not
 analyzed  for the target organic compounds.

 5.10  EP  TOXICITY OF RESIDUE

 EP toxicity tests  were  performed  on the  feed  and  residue   samples  of the
 optimization Run No.  1.   The results of  the  toxicity tests are indicated on
 Table  5.10-1.   No  organic  parameters in  EP  leachate were  analyzed because
 the residue samples from all test burns consistently  showed  target organic
 compounds  below  the analytical   detection  limits.  Moreover,   for organic
 analyses, residue  samples  were extracted  using  methylene chloride  solution.
 Therefore,  it is assumed that no  organics can be detected in  the EP extract.
 The  EP toxicity  test on  the  feed  sample  was  performed to determine the
 mobility  of toxic  metals  present  in Basin  F  soils   and  any  effects the
 incineration process would have on the behavior of these  toxic metals.

 It  can be  seen from  Table  5.10-1  that  the toxic metal  concentration in
 neither  extract exceeded  the  EP  Limit  concentrations.  Moreover,  it was
 observed  that  arsenic was  not reported  to be  present  in the  feed  extract
while small amount of arsenic leached out from the residue sample.

5.11  LIQUID TEST BURN RESULTS

      (Later)
                                     5-15

-------
Fil« >VN119  46.0-460.0 *»u.



100000*


 90000*


 •0000*


 70000*


 60000*


 60000*


 40000*


 30000*


 20000*


 10000*

                                            Full

                                          1200
     1680
                                  32
                                            36
                    12 '  16  '  20  '  24   '  20  '  32  '  3*  '  40
data file header from :  >UN119
                           Operator:  CHUCK
MS
                                                    11/19/66  2:42
                                                    BTL*12
pie:  HEAI  $6866
c  :  Fu 11
. *:     2   MS model:   96   SU/HU rev.:  IA   ALS  *  :   0
ethod file:  HE9503     Tuning  file:  MT9501   No.  of  extra  records:   1
jrce  temp.:   190   Analyzer  temp.:   200     Transfer  line temp.  :
   Chroma tographic  temperatures  :   49.    300.      0.
   Chrometographic  times,  min.   :   4.0    10.0     0.0
   Chromatogrephic  rate, deg/min:  10.0     0.0     0.0
          0.     0.
         0.0    0.0
         0.0    0.0
                             Figure 5.9-1
             RECONSTRUCTED ION CHROMATOGRAPH FOR
             PRODUCTS OF  INCOMPLETE COMBUSTION  IN
             OFF-GASES OF  THE OPTIMIZATION  RUN NO. 1

-------
          >VN126 46.0-460.0 A»u. MEHI •6876
«f«
                                            Full

                                          1266
                                                    1«66
       866666-
       766666-
       66666
       666666-
       486086-
       36eeee-
       zeeooo-
       160666-
lata file header from : >UN120
                                                          11x19/86  3:32
                                                          BTL*13
ile: HEAI *687f            Operator: CHUCK     MS
:   : Fu 1 1
 *:    2  MS model:  96  SU/HU rev.: IA  ALS * :  0
thod file: HE9503    Tuning file: MT9501   No. of extra records:   1
irce temp.:  190   Analyzer temp.:  200     Transfer line temp. :  250
                   •
  Chromatographic temperatures :   45.   300.     0.     0.      0.
  Chromatographic times, min.  :   4.0   10.0    0.0    0.0    0.0
  Chromatographic rate, deg/min:  10.0    0.0    0.0    0.0    0.0
                             Figure 5.9-2
             RECONSTRUCTED ION CHROMATOGRAPH FOR
             PRODUCTS OF  INCOMPLETE COMBUSTION IN
             OFF-GASES OF  THE OPTIMIZATION RUN NO. 2

-------
                                  TABLE 5.9-1

            SUMMARY OF IDENTIFIED PRODUCTS OF INCOMPLETE COMBUSTION
                  IN OFF-GAS SAMPLES OF TWO OPTIMIZATION RUNS
Compound
T Primary (°C)
T Secondary (°C)
02 (X)
Optimization Run No.

Octamethyi Cyclotetrasiloxane
1 , 2-Dichlorobenzene
Tetramethyl Pentane
1, 2, 3-Trich lorobenzene
Chloro-4-(methylthio)-Benzene
Dodicamethyl Cyclohexasiloxane
Tetrachlorobenzene
Pent ach lorobenzene
12-Methyl-l-Tetradecanol
4-Methoxy-Benzoic acid Trimethylsilyl ester
Tetrachloro-5-dichloromethylene-Cyclopentadiene
Isocyano-Naphthalene
Pentadecyl-1, 3-Dioxolane
Ethyi-Indolecaiboxylic acid ethyl ester
Ethyl-methyl-Pyridinethione
Benzeneacetic acid
Sulfur, mol (S8)
Total Amount
900
1200
5.4

1

25,000
1700
540
1900
12,000
8800
3000
3700
4000
670
770
640
710
NO
NO
NO
1600
Estimated fuo")
900
1200
7

2

ND
NO
NO
ND
ND
8700
ND
ND
1000
760
ND
NO
640
6200
2200
2200
5000
2306E

-------
                                 TABLE 5.10-1


                           EP TOXICITY TEST RESULTS
                EP Limit
         Concentration (mg/L)    Feed Samples (mg/1)    Residue Sample (mg/1)
As
Ba
Cd
Cr
Pb
Hg
Ag
Se
5.0
100.0
1.0
5.0
5.0
0.2
5.0
1.0
0
0.212
0
0.017
0.098
0.020
0.043
0.273
0.081
0.200
0
0.037
0.033
0.020
0.040
0.268
2306E

-------
                          6.0  SUMMARY  AND  CONCLUSIONS
 The data generated in the  laboratory  tests thus far conducted indicate that
 the toxic  organics  identified in the  Basin F soil  samples  are  amenable to
 incineration.   The  data  suggests  that  a ORE  of  >99.99  percent  can  be
 achieved at relatively  low  reactor  temperatures (650°C), a  total gas phase
 residence  time   of   approximately  7.0   seconds,   and  flue   gas   oxygen
 concentrations of 5-7 percent.  Examination of the  available literature and
 consideration   of chemical  kinetic  principals  suggest  that most  of  the
 identified  toxic  organics are  thermally fragile and easily decomposed.

 The sulfone and  sulfoxide  compounds (CPMS02, CPMSO, and  CPUS)  appear, from
 a  theoretical  standpoint,   to be  the most stable  toxic  compounds  in  the
 waste.    Oxathiane and  Dithiane,   which   are  basically  hydrocarbons  with
 thioether and  ether  linkages, are  also expected  to be  moderately  stable.
 However,  it   is  felt  that none  of  these  materials  represent  a  special
 challenge to available incineration  technologies.

 Analysis  for products of  incomplete combustion  indicated that  a number of
 chlorinated and nonchlorinated products were  formed  during  the low tempera-
 ture  test  runs.   At  higher  temperatures,  these compounds  appeared  to be
 destroyed and  only a  few products  were observed.  The majority of these high
 temperature PICs  were siloxanes and  partially oxidized hydrocarbons (alcohols
 and esters).   Siloxanes may  result  from  the thermal  degradation  of  the
 stationary  phase  GC  columns or sealing  materials containing silicone  rubber
 (such  as GC septa).   In light  of  this,  one must consider  the  possibility
 that  their  observation  is  due to  experimental artifact;  although,  their
 precursor may  also be in  the original  Basin F  sample.  The  alcohols and
 esters  may  have  been  formed  in "cool"  regions  (300-500°C)  of the transfer
 lines of  the laboratory system.

The observation of chlorinated olefins and aromatics in addition  to benzene,
toluene,  and   naphthalene   is  as  expected.   These  compounds   have  been
previously  shown, both  experimentally  and  theoretically,  to  be thermally
stable.   It   is   surprising  that  such   compounds  as  benzene,  toluene,

-------
naphthalene, and  hexachlorobenzene were not  observed  in  the  high  temperature
runs.  They  were  expected due to the extreme  stability  of hexachlorobenzene
and  the  expected  yields  of  the  other three species.  It  is  also surprising
that some chlorinated and nonchlorinated PNAs  were  not observed,  as previous
laboratory  studies have  shown that  they can be  major  products at  higher
temperatures.

One reason for the lack of observation  of  these compounds may have been that
most of  the  off-gas GC-MS  analyses  were  run  in the  selected ion monitoring
(SIM)  mode.   This means  that only a limited  number of  species  (similar  in
structure to the   POHCs analyzed  for in the waste  feed)  would be observed.
Still, these higher molecular weight species  were  not observed  in the full
scan PIC runs.  The high  molecular weight  materials in question (naphthalene
and  hexachlorobenzene)  are  difficult to  transport,  requiring  a  temperature
of 200-250°C to maintain  them in the gas  phase.  If any cold spot exists in
the transfer lines these  species  may  be condensed out and not be observed in
the off-gas analysis.

Consequently,  it  is felt that the  PIC issue for  Basin F  wastes deserves
further study.  Special attention should be paid to being  sure that quantita-
tive  transport of  combustion products   is  assured.    Gas  chromatographic
analysis using a  flame  ionization detector  (FID) should  be employed because
this technique  responds  to a broad  spectrum of  organics,  more completely
identifying the full range  of possible  products.   Mass spectral analysis may
then be  employed   to analyze for specific compounds observed  in the GC/FID
trace  as well as other  suspected  products   of   special  interest  such  as
chlorinated aromatics,  PNAs, benzene, toluene,  and  naphthalene.

In summary,  however, it is concluded  that  Basin F  wastes  are incinerable and
that combustion of these  wastes at the following conditions would result in
the most complete oxidation.

          Primary Kiln Temperature                  900°C
          Afterburner Temperature                 1200°C
          Gas Residence Time in Afterburner           2 seconds
          Oxygen Level in Off-Gases                   7 percent
                                      6-2

-------
                                  APPENDIX A






            ANALYTICAL RESULTS OF FEED,  RESIDUE AND OFF-GAS SAMPLES
2306E

-------
                                 FEED ANALYSES
2306E

-------
                                            H1TTHAM EBASCO Associates

                     Results of Feed Soil Analysis
  COMPOUND

 1) Oxathiane
 2) DCPD
 3) DIMP
 4) DMMP
 5) Dithiane
 6) DBCP
 7 ) Vapona
 8) CPMS
 9) HCCPD
10) CPMSO
11) CPMSO2
12) Atrazine
13) Malathion
14) Aldrin
15) Parathion
16) Isodrin
17)  Supona
18)  DDE
19)  Dieldrin
20)  Endrin
21)  DDT
22)  Chlordane

SURROGATE Recoveries

31)  1,3-Dichlorobenzene-d4
32)  Diethylphthalate-d4
33)  Dloctylphthalatc-d4
54)  Chlorophenol-d4
                               HEAI*
                               4338
<0.9
 160
<0.8
<0.8
<0.3
  41
<0.6
2000
<0.3
 120
 490
<3.0
<0.4
2200
<0.6
 240
  13
<0.9
1800
 310
<0.3
<2.0
  90
 114
 126
  86
             HEAI*
             4339
                 ug/g
<0.9
 170
<0.8
<0.8
<0.3
  47
<0.6
1900
<0.3
 140
 460
<3.0
<0.4
2100
<0.6
 300
  14
<0.9
1600
 350
<0.3
<2.0
  76
  96
  81
  72
             HEAI*
             4340
<0.9
 130
<0.8
<0.8
<0.3
  35
<0.6
1800
<0.3
 110
 460
<3.0
<0.4
2100
<0.6
 250
  15
<0.9
1500
 270
<0.3
<2.0
  75
 119
 100
  67
             HEAI*
             4341
<0.9
 120
<0.8
<0.8
<0.3
  33
<0.6
1500
<0.3
  95
 360
<3.0
<0.4
1700
<0.6
 200
  13
<0.9
1200
 240
<0.3
<2.0
  72
 102
  78
  63

-------
                                            HITTMAN EBASCO Associates

                     Results of Feed Soil Analysis
  COMPOUND

 1) Oxathiane
 2) DCPD
 3) DIHP
 4) DNMP
 5) Dithiane
 6) DBCP
 7) Vapona
 8) CPMS
 9) HCCPD
10) CPMSO
11) CPHSO2
12) Atrazine
13) Malathion
14) Aldrin
15) Parathion
L6)  Isodrin
17)  Supona
L8)  DDE
L9)  Dieldrin
20)  Endrin
21)  DDT
22)  Chlordane

SURROGATE Recoveries

51)  1,3-Dichlorobenzene-d4
52)  Diethylphthalate-d4
53)  Dioctylphthalate-d4
54)  Chlorophenol-d4
HEAI*
4342
run 6

HEAI*
4343
run 7
ug/g
HEAI*
4344
run 8

HEAI*
4345
run 9

<0.9
150
<0.8
<0.8
<0.3
36
<0.6
2300
<0.3
51
200
<3.0
<0.4
2400
<0.6
110
19
<0.9
1600
310
<0.3
<2.0
<0.9
110
<0.8
<0.8
<0.3
31
<0.6
2100
<0.3
57
200
<3.0
<0.4
2300
<0.6
130
19
<0.9
1800
330
<0.3
<2.0
<0.9
110
<0.8
<0.8
<0.3
28
<0.6
2100
<0.3
47
170
<3.0
<0.4
1900
<0.6
100
15
<0.9
1400
260
<0.3
<2.0
<0.9
110
<0.8
<0.8
<0.3
29
<0.6
2100
<0.3
47
160
<3.0
<0.4
2300
<0.6
130
22
<0.9
1800
340
<0.3
<2.0
140
 68
136
124
121
 74
158
106
125
 70
130
111
102
 64
158
 97

-------
                       HITTMAN EBASCO Associates

Results of Feed Soil Analysis
 COMPOUND

.) Oxathiane
!) DCPD
I) DIMP
-) DMMP
0 Dithiane
 ) DBCP
 ) Vapona
 ) CPMS
 ) HCCPD
 ) CPMSO
 ) CPMS02
 ) Atrazine
 ) Malathion
 ) Aldrin
 ) Parathion
 ) . Isodrin
 ) Supona
 ) DDE
 ) Dieldrin
 ) Endrin
 ) DDT
 ) Chlordane

RROGATE Recoveries

 ) 1,3-Dichlorobenzene-d4
 ) Diethylphthalate-d4
 ) Dioctylphthalate-d4
 ) Chlorophenol-d4
          HEAI*
          4346
          runftlO
          92
          64
          95
         102
 HEAI*
 4347
 runail

 ug/g
 88
 62
 85
105
 HEAI*
 4348
 run«12
<0.9
59
<0.8
<0.8
<0.3
13
<0.6
1400
<0.3
31
150
<3.0
<0.4
1700
<0.6
89
7.8
<0.9
1000
170
<0.3
<2.0
<0.9
100
<0.fr
<0.8
<0.3
23
<0.6
2100
<0.3
53
270
<3.0
<0.4
3600
<0.6
190
17
<0.9
1800
300
<0.3
<2.0
<0.9
93
<0.8
<0.8
<0.3
22
<0.6
2000
<0.3
53
250
<3.0
<0.4
3700
<0.6
180
16
<0.9
1800
320
<0.3
<2.0
 84
 68
101
100

-------
                                           HITTMAN  EBASCO  Associates

                   Results  of  Feed  Soil Analysis
 COMPOUND

L)  Oxathiane
>)  DCPD
J)  DIMP
I)  DMMP
>)  Dithiane
,)  DBCP
')  Vapona
:)  CPMS
')  HCCPD
 )  CPMSO
 )  CPMS02
 )  Atrazine
 )  Malathion
 )  Aldrin
 )  Parathion
 )  Isodrin
 )  Supona
 )  DDE
 )  Dieldrin
 )  Endrin
 )  DDT
 )  Chlordane

RROGATE Recoveries

 )  1,3-Dichlorobenzene-d4
 )  Diethylphthalate-d4
 )  Dioctylphthalate-d4
 )  Chlorophenol-d4
                              HEAI*
                              4349
                              run*13
<0.9
  70
<0.8
<0.8
<0.3
  IS
<0.6
1600
<0.3
  46
 190
<3.0
<0.4
2300
<0.6
 110
  11
<0.9
1100
 200
<0.3
<2.0
107
107
 94
 95
 HEAI*
 4350
 run*14

 ug/g

<0.9
  88
<0.8
<0.8
<0.3
  20
<0.6
1700
<0.3
  84
 310
<3.0
<0.4
3600
<0.6
 220
  20
<0.9
1600
 390
<0.3
<2.0
 68
101
 88
 73
                         HEAI*
                         4351
                         run*15
<0.9
  95
<0.8
<0.8
<0.3
  24
<0.6
2000
<0.3
  87
 300
<3.0
<0.4
3300
<0.6
 200
  18
<0.9
1700
 390
<0.3
<2.0
 90
110
135
 78

-------
                       HITTHAN EBASCO Associates

Results of Feed Soil Analysis
COMPOUND

L) Oxathiane
!) DCPD
I) DIMP
,) DMMP
.) Dithiane
) DBCP
) Vapona
) CPMS
) HCCPD
) CPMSO
) CPMS02
) Atrazine
) Malathion
) Aldrin
) Parathion
) Isodrin
) Supona
) DDE
) Dieldrin
) Endrin
) DDT
) Chlordane

RROGATE Recoveries

) 1,3-Dichlorobenzene-d4
) Diethylphthalate-d4
) Dioctylphthalate-d4
) Chlorophenol-d4
          HEAI*
          4352
          run#16
           33
           81
          145
 HEAI*
 4353
 run#17

 ug/g
 24
 87
154
HEAI*
4354
run*18
<0.9
100
<0.8
<0.8
<0.3
17
<0.6
2200
<0.3
100
350
<3.0
<0.4
3300
<0.6
180
17
<0.9
1500
390
<0.3
<2.0
<0.9
85
<0.8
<0.8
<0.3
12
<0.6
2100
<0.3
100
330
<3.0
<0.4
3100
<0.6
180
21
<0.9
1500
370
<0.3
<2.0
<0.9
140
<0.8
<0.8
<0.3
42
<0.6
2600
<0.3
99
330
<3.0
<0.4
3500
<0.6
190
22
<0.9
1600
400
<0.3
<2.0
 15
 79
142

-------
                       HITTMAN EBASCO Associates

Results of Feed Soil Analysis
 COMPOUND

I)  Oxathiane
>)  DCPD
5)  DIMP
I)  DMMP
i)  Dithiane
.)  DBCP
')  Vapona
i)  CPMS
i)  HCCPD
>)  CPMSO
 )  CPMS02
 )  Atrazine
 )  Malathion
 )  Aldrin
 )  Parathion
 )  Isodrin
 )  Supona
 )  DDE
 )  Dieldrin
 )  Endrin
 )  DDT
 )  Chlordane

RROGATE Recoveries

 )  1,3-Dichlorobenzene-d4
 )  Diethylphthalate-d4
 )  Dioctylphthalate-d4
 )  Chlorophenol-d4
          HEAI*
          4355
          run#19
                ug/g
         <0.9
          160
         <0.8
         <0.8
         <0.3
           48
         <0.6
         2700
         <0.3
          110
          360
         <3.0
         <0.4
         3900
         <0.6
          210
           26
         <0.9
         1800
          500
         <0.3
         <2.0
          28
          76
         152
 HEAI*
 4356
 run*20
<0.9
 240

-------
                                            HITTHAM EBASCO Associate*
  COMPOUND
 1)
 2)
 3)
 4)
 5)
 6)
 7)
 6)
 9)
10)
11)
12)
13)
14)
15)
    Oxathiane
    DCPD
    DIMP
    DMMP
    Dithiane
    DBCP
    Vapona
    CPMS
    HCCPD
    CPM5O
    CPMS02
    Atrazine
    Malathion
    Aldri-n.
    Parathion
    Supona
    DDE
17)
18)
eoj— Endrin
Zl)  DDT
22)  Chlordane
                     Results of Feed  Soil Analysis
                               HEAI*
                               4338
                               ?UN* 2
  <320
 56000
  <280
  <280
  <100
 14000
  <210
700000
  <100
 42000
170000
 <1000
  <140
770000
  <210
  4600
  <320
0-30OOO
1-000OO'
  <100
  <700
HEAXft
4339
B?l IAJ *t ^
&vn " »
Total
<320
60000
<280
<280
<100
16000
<210
660000
<100
49000
160000
<1000
<140
•740000
<210
VOOOOO
4900
<320
$€0000.
T20DOO
<100
<700
HEAI«
4340
ug
<320
46000
<280
<280
<100
12000
<210
630000
<100
38000
160000
<1000
<140
740000
<210
6604)0-
5200
<320
•520000
94000
<100
<700
                                                                   HEAI«
                                                                   4341
                                                                   Eo«^*r
  <320
 42000
  <280
  <280
  <100
 12000
  <210
520000
  <100
 33000
130000
 <1000
  <140
600000
  <210
 •7 OX) 00
  4600
  <320
420000
 64000
  <100
  <700

-------
                                            HITTMAN EBASCO Associates
                     Results of Feed Soil Analysis
  COMPOUND

 1)  Oxathiane
 2)  DCPD
 3)  DIMP
 4)  DHMP
 5)  Dithiane
 6)  DBCP
 7)  Vapona
 8)  CPMS
 9)  HCCPD
LO)  CPMSO
11)  CPMSO2
.2)  Atrazine
.3)  Malathion
.4)  Aldrin
.5)  Parathion
.6)  Isodrin
.7)  Supona
 8)  DDE
.9)  Dieldrin
:0)  Endrin
11)  DDT
:2)  Chlordane
  020
 52000
  <290
  <290
  <110
 13000
  <220
800000
  <180
 18000
 70000
 <1100
  <140
840000
  <220
 38000
  6600
  <320
560000
110000
  <110
  <720
HEAI*
4343
run 7
Total ug
<320
38000
<290
<290
11000
<220
740000
<180
20000
70000
<1100
<140
800000
<220
46000
6600
<320
630000
120000
HEAI*
4344
run 8

<320
38000
<290
<290
9800
<220
740000
<180
16000
60000
<1100
<140
660000
<220
35000
. 5200
<320
490000
91000
<720
<720
  <320
 38000
  <290
  <290
  <110
 10000
  <220
740000
  <180
 16000
 56000
 <1100
  <140
800000
  <220
 46000
  7700
  <320
630000
120000
  <110
  <720

-------
                                           HITTMAN EBASCO Associates

                    Results of Feed Soil Analysis
 COMPOUND

1)  Oxathiane
2)  DCPD
3)  DIMP
I)  DUMP
5)  Dithiane
>)  DBCP
')  Vapona
5)  CPMS
»)  HCCPD
))  CPMSO
. )  CPMS02
!)  Atrazine
I)  Malathion
,)  Aldrin
>)  Parathion
 )  Isodrin
')  Supona
.)  DDE
1)  Dieldrin
 )  Endrin
 )  DDT
 )  Chlordane
                              HEAI*
                              4346
                              runtflO
             HEAI*
             4347
             run*ll

             Total ug
            HEAI*
            4348
            run*12
<320
21000
<290
<290
4600
<220
490000
<180
11000
52000
<1100
<140
600000
<220
31000
2700
<320
350000
60000
<320
35000
<290
<290
8000
<220
740000
<180
19000
94000
<1100
<140
1300000
<220
66000
6000
<320
630000
100000
<320
33000
<290
<290
7700
<220
700000
<180
19000
88000
<1100
<140
1300000
<220
63000
5600
<320
630000
110000
<720
<720
<720

-------
                                         HITTMAN EBASCO Associates

                  Results  of  Feed Soil Analysis
:OMPOUND

)  Oxathiane
)  DCPD
)  DIMP
I  DUMP
)  Dithianc
I  DBCP
I  Vapona
i  CPUS
I  HCCPD
  CPMSO
i  CPMSO2
  Atrazine
  Malathion
  Aldrin
  Parathi on
  Isodrin
  Supona
  DDE
  Dieldrin
  Endrin
  DDT
  Chlordane
                             HEAI*
                             4349
                             run«13
             HEAI*
             4350
             run«14

             Total ug
            HEAI*
            4351
            run«15
<320
24000
<290
<290
5200
<220
560000
<180
16000
66000
<1100
<140
800000
<220
38000
3800
<320
380000
70000
<320
31000
<290
<290
7000
<220
600000
<180
29000
110000
<1100
<140
1300000
<220
77000
7000
<320
560000
14000
<320
33000
<290
<290
8400
<220
700000
<180
30000
100000
<1100
<140
1200000
<220
70000
6300
<320
600000
14000
<720
<720
<720

-------
                                          HITTHAN EBASCO Associates

                   Results of Feed Soil Analysis
COMPOUND

)  Oxathiane
)  DCPD
)  DIMP
)  DUMP
)  Dithiane
)  DBCP
)  Vapona
)  CPUS
)  HCCPD
)  CPMSO
)  CPMSO2
  Atrazine
  Malathion
  Aldrin
  Parathion
  Isodrin
  Supona
  DOE
  Dieldrin
  Endrin
  DDT
  Chlordane
                             HEAI*
                             4352
                             run*16
             HEAI*
             4353
             run#17

             Total ug
            HEAI*
            4354
            run*lB
<320
35000
<290
<290
6000
<220
770000
<180
35000
120000
<1100
<140
1200000
<220
63000
6000
<320
520000
140000
<320
30000
<290
<290
4200
<220
740000
<180
35000
120000
<1100
<140
1100000
<220
63000
7400
<320
520000
130000
<320
49000
<290
<290
15000
<220
910000
<180
35000
120000
<1100
<140
1200000
<220
66000
7700
<320
560000
140000
<720
<720
<720

-------
                                          HITTMAN  EBASCO  Associates

                   Results  of  Feed  Soil  Analysis
COMPOUND

)  Oxathiane
)  DCPD
)  DIMP
)  DUMP
)  Dithiane
)  DBCP
)  Vapona
I  CPMS
I  HCCPD
I  CPMSO
I  CPMS02
i  Atrazine
!  Malathion
i  Aldrin
i  Parathion
  Isodrin
  Supona
  DDE
  Dieldrin
  Endrin
  DDT
  Chlordane
                             HEAI*
                             4355
                             run#19
             HEAI#
             4356
             run#20
     Total  ug
<320
56000
<290
<290
17000
<220
940000
<180
38000
130000
<1100
<140
1400000
<220
74000
9100
<320
630000
180000
<320
84000
<290
<290
17000
<220
910000
<180
32000
98000
<1100
<140
1300000
<220
63000
12000
<32X)
980000
210000
<720
<720

-------
                               RESIDUE ANALYSES
2306E

-------
                                            HITTMAN EBASCO Associates

                         Results of Residue Analysis
  COMPOUND

  1) Oxathiane
  2) DCPD
  3) CIMP
  4) DHHP
  5) Dithiane
  6) DBCP
  7) Vapona
  8) CPUS
  9) HCCPD
 10) CPMSO
 11) CPMSO2
 12) Atrazine
 13) Malathion
 14) Aldrin
 15) Parathion
 16) Isodrin
 17) Supona
 18) DDE
 L9) Dieldrin
 10) Endrin
 21) DDT
 22) Chlordane

 SURROGATE Recoveries

 51)  1,3-Dichlorobenzene-d4
 52)  Diethylphthalate-d4
53)  Dioctylphthalate-d4
54)  Chlorophenol-d4
                               HEAI*
                               4595
                               run 2
 61
120
 86
 59
             HEAI*
             4602
             run 3
             HEAI*
             4633
             run 4
                  ug/g
 45
112
135
 44
 46
113
 93
 41
             HEAI*
             4647
             run 5
<0.008

-------
                                           HITTMAN EBASCO Associates

                        Results of Residue Analysis
  COMPOUND

 1) Oxathiane
 2) DCPD
 3) DIMP
 4) DHMP
 5). Dithiane
 6) DBCP
 7) Vapona
 8) CPMS
 9) HCCPD
 0) CPMSO
 1) CPMSO2
 2) Atrazine
 3) Malathion
 4) Aldrin
 5) Parathion
 6) Isodrin
 7 ) Supona
 8) DDE
 9) Dieldrin
 0) Endrin
 1 ) DDT
2) Chlordane

URROGATE Recoveries

1) 1,3-Dichlorobenzene-d4
2) Diethylphthalate-d4
3) Dioctylphthalate-d4
4) Chlorophenol-d4
HEAI*
4656
run 6
HEAI*
4667
run 7
HEAI*
4686
run 8
HEAI*
4697
run 9
<0.05
                  ug/g
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
<0.03
<0.05
<0.05
<0.05
<0.03
<0.01
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
0.03
<0.05

-------
                                           HITTMAN EBASCO Associates

                        Results of Residue Analysis
 COMPOUND

1) Oxathiane
2) DCPD
31 DIMP
4) DUMP
5) Dithiane
6) DBCP
7) Vapona
3) CPUS
9) HCCPD
D) CPMSO
L) CPMS02
>) Atrazine
1) Malathion
l) Aldrin
i) Parathion
i) Isodrin
') Supona
I) DDE
» Dieldrin
») Endrin
. } DDT
'.) Chlordane

IRROGATE Recoveries

 )  1,3-Dichlorobenzene-d4
!)  Diethylphthalate-d4
l)  Dioctylphthalate-d4
t)  Chlorophenol-d4
                                  HEAI*
                                  4715
                                  run 10
64
51
50
98
            HEAI#
            4725
            run 11

             ug/g
101
 53
 99
138
             HEAI*
             4753
             run 12
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
0.08
<0.02
<0.05
0.05
<0.05
<0.05
0.23
<0.05
<0.01
<0.05
<0.03
0. 10
<0.05
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
4.0
<0.05
<0.05
3.0
<0.05
0.04
<0.05
<0.03
2.8
<0.05
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
0.87
<0.05
<0.05
0.05
<0.05
<0.01
<0.05
<0.03
0.03
<0.05
<0.05
<0.05
60
55
45
99

-------
                   HITTMAN EBASCO Associates

Results of Residue Analysis
 COMPOUND

1) Oxathiane
2) DCPD
3) DIMP
I) DMMP
5) Dithiane
5) DBCP
7) Vapona
3) CPMS
?) HCCPD
)) CPMSO
L) CPMS02
>) Atrazine
3) Malathion
I) Aldrin
j) Parathion
>) Isodrin
') Supona
!) DDE
)) Dieldrin
)) Endrin
: ) DDT
!) Chlordane

JRROGATE Recoveries

.) 1,3-Dichlorobenzene-d4
>) Diethylphthalate-d4
J) Dioctylphthalate-d4
I) Chlorophenol-d4
          HEAIft
          4763
          run 13
          51
          96
          80
          79
HEAI*
4785
run 14

ug/g
54
97
82
80
HEAI*
4799
run 15
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
<0.03
<0.05
<0.01
<0.05
<0.03
<0.02
<0.05
<0.05
<0.05

-------
                                          HITTMAN EBASCO Associates

                       Results of Residue Analysis
COMPOUND

) Oxathiane
) DCPD
) DIMP
) DMMP
) Dithiane
) DBCP
) Vapona
) CPMS
) HCCPD
) CPMSO
) CPMSO2
) Atrazine
) Malathion
) Aldrin
) Parathion
)  Isodrin
)  Supona
)  DDE
)  Dieldrin
)  Endrin
)  DDT
)  Chlordane

UROGATE Recoveries

)  1,3-Dichlorobenzene-d4
)  Diethylphthalate-d4
)  Dioctylphthalate-d4
)  Chlorophenol-d4
                                 HEAI*
                                 4961
                                 runtflfi
 83
 60
155
 34
             HEAI*
             5155
             runtfl?

             ug/g
45
65
83
48
            HEAI*
            5190
            run*18
0
0
0
0
0
0
0

0
0

0
0

0
0
0
0

0
0
0
.005
.005
.05
.05
.005
.005
.05
17
.02
.05
2.7
.05
.05
16
.05
.27
.10
.03
9.2
.38
.05
.05
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
0
<0
<0
<0
<0
0
<0
<0
<0
.005
.005
.05
.05
.005
.005
.05
.05
.02
.05
.05
.05
.05
.25
.05
.01
.05
.03
.06
.05
.05
.05
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
0
<0
<0
<0
<0
0
<0
<0
<0
.005
.005
.05
.05
.005
.005
.05
.05
.02
.05
.05
.05
.05
.81
.05
.01
.05
.03
.93
.05
.05
.05
 40
 53
149
 39

-------
                                          HITTMAN EBASCO Associates

                       Results of Residue Analysis
COMPOUND
1) Oxathiane
2) DCPD
3) DIMP
4) DMMP
5) Dithiane
6) DBCP
7) Vapona
8) CPMS
9) HCCPD
0) CPMSO
1) CPMS02
2) Atrazine
3) Malathion
4) Aldrin
5) Parathion
6) Isodrin
7) Supona
8) DDE
9) Dieldrin
0) Endrin
1 ) DDT
2) Chlordane
URROGATE Recover
1) 1 ,3-Dichlorob






















ies
enz
2) Diethylphthalate
3) Dioctylphthal
ate
4) Chlorophenol-d4
                                 HEAI*
                                 5247
                                 run#19
                                 60
                                 62
                                 92
                                 66
 HEAI*
 5275
 run*20

 ug/g
 97
 78
105
119
HEAI*
5297
run#21
<0.005
<0.005
<0.05
<0.05
<0.005
(0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
<0.03
<0.05
<0.01
<0.05
<0.03
<0.02
<0.05
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
0.06
<0.02
<0.05
<0.05
<0.05
<0.05
<0.03
<0.05
<0.01
<0.05
<0.03
<0.02
<0.05
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
0.09
<0.05
<0. 01
<0.05
<0.03
0.03
<0.05
<0.05
<0.05
85
70
85
88

-------
                                            HITTMAN EBASCO Associates

                         Results of Residue Analysis
  COMPOUND

 1) Oxathiane
 2) DCPD
 3) DIMP
 4) DHMP
 5) Dithiane
 6) DBCP
 7) Vapona
 8) CPMS
 9) HCCPD
10) CPMSO
ll) CPMSO2
12) Atrazine
13) Malathion
i4) Aldrin
L5) Parathion
16) Isodrin
i7 ) Supona
18) DDE
L9) Dleldrin
JO)  Endrin
51)  DDT
12)  Chlordane
                               HEAI*
                               4595
                               run 2
HEAI*
4602
run 3
HEAI*
4633
run 4
Total ug
                     HEAI*
                     4647
                     run 5
<
<
<
<
<
<
<
<
<
<

<
<
<
<
<
<
<

<
<
<
1.5
1.5
15
15
1 . 5
1 . 5
15
15
5.5
15
46
IS
IS
9.2
15
15
15
9.2
27
15
15
15
<1
<1
<
<
<1
3
<
<

-------
                                            HITTMAN EBASCO Associates

                         Results of Residue Analysis
  COMPOUND

 1) Oxathiane
 2) DCPD
 3) DIMP
 4) DUMP
 5) Dithiane
 6) DBCP
 7) Vapona
 8) CPUS
 9) HCCPD
10) CPMSO
LI) CPMSO2
L2) Atrazine
.3) Malathion
.4) Aldrin
.5) Parathion
.6) Isodrin
.7) Supona
.8) DDE
.9) Dieldrin
10) Endrin
!1) DDT
!2) Chlordane
                               HEAI*
                               4656
                               run 6
HEAI*
4667
run 7

 Total ug
HEAI*
4686
run 8
HEAI*
4697
run 9
<0.78
<0.78
< 7.8
< 7.8
<0.78
<0.78
< 7.8
< 7.8
< 3.1
< 7.8
< 7.8
< 7.8
< 7.8
< 3.1
< 7.8
< 1.6
< 7.8
< 3.1
< 1 ,6
< 7.8
< 7.8
< 7.8
<0.92
<0.92
< 9.2
< 9.2
<0.92
<0.92
< 9.2
< 9.2
< 3.7
< 9.2
< 9.2
< 9.2
< 9.2
5.6
< 9.2
< 1 .8
< 9.2
< 3.7
< 1 .8
< 9.2
< 9.2
< 9.2
<0.90
<0.90
< 9.0
< 9.0
<0.90
<0.90
< 9.0
< 9.0
< 3.6
11
< 9.0
< 9.0
< 9.0
33
< 9.0
< 1 .8
< 9.0
< 3.6
18
< 9.0
< 9.0
< 9.0
<0.83
<0.83
< 8.3
< 8.3
<0.83
<0.83
< 8.3
< 8.3
< 3.3
< 8.3
< 8.3
< 8.3
< 8.3
8.3
< 8.3
< 1.7
< 8.3
< 3.3
< 1.7
< 8.3
< 8.3
< 8.3

-------
                                           HITTHAN EBASCO Associates

                        Results of Residue Analysis
 COMPOUND

1) Oxathiane
2) DCPD
3) DIMP
I) DUMP
5) Dithiane
s) DBCP
7) Vapona
i) CPMS
n HCCPD
)) CPMSO
L) CPMSO2
!) Atrazine
)) Malathion
L) Aldrin
i) Parathion
i) Isodrin
') Supona
I) DDE
i) Dicldrin
i) Endrin
.) DDT
:) Chlordane
                              HEAI*
                              4715
                              run 10
<0.7
<0.7
<7.5
<7.5
<0.7
<0.7
<7.5
  12
<2.6
<7.5
 7.5
<7.5
<7.5
  34
<7.5

<7.5
<3.6
  15
<7.5
<7.5
<7.5
             HEAI*
             4725
             run 11
HEAI*
4753
run 12
                Total ug
<0.7
<0.7
<7.5
<7.5
<0.7
<0.7
<7.5
<7.5
<2.6
<7.5
600
<7.5
<7.5
450
<7.5
6.0
<7.5
<3.6
420
<7.5
<7.5
<7.5
<0.7
<0.7
<7.5
<7.5
<0.7
<0.7
<7.5
<7.5
<2.6
<7.5
130
<7.5
<7.5
7.5
<7.5
<1 . 5
<7.5
<3.6
4.5
<7.5
<7.5
<7.5

-------
                                           HITTMAN EBASCO Associates

                        Results of Residue Analysis
 COMPOUND

1) Oxathiane
2) DCPD
3) DIMP
4) DMMP
5) Dithiane
&) DBCP
7) Vapona
3) CPUS
9) HCCPD
)) CPMSO
I) CPMSO2
2) Atrazine
3) Malathion
I) Aldrin
j) Parathion
>) Isodrin
') Supona
)) DDE
M Dieldrin
)) Endrin
. J DDT
!) Chlordane
                              HEAI#
                              4763
                              run 13
<0
  .7
   7
  ,5
   5
  .7
   7
  .5
   5
  ,6
   5
  ,5
   5
   5
   6
   5
<7.5
<7.5
<3.6
<1 .8
<7.5
<7.5
<7. 5
<7
<0
<7
<2
<7
<7
<7
             HEAI#
             4785
             run 14
                         HEAI*
                         4799
                         run 15
                Total ug
<0.7
<0.7
<7.5
<7.5
<0.7
<0.7
<7.5
160
<2.6
<7.5
15.
<7.5
<7.5
10
<7.5
<7.5
<7.5
<3.6
6.0
<7.5
<7.5
<7.5
<0.7
450
<7.5
<7.5
<0.7
140
<7.5
380000
<2.6
800000
130000
<7.5
<7.5
260000
<7.5
24000
2100
<3.6
330000
12000
<7.5
<7.5

-------
                                          HITTMAN  EBASCO  Associates
                       Results of  Residue  Analysis
COMPOUND

)  Oxathiane
)  DCPD
)  DIMP
)  DMMP
I  Dithiane
I  DBCP
I  Vapona
I  CPUS
i  HCCPD
i  CFMSO
  CPMSO2
  Atrazine
  Halathion
  Aldrin
  Parathion
  Isodrin
  Supona
  DDE
  Dieldrin
  Endrin
  DDT
  Chlordane
HEAI*
4961
run*16
190 gm
HEAI*
5155
run*17
184 gm
HEAI*
5190
run*18
183 gm
Total ug
<0.95
<0.95
<9.5
<9.5
<0.95
<0.95
<9.5
3230
<3.8
<9.5
510
<9.5
<9.5
3000
<9.5
51
19
<5.7
1700
72
<9.5
<9.5
<0
<0
<9
<9
<0
<0
<9
<9
<3
<9
<9
<9
<9

<9
<1
<9
<5

<9
<9
<9
.92
.92
.2
.2
.92
.92
.2
.2
.8
.2
.2
.2
.2
46
.2
.8
.2
.5
11
.2
.2
.2
<0
<0
<9
<9
<0
<0
<9
<9
<3
<9
<9
<9
<9
1
<9
<1
<9
<5
1
<9
<9
<9
.92
.92
.2
.2
.92
.92
.2
.2
.8
.2
.2
.2
.2
50
.2
.8
.2
.5
.7
.2
.2
.2

-------
                                          HITTMAN  EBASCO Associates

                       Results of Residue Analysis
COMPOUND

)  Oxathiane
)  DCPD
)  DIMP
}  DMMP
)  Dithiane
)  DBCP
)  Vapona
)  CPUS
  HCCPD
  CPMSO
  CPMS02
  Atrazine
  Maiathion
  Aldrin
  Parathion
  Isodrin
  Supona
  DDE
  Di eldrin
  Endr i n
  DDT
  Chlordane
HEAI*
5247
run*19
187 gm
HEAI*
5275
run*20
186 gm
HEAI*
5297
run#21
136 gm
Total ug
<0.93
<0.93
<9.3
<9.3
<0.93
<0.93
<9.3
<9.3
<3.7
<9.3
<9.3
<9.3
<9.3
<5.6
<9.3
<1 .9
<9.3

-------
                              OFF-GASES  ANALYSES
2306E

-------
                                            HITTMAN  EBASCO Associates

              Composite of Charcoal, XAD-2,  and  filter
  COMPOUND

 1) Oxathiane
 2) DCPD
 3) DIMP
 4) DUMP
 5) Dithiane
 6) DBCP
 7) Vapona
 6) CPMS
 9) HCCPD
.0) CPMSO
.1) CPMSO2
 2)  Atrazine
 3)  Malathion
 4)  Aldrin
 5)  Parathion
 6)  Isodrin
 7)  Supona
 8)  DDE
 9)  Dieldrin
 0)  Endrin
 1)  DDT
 2)  Chlordane

 URROGATE  Recoveries

1) 1,3-Dichlorobenzene-d4
2) Diethylphthalate-d4
3) Dioctylphthalate-d4
4) Chlorophenol-d4
                               HEAI*
                               4599
                               run 2
<0.005
<0.005
<0.05
<0.05
<0.005
  1.1
<0.05
   27
<0.02
<0.05
  3.2
<0.05
   05
   21
   05
   50
   05
   03
   23
   05
   05
<0

<0
 0.
<0
<0
<0.05
 79
 89
 92
 75
HEAI*
4603
run 3
Total
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
57
<0.02
290
<0.05
<0.05
<0.05
480
<0.05
8.8
<0.05
<0.03
190
<0.05
<0.05
<0.05
%
54
65
106
56
HEAI*
4638
run 4
ug
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
.35
<0.05
<0.05
<0.03
<0.05
<0.01

-------
                                            HITTMAN EBASCO Associates

              Composite of Charcoal, XAD-2, and  filter
  COMPOUND
 1
 2
 3
 4
 5
 6)
 7)
 8)
 9)
 0)
 1)
 2)
 3)
 4)
 51
 6)
 7)
 8)
 9)
0)
 1 )
2)
 Oxathiane
 DCPD
 DIMP
 DMMP
 Dithiane
 DBCP
 Vapona
 CPUS
 HCCPD
 CPMSO
 CPMS02
 Atrazine
 Malathion
 Aldrin
 Parathion
 Isodrin
 Supona
 DOE
 Dieldrin
 Endrin
 DDT
Chlordane
URROGATE Recoveries

1)  1,3-Dichlorobenzene-d4
2)  Diethylphthalate-d4
3)  Dioctylphthalate-d4
I)  Chloroph«nol-d4
                               HEAI*
                               4658
                               run 6
   005
   .005
   .05
   .05
   .005
   ,005
   .05
   05
   .02
   05
   ,05
   .05
   .05
   ,03
   .05
   01
   .05
   03
   .01
<0.05
<0.05

-------
                              HITTHAN EBASCO Associates

Composite of Charcoal, XAD-2, and filter
 COMPOUND

1) Oxathiane
2) DCPD
3) DIMP
4) DMMP
5) Dithiane
6) DBCP
7) Vapona
8) CPUS
9) HCCPD
D) CPMSO
1) CPMS02
2) Atrazine
3) Malathion
1) Aldrin
5) Parathion
5) Isodrin
7) Supona
n DDE
I) Dieldrin
)) Endrin
L) DDT
I) Chlordane

JRROGATE Recoveries

.)  1,3-Dichlorobenzene-d4
n  Diethylphthalate-d4
n  Dioctylphthalate-d4
I)  Chlorophenol-d4
                     HEAI*
                     4717
                     run 10
                    130
                     72
                     80
                    106
 HEAI*
 4727
 run 11

Total ug
107
 52
101
  4
 HEAI*
 4755
 run 12
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
<0.03
<0.05
<0.01
<0.05
<0.03
0.36
<0.05
<0.05
<0.05
< 0.00 5
<0.005
<0.05

-------
                                          HITTMAN EBASCO Associates

            Composite of Charcoal,  XAD-2,  and filter
COMPOUND

) Oxathiane
) DCPD
) DIMP
) DMMP
) Dithiane
) DBCP
) Vapona
) CPUS
) HCCPD
) CPMSO
) CPMSO2
) Atrazine
) Malathion
) Aldrin
) Parathion
) Isodrin
) Supona
) DDE
) Dieldrin
) Endrin
) DDT
) Chlordanc

RROGATE Recoveries

) 1,3-Dichlorobenzene-d4
) Diethylphthalate-d4
) Dioctylphthalate-d4
) Chlorophenol-d4
                                 HEAI*
                                 4765
                                 run 13
59
68
49
58
            HEAI*
            4787
            run 14

           Total ug
107
 26
 48
 56
             HEAI*
             4801
             run 15
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
<0.03
<0.05
<0.01
<0.05
<0.03
<0.01
<0.05
<0.05
<0.05
<0.005
2.9
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
1.4
<0.05
<0.05
0.7
<0.05
<0.01
18
<0.03
-1.2
<0.05.
<0.05
<0.05

-------
                              HITTMAN  EBASCO Associates

Composite of Charcoal,  XAD-2,  and  filter
   COMPOUND

  1) Oxathiane
  2) DCPD
  3) DIMP
  4) DMMP
  5) Dithiane
  6) DBCP
  7) Vapona
  8) CPMS
  9) HCCPD
 10) CPMSO
 11) CPMSO2
 12) Atrazine
 13) Halathion
 14) Aldrin
 15) Parathion
 16) Isodrin
 17) Supona
 18) DDE
 19) Dieldrin
  D) Endrin
**21 ) DDT
 22) Chlordane

 SURROGATE Recoveries

 SI) 1,3-Dichlorobenzene-d4
 52) Diethylphthalate-d4
 S3) Dioctylphthalate-d4
 54) Chlorophenol-d4
                     HEAI*
                     4963
                     run#16
                     37
                     63
                     73
                     33
 HEAI*
 5157
 run*17

Total ug
 37
 88
 73
 29
HEAI*
5192
run*18
<0.005
3.2
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
3.2
<0.05
0.38
0.75
<0.03
<0.01
<0.05
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
2.0
<0.05
0.39

-------
                                            HITTHAN EBASCO Associates

              Composite of Charcoal, XAD-2, and filter
  COMPOUND

  1) Oxathiane
  2) DCPD
  3) DIMP
  4) DUMP
  5) Dithiane
  6) DBCP
  7) Vapona
  8} CPMS
  9) HCCPD
10) CPMSO
11) CPMS02
12) Atrazine
13) Malathion
14) Aldrin
15) Parathion
16) Isodrin
17) Supona
18) DDE
  ") Dieldrin
„,  ) Endrin
21 ) DDT
22) Chlordane

SURROGATE Recoveries

SI) 1J3-Dichlorobenzene-d4
S2) Diethylphthalate-d4
S3) Dioctylphthalate-d4
S4 ) Chlorophenol-d4
HEAI#
5249
run#19
HEAI#
5277
run*20
HEAI*
5300
run#21
47
39
71
63
           Total ug
<0.005
<0.005
<0.05
<0.05
<0.005
0.16
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
0.30
<0.05
<0.01
<0.05
<0.03
0.94
3.7
<0.05
<0.05
<0.005
<0.005
<0.05
<0.05
<0.005
<0.005
<0.05
2.0
<0.02
<0.05
12
<0.05
<0.05
<0.03
<0.05
<0.01
<0.05
<0.03
0.55
4.6
<0.05
<0.05
<0.005
490 "
<0.05
<0.05
<0.005
930 <
<0.05
<0.05
<0.02
<0.05
<0.05
<0.05
<0.05
1500
<0.05
<0.01
<0.05
<0.03
22
<0.05
<0.05
<0.05
61
60
97
91
                              .3
 62
 55
127
 73

-------
                                          HITTMAN E8ASCO  Associates

                            Blank Sample Results
COMPOUND
1)
2)
3)
4)
5)
6)
7)
8)
9)
10)
11)
12)
13)
14)
15)
16)
17)
18)
19)
0)
i)
22)
Oxathiane
DCPD
DIMP
DUMP
Dithiane
DBCP
Vapona
CPMS
HCCPD
CPMSO
CPMS02
Atrazine
Malathion
Aldrin
Parathion
Isodrin
Supona
DDE
Dieldrin
Endr in
DDT
Chlordane
SURROGATE Recover
SI )
52)
S3)
54)




















ies
1 ,3-Dichlorobenzene-d4
Diethylphthalate-d4
Dioctylphthalate-d4
Chlorophenol-d4
                           HEAI QC#
                            0828C
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
                            <0
,005
 005
,05
 05
,005
 005
,05
 05
.02
 05
.05
 05
.05
,03
.05
,01
.05
,03
.01
.05
.05
.05
                               70
                               64
                               88
                               81
             HEAI  QC*
              0902A
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
 005
 005
 OS
 05
 005
 005
,05
 05
.02
,05
.05
.05
.05
.03
.05
.01
.05
.03
.01
.05
.05
.05
                59
                69
                86
                62

-------
                                  APPENDIX B

                CHEMICAL STRUCTURES OF 22 SEMIVOLATILE ORGANIC
                               TARGET COMPOUNDS
2306E

-------
             CROSS REFERENCE TO STRUCTURES OF COMPOUNDS TESTED FOR
                   IN THE BENCH SCALE LABORATORY TEST PROGRAM
 1.   Oxathiane  -  Thioxane, C^sSO.l.A-Oxathiane
 2.   DCPD  -  dicyclopentadlene, C-|QHi2» 3a,4,7,7a-Tetrahydro-
     4,7-methanoindene

 3.   DIMP  -  diisopropylmethylphosphonate,

 4.   DMMP  -  dimethylmethylphosphonate,
 5.  Dfthlane - Nabam, C4HsN2Na2S4, Ethylenebis(dithiocarbamic
    acid)disodium salt
6.  DBCP - Nemagon, dibromochloropropane, Cs^BrgCT, 3-Chloro-l,2-
    dibromopropane

7.  Vapona - dichlorvos, C4H7C12P04 0,0-dimethyl
    0-(2,2-dichlorovinyl phosphate)
8.  PCPMS - p-chlorophenylmethylsulfide,

9.  HCPD - CsCls, hexachlorocyclopentadiene

10. PCPMSO - p-chlorophenylmethylsulf oxide, C7H7C1SO

11. PCPMS02 - p-chlorophenylmethylsulf one,
12. Atrazlne - C8Hi4NsCl, 2-chloro-4-ethylamino-6-isopropylamino-
    s-triazine

13. Malathlon - CioHi906PS2, S - (1-2 dicarbethoxyethyDO.O-
    dimethyldithiophosphate
14. Aldn'n - Ci2HsCl6, ],2,3,4,10,10-hexachloro-l,4,4a,5,8,8a-
    hexahydro-1, 4: 5, 8-dimethano naphthalene
15. Parathlon - CioH^NOsPS, 0,0-dietlyl 0-p-nitrophenyl
    phosphorothioate

16. Isodrin - C^HsCle* l,2,3,4,10,10-hexachloro-l,4,4a,8,8a
    hexahydro-l,4:5,8-endo-dimethanonaphthalene
17. Supona - Chlorfenvinphos, C^H^ClsOs?, 0,0-diethyl 0-[2-chloro-
    l-(2,4-dichlorophenyl)v1nyl J phosphate

18. P.P'-DDE - Ci4HgCl4, l,l-dichloro-2,2-bis-(p-chloropheny1)ethylene
0488D
                                      -1-

-------
              CROSS REFERENCE TO STRUCTURES OF COMPOUNDS TESTED FOR
             IN THE BENCH SCALE LABORATORY  TEST  PROGRAM  (Continued)
 19.  Dfeldrin - C^HsCls0*  1, 2,3,4, 10,10-hexachloro-6, 7-epoxy-
     l,4,4a,5,6,7,8,8a-octahydro-l,4,5,8-dimethanonaphthalene
 20.  Endrln - C^gHsCleO,  1,2, 3,4,10, 10-hexachloro-6,7-epoxy,
     l,4,4a,5,6,/,8,8a-octahydro-endo-endo-l,4:5,8-dimethanonaphthalene

 21.  P.P'-DDT - dlchloro  diphenyl trichloroethane
     l,l,l-trichloro-2,2-bis(p-chlorophenyl)ethane
 22.  Chlordane  -  Cio^Cls.  1,2,4,5, 6,7, 8,8-octachloro-4,7, methane-
     3a,4,7,7a-tetrahydroindane
0488D
                                      -2-

-------
' 1
         0
CHo
    HoC-P-0-C-H
     '
         0
    H3C-C-CH3
         H
                0
                0
                        H-C
                           IH
                C- C-CI
                Br  (I

-------
   0
 O=P-O
   0
   CH3
  ___ /" —i—
Cl
c
Cl
                  8
                    s
                  xk,
                  "t
                    Cl
Cl
Cl
Cl
Cl
                 10

                  12
                            N
                        V
                          ty
                        H-C-CH3

-------
81

            II
            0
Z.T
        H
91
SI
               >0
             OH
                      £,.

-------
zz
IZ
                   61

-------
                                  APPENDIX C

           CHEMICAL STRUCTURES OF IDENTIFIED PRODUCTS OF INCOMPLETE
             COMBUSTION IN OFF-GASES FROM RUN NOS. 12, 13, AND 14
2306E

-------
             '                      ALPHABETIZED CROSS-REFEREN/
                                      OF PRODUCTS OF INCOMPLETE
1.    Benzene
2.    Benzeneacetlc acid
3.    Benzonltrlle
4.    3,5-bls (l,l-din)ethylethyl)-1,2-Benzenediol
5.    3,4 bis [(Tr1m1ehyl1s11y)oxyl]  - Estratrienone
6.    Bromobenzene
7.    l-Bromo-2-Chlorobenzene
8.    5-Bromo-6-methyl-3-(l-methylpropyl)-Pyrimidinedione
9.    Chlorobenzene
10.   4-Chloro-Benzonitrile
11.   3-Chloro-l,r-B1phenyl-4-Ol
12.   Chloro-4-(methylthio)-Benzene
13.   3-Chloro-2-Propenenitrile
14.   Cyclohexane
15.   Decamethyl-Cyclopentasiloxane
16.   1,2-Dichlorobenzene
17.   1,4-Dichlorobenzene
18.   2,6-Dichlorobenzonitrile
19.   4,7-D1chloro-benzo-2,l,3-Thiadiazole
20.   2,5-Dichloro-Thiazolopyrimidine
21.   5,7-Dichloro-Thlazolopyrimidine
22.   2,2-Dimetnyl Hexane
23.   Dodecamethyl-Cyclohexasiloxane
24.   Ethyl-Indole carboxyllc acid ethyl  ester
25.   Ethyl-methyl-Pyrldinethione
26.   Hexachlorobenzene
27.   Hexachloro-l,3-Butadiene
28.   Hexachlorodifluoro-Pentadiene
  T0 THE STRUCTURES
-JMBUSTION (PICs)
  29.   Hexamethyl Cyclotrisiloxane
  30.   Hexane
  31.   Hexanedioic acid, dioctyl ester
  32.   Isocyano-Naphthalene
  33.   4-Methoxy-Benzoic acid Trimethylsilyl ester
  34.   Methylbenzene
  35.   2-Methyl Benzofuran
  36.   3-Methyl-2-Butanone
  37.   Methyl Cyclopentane
  38.   12-methyl Tetradecanol
  39.   12-methyl-l-Tetradecanol
  40.   N-ethyl-Cyclohexylamine
  41.   N-methyl-5-n1tro-2-Pyridinarnine
  42.   Naphthalene
  43.   Octamethyl Cyclotetrasiloxane
  44.   Pentachlorobenzene
  45.   Pentadecyl-l,3-Dioxolane
  46.   2-Pentadecyl-l,3-Dioxolane
  47.   Silicate anion tetramer
  48.   Tetrachlorobenzene
  49.   1,2,4,5-Tetrachlorobenzene
  50.   Tetrachloro-5-dichloromethylene-Cyclopentadiene
  51.   Tetrachloroethane
  52.   Tetramethyl Pentane
  53.   2,4,6-Trichloro  Benzenamine
  54.   1,2,3-Trichlorobenzene
  55.   1,3,5-Trichlorobenzene
  56.   0,0,0-Tris-Trimethyl  Epinephrine
  57.   0,0,0-Tris-Trimethylisilyl Epinephrine

-------
                      0
                      I
H
  OH
  C(CHi):
                 POSSIBE STRUCTURE
   Cl
                    N
                    N
                     CH3
Cl

-------
D
       D
  NsO
             81
                           D
                         D
                                                           91
        0

        !S
                                                H
                                                I    I
                                              6  A
H



H
                                                             €1
^H?
                                   0-H
   D
             Zl
                                  II
                                                   D
    01

-------
19
20
21
22
        CH3
        CH3
                         24
25
26
                                     Cl
                                     Cl
27
                                                      Cl
                                         xcr
                                     a""  Nci

-------
                              ?
                             f\>
                          0=0
                                                  II
                                                  II
            en
                                          o— cn_o
                                          x  /••     \
                                         ^ o       L
                                             \
                                               \
                                               o

                                              oJ
                                                        0
                                                       oJ
            os
                                    U)
X-O-X
     I


    o-=o
     r
    vX>
vJj
                                               OJ

                                                O
                                               ro

-------
37
38
                                    H
                          H CH3     H
39
                                              SAME AS  38
40
41
42
         N-C-OH
                                  NH2
                               CH3
43
44
45
                              Cl
                           Cl
            Cl
            Cl
                                                 O
       CH3
         Cl

-------
r
46
H C-CCHp) -CHp
3 R
*bc — o
0 1
M ^C — C —H
H H
49


SAME AS L*S

52

H Cl Cl H H
1 1 I i I
H-C-C-i-C-C-H
1 1 1 1 1
H Cl Cl H H
47






50
c' 	 ,0
1 1
ci\/ Cl
ChC-CI
53
N-H
0,.
^-'


Cl
48
Cl
P1 ci

..
Cl

51
Cl Cl
1 1
Cl- C- C-CI
1
H H
-
54
Cl
i
aci


v-l
______^_ _^— —

-------
55
       Cl
Cl
58
61
         56
                                  -C-N
         59
         62
57
                                                  5i(CHi>
  /
                                                      c-c -
                                                H
                                                I
                                                N
                                                I
60
63

-------
                                  APPENDIX 0





                                  REFERENCES
2306E

-------
                                  REFERENCES
Babcock and Wilcox.  1978.  Steam:   Its  Generation  and  Use.   The  Babcock  and
Wilcox Company, New York, New York.

Benson, S.W.   1976.  Thermochemical  Kinetics,  John Wiley and Sons,  2nd ed.,
New York, New York.

Benson, S.W. and H.E. O'Neal.   1970.   Kinetic  Data  on Gas Phase Unimolecular
Reactions, NSRDS-NBS21, C13.48:21.

Bonner, T.  et al.   1981.   Hazardous Waste Incineration  Engineering.   Noyes
Data Corporation, Park Ridge, New Jersey.

Bunts, R.E., N.R.  Francinques and A.J. Green.   1977.   "Basin F Investigative
Studies,  Chemical  Assessment  and Survey."   Environmental  Laboratory,  U.S.
Army Engineers Waterways Experiment Station, Vicksburg, Mississippi.

Dellinger, B.   1984.   Determination of  the Thermal Decomposition Properties
of 20 Selected Hazardous Organic Compounds.  EPA-600/2-84-138.  August.

Dellinger, B., et al.  1984.  Hazardous Waste, Vol. 1, No. 2, pp. 137-157.

Ebasco  Services  Incorporated.   1986a.   Final  Technical  Plan, Task No.  17.
June.

Ebasco  Services  Incorporated.   1986b.   Final  Laboratory  Test   Plan  for
Incineration of Basin F Wastes at Rocky Mountain Arsenal.  June.

Environmental   Science   and   Engineering,    Inc.     1986.    Draft   Final
Contamination Assessment Report, Source 26-6:  Basin F.  October.

Federal Register.   1981.  Vol.. 46,  No.  15, 40 CFR Parts 122,  264 and  265.
January.
                                      D-l

-------
  Frankel,  I.,  N.  Sanders,  and  G.  Vogel.   1983.   Survey  of  Incinerator
  Manufacturing Industry.  Chemical Engineering Process 79(3):44-55.

  Frenklack, M., et al.  1986.  Combust. Flame, Vol. 64:141-155.
                                          v
  Graham, J.L., et al.  1986.  Env. Scl. &Tech., Vol. 20, No. 7, pp. 703-710.

  Kramllch,  J.  et al.   1984.   Laboratory-Scale  Flame-Mode Hazardous  Waste
  Thermal Destruction Research.  EPA-600/2-84-086.  April.

  Lee,  C.C.  and G.L. Huffman.   1984.   An Overview  of "Who  is  Doing  What" in
  Laboratory and  Bench-Scale Hazardous Waste  Incineration Research.  EPA-600/
  D-84-209.  August.

  Myers, T.E. and  D.W. Thompson.   1982.   "Basin F Overburden and Soil Sampling
  and Analysis Study, Rocky  Mountain Arsenal."  Environmental Laboratory, U.S.
.  Army Engineer Waterways Experiment Station, Vicksburg, Mississippi.

  Registry of Toxic Effects  of Chemical  Substances.  1979 Edition.  Volume One
  and Volume Two.  NTIS-PB81-154478.

  Taylor, P.H., and B. Dellinger, submitted Env. Sci. & Tech.
                                       D-2

-------
                                    DRAFT
                   LABORATORY TEST PLAN FOR INCINERATION OF
                               BASIN F  WASTES AT
                            ROCKY MOUNTAIN ARSENAL
                                  APRIL 1986

                                  TASK  NO.  17
                         CONTRACT NO DAAK11-84-D-0017
THE VIEWS, OPINIONS,  AND/OR FINDINGS CONTAINED IN THIS REPORT ARE THOSE OF
THE AUTHOR(S) AND  SHOULD NOT BE CONSTRUED AS AN OFFICIAL DEPARTMENT OF THE
ARMY  POSITION,  POLICY,  OR  DECISION,  UNLESS  SO  DESIGNATED BY  OTHER
DOCUMENTATION.
THE USE  OF TRADE NAMES  IN  THIS REPORT  DOES  NOT CONSITITUTE AN  OFFICIAL
ENDORSEMENT OR APPROVAL  OF  THE  USE  OF SUCH  COMMERCIAL  PRODUCTS.   THIS  REPORT
MAY NOT BE CITED FOR PURPOSES OF ADVERTISEMENT.
2140E

-------
                               TABLE  OF CONTENTS
SECTION                                                                PAGE

1.0  TEST PLAN OVERVIEW                                                1-1
     1.1  INTRODUCTION                                                 1-1
     1.2  LABORATORY TEST PROGRAM OBJECTIVES                           1-3
     1.3  TECHNICAL APPROACH OVERVIEW                                  1-4
     1.4  EXPECTED RESULTS                                             1-5

2.0  BENCH-SCALE INCINERATION                                          2-1
     2.1  BENCH-SCALE TEST SYSTEM                                      2-1
          2.1.1   Rationale for a Bench-Scale System                   2-1
          2.1.2   Design Philosophy                                    2-1
          2.1.3   Sample Size                                          2-2
          2.1.A   Primary Furnace                                      2-2
          2.1.5   Fly Ash Trap                                         2-2
          2.1.6   Secondary Combustion Gas                             2-3
          2.1.7   Secondary Furnace                                    2-3
          2.1.8   Cooling Section                                      2-4
          2.1.9   Sample Collection                                    2-4
          2.1.10  Range of Test Conditions                             2-4
     2.2  SAMPLE COLLECTION SYSTEM                                     2-4
          2.2.1   Particulate and Residue Collection                   2-5
          2.2.2   Gas Collection                                       2-7
     2.3  BENCH-SCALE TEST OPERATIONS                                  2-8
          2.3.1   Soil Tests                                           2-8
          2.3.2   Sludge Tests                                         2-9
          2.3.3   Liquid Tests                                         2-10

3.0  FEEDSTOCK CONSIDERATIONS                                          3-1
     3.1  INTRODUCTION                                                 3-1
     3.2  SAMPLE CONSIDERATIONS                                        3-1
     3.3  SAMPLE TESTING                                               3-2
          3.2.1   Feedstock Characterization                           3-3
          3.2.2   Analytical Screening for Potential POHCs             3-4
2140E

-------
                              TABLE OF CONTENTS
                                 (Continued)

SECTION                                                                PAGE

4.0  SELECTION OF TEST PARAMETERS                                      4-1
     4.1  INTRODUCTION                                                 4-1
     4.2  TEST MATRIX PARAMETERS                                       4-2
          4.2.1  Selection of Time  Parameter                           4-3
          4.2.2  Selection of Temperature Parameter                    4-3
          4.2.3  Oxygen Concentration                                  4-5
          4.2.4  Test Execution                                        4-7
     4.3  SELECTION OF PRINCIPAL ORGANIC HAZARDOUS
          CONSTITUENTS (POHCs)                                         4-7
     4.4  SELECTION OF ANALYTICAL PARAMETERS                           4-9

5.0  ANALYTICAL DETAILS                                                5-1
     5.1  SAMPLE HANDLING AND SAMPLE FLOW                              5-1
     5.2  ANALYTICAL PROTOCOL SUMMARY                                  5-2
          5.2.1  Volatile Organics in Soil and Solid Samples
                 by Gas Chromatography/Mass
                 Spectrometry (GC/MS)                                  5-2
          5.2.2  Semivolatile Organics in Soil and
                 Solid Samples by Gas Chromatography/
                 Mass Spectrometry (GC/MS)                             5-3
          5.2.3  Metals in Soil and Solid Samples by
                 Inductively Coupled Argon Plasma (ICP)
                 Emission Spectrometry                                 5-3
          5.2.4  Arsenic in Soil and Solid Samples by Graphite
                 Furnace Atomic Absorption (AA)                        5-4
          5.2.5  Mercury in Soil and Solid Samples by Cold
                 Vapor Atomic Absorption (CVAA) Spectroscopy           5-4
          5.2.6  Extraction Procedure (EP) Toxicity Protocol
                 for Soils, Incineration Residues, and Solids          5-5
          5.2.7  Ignitability in Soil and Solid Samples                5-5
                                      ii
2140E

-------
                               TABLE  OF CONTENTS
                                  (Continued)

SECTION                                                                PAGE

     5.2  ANALYTICAL PROTOCOL SUMMARY (Continued)
          5.2.8   Corrosivity Toward Steel in Soil and
                  Solid Samples                                        5-5
          5.2.9   Reactivity in Soils and Solid Samples                5-6
          5.2.10  Proximate Analysis of Soil and Solid Samples         5-6
          5.2.11  Unknown Identification in Soil, Solid, and
                  Sludge Samples by Gas Chromotography/
                  Mass Spectrometry (GC/MS)                            5-7
          5.2.12  Volatile Halogenated Organics in Liquid Samples      5-8
          5.2.13  Volatile Aromatic Organics in Liquid Samples         5-8
          5.2.14  Organochlorine Pesticides in Liquid Samples          5-8
          5.2.15  Organosulfur Compounds in Liquid Samples             5-9
          5.2.16  Organophosphorous Pesticides in Liquid Samples       5-9
          5.2.17  Phosphonates in Liquid Samples                       5-10
          5.2.18  Metals in Liquid Samples                             5-10
          5.2.19  Ignitability in Liquid Samples                       5-11
          5.2.20  Corrosivity Toward Steel in Liquid Samples           5-11
          5.2.21  Reactivity in Soils and Solid Samples                5-11
          5.2.22  Proximate Analysis of Liquid Samples                 5-12
          5.2.23  Volatile Organics in Incineration Off-Gas
                  Samples by Gas Chromotography/
                  Mass Spectrometry (GC/MS)                            5-13
          5.2.24  Acid Gases in Incineration Off-Gas Samples           5-14
          5.2.25  Volatile Metals by Inductively Coupled
                  Argon Plasma (ICP) Emissions Spectrometry
                  in Incineration Off-Gas Samples                      5-14
          5.2.26  Volatile Metals/Arsenic in Incineration Off-Gas
                  Samples by Graphite Furnace Atomic
                  Absorption (AA) Gas Spectrometry                     5-14
                                      iii
?140E

-------
                               TABLE  OF CONTENTS
                                  (Continued)

SECTION                                                                PAGE

     5.2  ANALYTICAL PROTOCOL SUMMARY (Continued)
          5.2.27  Volatile Metals/Mercury in Incineration
                  Off-Gas Samples by Cold Vapor Atomic
                  Absorption (CVAA) Spectrometry                       5-15
          5.2.28  Moisture Content in Incineration Off-Gas Samples     5-15
          5.2.29  Organophosphorous,  Organosulfur, and
                  Organochlorine Compounds in Incineration
                  Off-Gas Samples by GC/Selective Detectors            5-15
     5.3  ANALYTICAL RESULTS                                           5-16
          5.3.1   System Performance Parameters                        5-16
          5.3.2   Analytical Results                                   5-16
     5.4  CERTIFICATION                                                5-16
     5.5  QA/QC                                                        5-16

6.0  EXPECTED RESULTS                                                  6-1
     6.1  INTRODUCTION                                                 6-1
     6.2  EXPECTED ORE RESULTS                                         6-1
     6.3  EXPECTED TECHNOLOGY SELECTION CONFIRMATION RESULTS           6-2
     6.4  OTHER EXPECTED RESULTS                                       6-3

     Appendix 1 - REFERENCES                                           A-l
                                      iv
2140E

-------
                                LIST OF TABLES
NUMBER
1.1-1   Chemical Characterization of Basin F Liquid
1.1-2   Hazardous Chemicals Contained in the Soils
1.1-3   Summary of Thermal Decomposition Data
2.2-1   Gas Sample Collection Matrix
3.1-1   Properties of Selected Compounds
4.3-1   Heats of Combustion for Hazardous Wastes
5.1-1   Analytical Methodology
5.1-2   Number of Analyses
FOLLOWING PAGE






      1-1






      1-1





      1-3






      2-7






      3-1






      4-8






      5-1






      5-1
2140E

-------
                               LIST OF FIGURES


NUMBER                                                         FOLLOWING PAGE

1.1-1   Schematic Diagram of Processes Occurring
        During the Destruction of a Solid Waste                      1-2

2.1-1   Laboratory-scale Incineration Unit                           2-1

2.1-2   Rotating Tube Furnace Arrangement                            2-2

2.1-3   Rotating Tube Unit                                           2-2

2.1-4   Test Condition Range, 7810 cm  Furnace Volume                2-4

2.1-5   Test Condition Range, 3124 cm  Furnace Volume                2-4

2.2.1   Sample Train                                                 2-5

2.2-2   Solid Residue Collection Flow Chart                          2-6

2.2-3   Modified Sampling Train for High Moisture Samples            2-7

3.1-1   Soil Sampling Location                                       3-2

4.2.1   Exhaust CO and Total Hydrocarbons and Fraction of
        Test Compound Remaining in Exhaust as a Function
        of Theoretical Air                                           4-6

5.1-1   Sample Analytical Flow                                       5-1
                                       vi
2140E

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                            1.0  TEST PLAN OVERVIEW
 1.1   INTRODUCTION

 Wastes  in  Basin F  at Rocky Mountain Arsenal (RMA), which require treatment,
 include liquid and  sludge  as well as  soils  associated with the  lagoon.
 These soils include fill,  placed above and below the liner, as  well  as  the
 3/8-inch  asphalt  liner  itself.   These materials,  which contain  various
 concentrations  of  hazardous compounds  as  shown  in Tables 1.1-1 and  1.1-2,
 are  candidates  for treatment by incineration.   If  treated  by  incineration,
 the  hazardous  organic compounds  present in Basin F wastes must  be destroyed
 at a destruction and  removal efficiency (ORE) of 99.99 percent.

 A  conventional incinerator  system,  including an  afterburner,  subjects a
 compound to a  variety of  severe environments which may  destroy hazardous
 waste at  the  desired ORE  levels.   Any  organic compound  subjected  to
 hazardous  waste incineration  may be subjected to at least three, if not  all,
 of the  following environments:

     1.  Pyrolvsis  -  Solids  are  volatilized  or  sublimed,  volatiles  and
        semivolatiles are  evolved in  the  gas  phase, and gaseous products may
        be  further fragmented into smaller compounds and radicals;

     2.  Oxidation  in the  flame  -  Volatile  compounds  and  radicals  are
        subjected  to a radical-rich  environment and converted into C02,
        H20, and products of incomplete combustion  (PICs);

     3.  Oxidation  in  a  high temperature,  postflame region  - Final thermal
        reactions  leading  to  complete oxidation  of the organic  constituents
        in the  incinerator's combustion zone occur;

    4.  Oxidation  in  a second  flame  - Subsequent  destruction (in  the
        afterburner)  of unreacted components of the hazardous wastes; and
                                      1-1
2140E

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                                 TABLE 1.1-1

                 CHEMICAL CHARACTERIZATION OF BASIN F LIQUID
Compound or Parameter
PH
Aldrin
Isodrin
Dieldrin
Endrin
Dithiane
DIMP
DMMP
Sulfoxide
Sulfone
Chloride
Sulfate
Copper
Iron
Nitrogen
Phosphorus (total)
Hardness
Fluoride
Arsenic
Magnesium
Mercury
Cyanide
COD
TOC
Units
-
ppm
PPb
ppb
ppb
ppb
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppb
ppm
ppm
ppm
Concentration Range!/
6.9
50.0
2.0
5.0
5.0
30.0
10.0
500.0
4.0
25.0
A8, 000.0
21,000.0
700.0
5.0
120.0
2,050.0
2,100.0
110.0
1.0
35.0
26.0
1.45
24,500.0
20,500.0
- 7.2
- 400
- 15
- 110
- 40
- 100
- 20
- 2,000
- 10
- 60
- 56,000
- 25,000
- 750
- 6
- 145
- 2,150
- 2,800
- 117
- 1.3
- 40
- 29
- 1.55
- 26,000
- 22,500
I/  Based on analysis of various samples from different locations and
    depths in the basin (Bunts et al. 1977).
2140E

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                                  TABLE 1.1-2
                  HAZARDOUS CHEMICALS CONTAINED IN THE SOILS
VOLATILE ORGANICS
    1,1-Dichloroethane
    Dichloromethane
    1,2-Dichloroethane
    1,1,1-Trichloroethane
    1,1,2-Trichloroethane
    Carbon tetrachloride
    Chloroform
    Tetrachloroethylene
    Trichloroethylene
    Trans-1,2-Dichloroethylene
Benzene
Toluene
Xylene
Ethylbenzene
Chlorobenzene
Methylisobutyl ketone
Dimethyldisulfide
Bicycloheptadiene
Dicyclopentadiene
SEMIVOLATILE ORGANICS
    Aldrin
    Endrin
    Dieldrin
    Isodrin
    p,p'-DOT
    p,p'-DOE
    Chlorophenylmethyl sulfide
    Chlorophenylmethyl sulfoxide
    Chlorophenylmethyl sulfone
    Hexachlorocyclopentadiene
Oxathiane
Dithiane
Malathion
Parathion
Chlordane
Azodrin
Vapona
Supona
DIMP
Atrazine
METALS
    Aluminum
    Arsenic
    Cadmium
    Chromium
    Copper
Iron
Lead
Mercury
Zinc
2140E

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    5.  Oxidation in a  second high temperature,  postflame  region - Final
        thermal oxidation  reactions  occur before the  combustion  gases are
        exhausted to pollution control devices.

In  general,  it is  believed that 99 percent  of the destruction  of any
hazardous organic compound  occurs in the  flame  region.  The postflame  region
destroys 99 percent of the  remaining one  percent  of material  to achieve the
99.99 percent  destruction  removal  efficiency  (ORE).    (For  detailed
discussions,  see  Kramlich  et al. 198A,  and  Dellinger  et al.  1984.)
Pyrolysis  reactions are  shown  in  Figure 1.1-1.   Flame  and  postflame
reactions are summarized in Figure 1.1-1 as "Thermal Oxidation."

The bench-scale laboratory  program,  designed  and  described in the following
pages,  recognizes  the  difficulty  in  handling the  compounds  listed  in
Tables 1.1-1  and  1.1-2  and the  complexity  of thermal destruction through
incineration  as  illustrated  in  Figure 1.1-1.  This program  is designed,
therefore, to accomplish the following:

    1.  Provide sufficient  information  on  the  physical, chemical,  and
        thermodynamic properties of  the compounds listed  in Table 1.1-1 and
        1.1-2 to ensure reasonable success  in designing and implementing an
        incineration program;

    2.  Provide a bench-scale  apparatus that  accurately simulates all or  a
        major portion of a  full-scale incineration system;

    3.  Demonstrate the achievement  or potential to achieve  99.99 percent
        ORE for hazardous compounds present in Basin F; and

    4.  Contribute to the selection of an incineration technology.

Data developed by Dellinger et al. (1984) demonstrate  that most organics  can
be incinerated to a ORE of 99.99 percent within two seconds at temperatures
of 600°C to 950°C (Table  1.1-3).   In addition, Kramlich et al. (1984), have
determined that excess air  used in the
                                      1-2
2140E

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PYRC
i

•LYSIS 	
\
PYROLYSI
!^P
PYROLYZED PRODUCT
MIX
ING
SOLID
MEL
TING
LIQUID
/APORI

SUBLIN/
ZATION
VAPOR
S
MIX


IATION
MIXING
IGNITION
\
ING
PARTIALLY OXIDIZED
PRODUCTS AND
INTERMEDIATES
MIX
ING
           THERMAL OXIDATION
                 1
               PARTIALLY
            OXIDIZED PRODUCT
             FIGURE 1.1-1
  SCHEMATIC DIAGRAM OF PROCESSES
OCCURRING DURING THE DESTRUCTION
         OF A SOLID WASTE

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flame mode of destruction  is  best  held within 30 percent to 40 percent
(35 percent excess  air  corresponds to 5.4 percent 0_ in the dry stack
gas) to produce the lowest levels  of CO and hydrocarbon emissions, and
ensure the most complete combustion  of any supplementary fuel, as well
as hazardous  wastes.  Consequently,  the  bench-scale  program has been
designed recognizing the  fairly narrow ranges of temperatures,  times,
and excess  air   associated with achieving 99.99 percent ORE of most
organic hazardous wastes.

1.2  LABORATORY TEST PROGRAM OBJECTIVES

The laboratory  test  program  has  been designed  to  accomplish  the
following objectives:

    o  Demonstrate  that  99.99 percent  ORE is  achievable for the hazardous
       wastes contained in the liquid,  sludge,  and  contaminated soils
       associated with Basin F;
    o  Determine  what  temperatures,  residence  times,  and  levels  of
       excess 02 can  be used to achieve 99.99 percent ORE  within the n
       cost-effective incinerator technology framework;
    o  Provide  sufficient  data  to  determine hazardous  waste destruction
       kinetics based on first order approximations;

    o  Provide  guidance  for  final  incineration technology  selection and
       optimization for  transition  from bench-scale to pilot plant  or  from
       bench-scale to a  full-scale  operation.   In this respect, bench-scale
       testing  is  designed to provide  guidance  for initial conditions and
       subsequent conditions to be tested by the next scale of operation.
                                      1-3
2140E

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                                 TABLE 1.1-3


                    SUMMARY OF THERMAL DECOMPOSITION DATA
Empirical
Compound Formula
Acetonitrile C^N
Tetrachloroethylene C2C1A
Acrylonitrile C3H3N
Methane CH^
Hexachlorobenzene C6C16
l,2,3,A-Tetra-
chlorobenzene CgH-Cl^
Pyridine C5H5N
Dichloromethane CH2C12
Carbon Tetrachloride CC1
Hexachlorobutadiene C*C16
l,2,A-Trichloro-
benzene C.hLCl,
1,2-Dichloro-
benzene C6HAC12
Ethane C2»6
Benzene C6^6
Aniline C6H?N
Monochlorobenzene C,H_C1
Nitrobenzene CgHLNO,,
Hexachlorethane C2C16
Chloroform CHClj
1,1, 1-Trichlorethane C_H Cl
Tonsetd)
760
660
650
660
650

660
620
650
600
620
6AO

630
500
630
620
SAO
570
A70
AID
390
T99(2)
900
850
830
830
820

800
770
770
750
750
750

7AO
735
730
730
710
670
600
590
570
T99.99(2)
950
920
860
870
880

850
8AO
780
820
780
790

780
785
760
750
780
700
6AO
620
600
I/  Temperature at which decomposition initiates at 2 seconds reaction time.
21  Temperature where 99 and 99.99% of the compound is destroyed at a 2
    second reaction time.

Source:  Dellinger et al. 198A.
21AOE

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1.3  TECHNICAL APPROACH OVERVIEW

Given the nature of the compounds being  destroyed  and  the  objectives of the
program, a technical  approach  has  been developed to ensure  success  of the
ultimate  full-scale  incineration effort.   This approach  recognizes the
inherent limitations  of  laboratory  investigations, along with the lack of
precise data concerning the feedstocks to be incinerated.

The technical approach involves using  equipment  that will  simulate three of
the major  incineration mechanisms:   1) pyrolysis; 2) postflame  (primary
incinerator); and 3)  postflame  (afterburner).  Basin F samples will  be sent
to  Hittman/Ebasaco  Associates  Inc.  (HEAI) for  preparation.  HEAI  will
perform the  actual  bench-scale incineration testing.   If  necessary, HEAI
will send the  feed  samples to UBTL and  CAL for laboratory analysis.   The
tests will be  carried out  with the  largest sample sizes possible given  the
constraints  of  laboratory  operations  in order  to  ensure data accuracy  in
scale-up.  Large-scale (e.g., 250-500  gram) samples are  to be used.  Because
relatively large  samples  are being used,  testing  of  the  consequences of
flame-mode destruction cannot be directly simulated.

The technical  approach is designed largely to focus  on and evaluate the
impact  of  incineration on Basin  F contaminated  soil.  The incineration
regime  found to be successful  with  soil then will  be confirmed for  the
incineration of liquid and  sludge.   This  approach,  initially,  does  not
designate one or more principal organic  hazardous  constituents  (POHCs), but
evaluates the   impact  of  incineration on  all compounds  identified in
Tables 1.1-1 and 1.1-2.

The technical  approach begins  with  limited characterization of selected
compounds in terms of physical,  chemical,  and  thermodynamic properties.  Of
most significance are  the  ash  fusion  temperatures  of the principle types of
soil and, consequently, the  potential for operating  any incineration  system
in  the  slagging mode.  The  technical approach then tests the  impact  of
incineration of contaminated soil  at  two temperatures,  two  residence  times
(in the afterburner),  and  two levels  of excess  0_.   Multiple runs will be
used to ensure that the ORE associated with any compound will not be masked,
                                      1-4

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regardless of concentration in the incoming material to be incinerated.  The
impact of  incineration  on sludge, liquid, and a  proportionate  mixture of
liquid, sludge,  and soil will be the final test  sequence.

The actual matrix of test conditions is summarized below:

Parameter             Maximum Value     Second Value    Minimum  Value

Temperature              1,250°C            900°C            650°C
Time                      5 sec             2 sec             N/A
0  Level                  5.4%              7.0%             N/A

This rationale,  discussed in Chapter 4, is based upon conditions expected to
occur in a full-scale incinerator  system.  Further,  this  rationale is based
upon providing  sufficient  spread in the parameters to permit extrapolation
of results between extreme points.

1.4  EXPECTED RESULTS

Test program  results will facilitate  scale-up  of the bench-scale  thermal
destruction system to either pilot  plant  or  full-scale  operations.   Expected
results include the following specific data:

    o  Evaluation of hazardous  chemicals  remaining in the residues of soils
       or sludges after incineration;

    o  Degree  of  destruction  associated  with  specific   pyrolysis and
       postflame  environments,  to  determine  acceptable  regimes  for
       incineration  processes  (e.g.,   temperature in  the  afterburner,
       residence time, and excess 02 in the  flue gas); and

    o  Sufficient  time,  temperature,  and oxygen concentration  data to
       extrapolate  rough optimal  conditions between the  tested  points
       identified above, assuming first order kinetics.
                                      1-5

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The  bench-scale program,  designed  to test  for the destruction  of all
hazardous waste compounds  identified  in  Tables  1.1-1 and  1.1-2,  will permit
final  selection  of POHCs  to  be  used for determination of the  success  of
larger-scale systems.  Additionally,  pretesting of soil, sludge, liquid, and
selected hazardous materials  will provide  essential  physical,  chemical,  and
thermodynamic  data for  design  and  operation  of  the  primary thermal
destruction  (incinerator)  unit  at  either  the  pilot-scale or  full-scale.
These data will include, but not necessarily be limited to:

    o  Ash fusion temperature of the soil;

    o  Thermal conductivity,  specific heat,  and heat capacity  of  the soil
       and sludge;

    o  Selected calorific  values, proximate  analyses,  and related data  for
       the compounds to be incinerated; and

    o  Corrosivity (with particular  respect  to refractories) of the  liquid
       with five percent chlorides and two percent sulfides.

These data will assist  in  the determination  of fuel requirements,  residence
times of solids,  and desired temperatures associated with the pilot plant
and full-scale primary  incinerator.   They  also  will be  used  to  determine the
maximum temperature  associated with the Linder furnace in  the bench-scale
test.  The  Linder furnace accomplishes  the  solids'  heatup  and volatile
evolution.   While  full-scale  operation may occur in the slagging  mode,  the
bench-scale apparatus will be operated below slagging temperatures.

The ultimate value of the  bench-scale test program will be  to  develop  data
for operation scale-up.  The  results described  above will assist not only in
determination of  a combustion regime  that will achieve 99.99 percent ORE,
but also will  confirm the most  appropriate  technology  for  incineration  of
Basin F waste.   Specific  parameters  associated with technology  selection
will be temperatures, the evolution  of  hazardous chemicals from  soil  and
sludge, residence times, and excess oxygen levels.  Specific technologies
                                      1-6
2140E

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to  which these data  can  be applied include  countercurrent  and cocurrent
rotary kilns, fluidized beds, and hearth-type furnaces.

The  bench  scale test regimes have  been  designed to achieve 99.99 percent
ORE.  The  most severe conditions including a temperature of 1250°C and a
residence  time  of 5 sec exceed those  used  by other researchers (see, for
example, Dellinger  et al.  1984) to achieve 99.99 percent ORE.  The margins
of  safety  to  ensure that  the  desired  ORE  is obtained  exist  both in
temperature and time.  These margins of  safety have been  selected based on a
review of  the  literature  associated with hazardous waste destruction,  where
the hazardous compounds are in dilute concentrations.

It  is recognized,  however,  that  the  laboratory  program simulates the
post-flame oxidation  zone,  but  does not simulate  flame-mode destruction of
hazardous  chemicals.   The  laboratory test program, then, does  not simulate
the  most severe environments available.  Such  environments  include higher
temperatures, if  shorter residence  times.  Typical flame  temperatures may be
about 1725°C  (2000 K), and  residence  times  may be 0.1  sec  (Perry  et al.
1963).   Further,   the  flame  environment  is characterized by  high
concentrations  of  free  radicals;  and consequently the  mechanisms for
hazardous  waste  destruction in  that  environment are  most  different from
those associated  with the  post-flame  oxidation  zone.   Radical dominated
mechanisms increase the rate of hazardous waste  destruction  relative to that
rate  associated with oxygen-rich non-flame environments  (Kramlich et al.
1984).   Consequently,  the  destruction  in an  incinerator typically occurs as
follows:   1) 99 percent  within the flame region and 2) 99  percent of the
remaining 1 percent of material in the post-flame region.

Given these data, it  is reasonable  to  conclude that the laboratory program,
by itself, will achieve 99.99 percent  ORE levels for the wastes in Basin F.
Dilute concentration  kinetics  as developed by previous research leads to
this  conclusion.    At  the  same time,  however,  the experiment is  not
simulating the  flame  mode destruction.  Consequently, it is not  simulating
one  mechanism  for  achieving  at  least  99 percent ORE.   Given  that
consideration, if the  laboratory  test  achieves in excess of 99 percent ORE,
it is reasonable  to conclude that  a pilot  plant or full-scale incinerator
would achieve 99.99 percent  ORE when combining  flame mode destruction with  a
strong post-flame oxygen-rich environment.
                                      1-7
2140E

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                        2.0  BENCH-SCALE INCINERATION


2.1  BENCH-SCALE TEST SYSTEM

     2.1.1  Rationale for a Bench-Scale System

     Thermal decomposition laboratory tests have been performed on both pure
     compounds  and  field  samples  to determine  incineration parameters,
     including temperature, residence time,  and  excess oxygen, required to
     decompose toxic chemicals.  These laboratory tests have been performed,
     primarily, using  milligram-to-gram  size samples.  These  small  sample
     sizes have  been adequate to characterize incineration  parameters  for
     pure compounds  and  compounds in high  concentrations.   For chemicals
     which are  present in low concentrations, these small sample sizes are
     not  adequate  to demonstrate 99.99% destruction due  to  the analytical
     limits of  detection  of the  off-gases.   It is of interest  to demonstrate
     99.99%  destruction   for  all toxic  constituents  in  a  feed  sample
     regardless of whether or  not that  constituent  is  chosen as a principal
     organic hazardous constituent  (POHC).   Although there are substantial
     data on the  thermal destruction of individual compounds,  incineration
     tests  on  field  samples  are necessary to  adequately  simulate the
     interaction  of  various  constituents  at  high  temperatures and the
     production of products of incomplete combustion  (PIC).  The bench-scale
     test unit  for Task  17 was  designed to measure ORE  up  to 99.99% for
     constituents of concern at Basin F for soil, sludge, and  liquid samples.

     2.1.2  Design Philosophy

     The  laboratory  bench-scale  unit was  designed to  evaluate  thermal
     destruction efficiency at temperatures up to  1300°C and residence  times
     from 2 to  5  seconds.  The unit  is a batch-load system  with two  furnaces
     and  a blended carrier gas to simulate combustion gases (Figure 2.1-1).
     The  first  furnace is used to volatilize the constituents.  The carrier
     gas moves  these constituents into the  secondary furnace which is used
                                      2-1

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          ROTATING
          FURNACE
INCINERATION
  FURNACE
(AFTERBURNER)
  GAS
 SUPPLY
CONTROLS
                     FLY ASH
                   SEPARATOR
                                        COOLING
                                        SECTION
                    SAMPLING
                     TRAIN

                            EXHAUST
                              PUMP
                    SECONDARY
                       GAS
                    PREHEATER
                         FIGURE 2.1-1
       LABORATORY SCALE INCINERATION UNIT

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     to  simulate  afterburners in a full-scale incineration  plant.   In the
     secondary  furnace,  additional blended  gases  with 0_  are added  and
     temperature  is  increased to decompose the hazardous  constituents.  The
     combustion  products in  the off-gas  are  then collected  in  various
     sorbents in the sampling train.
     2.1.3  Sample Size

     The first design  consideration  was  that  of the overall apparatus size.
     The primary  concern with respect to  this was that of being  able to
     collect and analyze  an  off-gas  constituent to  demonstrate 99.99% ORE of
     a chemical present  in the feed  sample in a few parts per billion.  For
     the chlorinated compounds which can be analyzed using GC/ECD, a sample
     size  of  several  hundred  grams  is  adequate.   Task  budget  and
     availability  of  a rotating  tube furnace, capable of handling  batch
     samples up to five  hundred grams, determined the  laboratory bench-scale
     unit design based on a sample size of 200-500 grams.

     2.1.4  Primary Furnace

     The primary  furnace (Figure  2.1-2) is  an electric   furnace  with a
     programmable temperature controller capable of maintaining 1000°C with
     gas flows up to 20  liters per minute. A gas supply  system is  used to
     provide blends  of N2>  C02,  and  02 to  simulate  various combustion
     processes in fuels.  The primary furnace barrel (Figure 2.1-3)  is 130
     mm in diameter and  200  mm in length.   The maximum temperature  rise of
     the primary  furnace is about  5.5°C  per  minute.  The carrier  gas
     velocity will be between 6 and 8 cm per second at test conditions.

     2.1.5  Fly Ash Trap

     Provisions will be made  for  a fly ash separator between the primary and
     secondary furnace.   The purpose  of this separator is  to  remove ash
     which may be  entrained  in the  carrier gas and to prevent plugging of
     the secondary furnace.   The ash separator will be a cyclone type  design
                                      2-2
•71 A or

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(Ins Supply
        Filter
   On/
101  Off
                          Temperature
                          Controllers
            Ji
                                             Temperature
                                             Recorder
                                             Programmer
                    FIGURE 2.1-2
 ROTATING  TUBE FURNACE  ARRANGEMENT

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  SLIP
  SEAL

  GAS
OUTLET
           RIDING
            RING
     DRIVE
     CHAIN
     SPROCKET
130 mm DIA.
                   RIDING
                    RING
            150 mm DIA.
                              GAS
                             INLET
                                                                   TYPE
                                                               THERMOCOUPLE
                              FIGURE 2.1-3
                     ROTATING  TUBE  UNIT

-------
V,
              capable  of removing particulates  down  to 100 microns.   It will be
              constructed  of  stainless steel  and insulated to  prevent heat loss
              between the primary and secondary furnaces.

              2.1.6  Secondary Combustion Gas

              Additional gases  will  be introduced between the primary  and secondary
              furnaces  to  simulate secondary  combustion gases.   The composition of
              this gas  will be  the same as that of the primary carrier gas and will
              increase  the  total gas flow rate by 50 percent.  The  carrier gas will
              be  preheated to  near  (± 50  C°) that  of the primary carrier  gas
              temperature.

              2.1.7  Secondary Furnace

              The  secondary furnace was  designed to heat  gases from  the primary
              furnace  along with the secondary airflow up to 1250°C and  to maintain
              the  gases at this temperature for  between  2  and 5 seconds.  To  have
              fully  developed flow  while avoiding  high pressure  losses in  the
              furnance,  a  velocity range  of 20 cm/sec to 500 cm/sec  was  established.
              For  this  velocity  range  and the  desired gas flow rate, the  furnace tube
              diameter  would  be approximately 2  1/2  cm.   For a residence time of  5
              seconds,  the furnace tube would be approximately  10  meters long.   The
              secondary furnace  tube will be constructed of fused quartz  to  provide a
              nonreactive  environment  at high  temperature.   With proper bending of
              the  quartz tube,  the secondary furnace would require a O.lA-cubic meter
              volume.   This size  is consistent with small pottery  kilns which are
              capable  of  withstanding a  temperature  of  up  to 1300°C.   Three
              temperature  probes  will  be  installed  in the  secondary furnace  to
              monitor  furnace temperature.  The kiln  should  be able  to maintain
              temperature  within ± 10  C°.

              Gas  residence time in the secondary furnace  can  be varied  by changing
              gas  flow  rate  or length of the  furnace  tube.   Since  the desired
              residence times range  from  2 to  5 seconds,  the  gas flow rate would have
                                               2-3

-------
     to  be  varied by a  factor  of 2.5 to  cover that range.  Since  this
     variation in  the  gas flow rate  is  too large to maintain  reasonably
     consistent test conditions, two furnace tube lengths will be used.

     2.1.8  Cooling Section

     The cooling  section  will  consist of a straight 2.5-cm diameter quartz
     tube approximately  3 feet long.  Exit temperature from the cooling
     section will be monitored  to insure that temperature will be maintained
     between 200°C  and  300°C.   Insulation will be applied  to the tube to
     adjust the exit temperature.

     2.1.9  Sample Collection

     All  off-gases from  the secondary  furnace will  enter  the  sample
     collection system.   The sample collection  system is designed to remove
     organic and  inorganic constituents  of concern.  A pump will be used
     downstream of the  sample collection  system to  maintain  a near
     atmospheric pressure  in the  entire  flow train.  The sample  collection
     system is described in detail in Section 2.2.

     2.1.10  Range of Test Conditions

     Once the design of  the  bench-scale  test  apparatus  is fixed, variations
     in  test  conditions  from  the  design  point are possible; however,
     parameters are  interdependent  for a  fixed furnace volume.  Residence
     time in the furnace  is  a  function of volume flow rate which is a func-
     tion of the  mass  flow rate,  pressure, and temperature (Figures 2.1-4
     and 2.1-5).  Actual  operating  regimes  will be established  as the design
     is finalized.

2.2  SAMPLE COLLECTION SYSTEM

     Collection of the gases generated from all test incineration runs will
     require a system for collection of non-particulate and particulate
                                      2-4
2140E

-------

-------
                      GAS FLOW RATE AT STANDARD CONDITIONS (l/m)
                                                 CO
                                                 o
                                                o
en
o
H
m

   10
Z
0
m

-------
     fractions.   Sampling of off-gases depends on  the  nature of POHCs and
     other large species.  In general, the sampling apparatus for collecting
     off-gas effluents  includes  three  major  components:

     o  One or more thermostatically controlled compartments to maintain the
        gas at a temperature consistent with the collection  medium, usually
        hot (200°C) for  particulate collection and cool  (20°C) for sorbent
        collection of the more volatile constituents;

     o  Sample collectors to  collect  the samples,  such as,  filters  and
        sorbents;  and

     o  Vacuum pump and gas  meter

     The sampling  train  used will be  similar  to the one shown  in Figure
     2.2-1.  Using this  sampling  train will provide both adequate trapping
     of particulate and  non-particulate fractions  from  the  off-gas.   The
     number of  impingers and sorbent  tubes  may  vary in number  and type
     depending upon the test run.  This device is  physically similar  to the
     Modified Method 5  (MM5) sampling  train.

     2.2.1  Particulate and  Residue Collection

     Bottom residue left  in the  kiln  from the  test burn will be removed  by
     the most efficient means available to  the lab which will be consistent
     with:

        o  Complete removal  (>99%);
        o  Prevention of outside contamination; and
        o  Prevention of damage  to the kiln.

     Bottom  residue removal will be dependent   upon  the  physical
     characteristic of the  test  sample after incineration.  The  bottom
     residue mass may  vary  from  <10%  of the  starting material weight  to  >90%
     depending  upon the  sample  matrix  (liquid,   sludge,  soil).  The
     laboratory anticipates  some flexibility will be required in attaining
                                      2-5
2140E

-------
                     HEATED AREA
TEMPERATURE SENSOR
  THERMOMETER
Y   ^FILTER HOLDER
                       THERMOMETER

                           CHECK VALVE
                RECIRCULATION PUMP

                         THERMOMETERS
                              DRY GAS   AIR-TIGHT
                               METER     PUMP
                                                              VACUUM LINE
                                FIGURE  2.2-1
                             SAMPLE TRAIN

-------
an  efficient  removal  of the bottom  residue.   Residue removal  and
cleaning of the  kiln will be adequate to assure subsequent test burns
are not cross-contaminated.  Bottom residue will be stored at about 4°C
in glass bottles with Teflon lined caps until combined with the fly ash.

The  fly  ash separator  will retain the  larger particulates carried
through the primary furnace tube.  As with  the bottom residue,  the
volume of  fly  ash produced will vary  with  respect to sample matrix.
Efficient removal of  the  fly ash to Teflon-capped  glass  bottles can be
expected.  The fly ash will be stored at about 4°C.

Filter cassettes  will be  used  to trap  particulates  which are  not
separated as fly ash  and  may vary  in  size from 1 to 100 microns.  The
filter used will  be a glass fiber type  and will be stored in a glass
bottle with a Teflon-lined cap at 4°C.

Figure 2.2-2  illustrates the flow of the  residue sample  into  the
analytical system.   The  three  solid fractions from the test burns are
weighed and the  weight summed to  estimate  the percentage of  sample
volatilized:
                                   WB + WF + WP
       % Sample Volatilized = (1 -       L      ) x 100
                                         WS
            Where    Wg = Weight of Bottom Residue
                     Wp = Weight of Fly Ash
                     Wp = Weight of Filter Particulates
                     W  = Weight of Original Sample
The bottom ash and  fly  ash  will be combined and homogenized.  Aliquots
of this  residue  will be taken  for the various chemical and  physical
analyses required to  determine  destruction efficiency of the POHCs and
the EP toxicity of the residue.

The particulate filter  is weighed  and  combined with the XAD-2 resin for
extraction and analysis.
                                 2-6

-------
Physical
 Tests
Inorganic
 Tests
Organic
 Tests
                                         Participates
                                            i
                                          Weighed
                                         Combine with
                                           XAD-2
                                           Extract
                                            1
                                           Analyse
                    FIGURE 2.2-2
SOLID RESIDUE  COLLECTION FLOW  CHART

-------
The  chemical and  physical  analyses to  be  performed on  these
incineration residues are described  in detail  in  Section  5.0.   Section
4.3  contains details  of  the analytical  test matrix after  the
incineration tests.

2.2.2  Gas Collection

The gas collection  procedures are dependent upon the  POHCs  that have
been selected for analysis to determine if  they have been destroyed to
99.99% ORE.  The PICs are  also important  in the selection of the types
of  impingers  and sorbents used.   As a  result  of the  initial sample
size, it  is  necessary  to completely extract and  concentrate the  XAD-2
sorbent,  and  combine it  with the  extracted  condensate, and  the other
impinger  solutions to achieve parts per trillion detection limits.

Table 2.2-1 describes the  types  of sorbent  and impinger solutions that
will  be  used  to  trap  organic  and inorganic  products  from the
incineration.  When the waste  sample  matrix  is  water or sludge,  a
condensate trap  will be  used to  reduce  the  volume of liquids delivered
to  the  sorbent  traps.    Figure  2.2-3  describes  this  trap.   The
condensate  collected  in  the trap  must  be   tested  for the  various
compound  classes.   An  aliquot of  the  liquid  can  be analyzed  for
volatile  and  semivolatile  organics and  acid and basic  inorganics (i.e.,
F~,  Cl",   phosphorous,  and  metals).   Section 5.2  provides  more
details on the analytical protocol for handling the condensate  fraction.

After a test run,  the  sorbents and  impinger fractions, as well as  the
condensate  when  applicable,  are transferred  to  glass bottles  with
Teflon-lined  caps  for  storage at about  4°C.  The analytical  protocols
which can be performed  on  the  various fractions  are described in
Section 5.0.
                                 2-7

-------
                                 TABLE 2.2-1
                         GAS SAMPLE COLLECTION MATRIX
Compound
 Class
   Sorbent
Impinger
Water *
 Trap
Volatile Organics
Tenax/Charcoal
                      Test
Semivolatile Organics   XAD-2


Volatile Metals




Acid Compounds


Cyanide


Basic Compounds
                                           Test


                    Silver Catalyzed       Test

                    Ammonia Persulfate
                    0.1 NaOH


                    0.1 NaOH


                    0.1 HC1
                      Test


                      Test


                      Test
*A water trap will be utilized when the test sample is sludge or liquid.
 (See text.)
2140E

-------
GAS FLOW.
         FILTER
                         CONDENSER
                   CONDENSATE
                      TRAP
TENAX/CHARCOAL
    TRAP
                                   IMPINGERS
                                    XAD-2
                    FIGURE 2.2-3
           MODIFIED SAMPLING TRAIN
         FOR HIGH MOISTURE SAMPLES
                                            VACUUM
                                             PUMP

-------
2.3  BENCH-SCALE TEST OPERATIONS

A detailed operating  procedure  will  be  developed after the final design of
the bench-scale unit and modified during the course  of the system checkout.
The following  sections  outline  some  of the operational  considerations  for
the soil, sludge, and liquid tests.

     2.3.1  Soil Tests

     Typical operation  of  the bench-scale test  aparatus for soil samples
     will involve the following:
     1.  Weigh out appropriate sample size (200-500 grams + 0.5 grams).

     2.  Place the sample  in the kiln barrel  and bolt the  barrel halves
         together.

     3.  Place the kiln barrel into  the  furnace  and attach the thermocouple
         and gas connections.

     4.  Set the  secondary  furnace  temperature and allow  it  to  reach test
         condition temperature before proceeding.

     5.  Switch on the evacuation exhaust pump.

     6.  Establish carrier gas flow at the desired blend and flow rate.

     7.  Start temperature ramp on primary furnace.

     8.  After reaching the desired test temperature on the  primary  furnace,
         start barrel rotation and maintain  desired test  conditions for one
         hour before starting shut down procedures.

     9.  Turn primary furnace off and stop barrel  rotation,  but  continue  gas
         flow.
                                      2-8

-------
     10.  After  primary  furnace has cooled  to 400°C, turn  off secondary
          furnace.

     11.  Divert gas from sampling train and remove collected samples.

     12.  After primary furnace has  cooled to near room temperature, remove
          kiln barrel and disassemble.

     13.  Remove residual sample from barrel.

     14.  Disassemble fly ash collection system and remove fly ash.

     15.  During  the course  of  the system  operation,   the following
          parameters  will  be monitored and  recorded:   N_,  CO-  and 0.
          flow rate  of primary and  secondary gasses, temperature  of the
          rotating kiln gas,  fly  ash separation system exit  gas, secondary
          furnace,  and cooling section  exit  gas,   particulate  sample
          isothermal box and impinger  isothermal  box.   Sample train flow
          meter delta pressure also will be monitored.

     2.3.2  Sludge Tests

     The operation of the bench-scale apparatus during sludge tests would be
     the same  as that for the  soil  tests  except  for those  considerations
     necessary to deal with  the high moisture  content  of the sample.  The
     following additions or changes would be made to the operating procedure:
     1-6.  Identical to soil tests (2.3.1).

       7.  The primary furnace temperature will  be raised to 90°C  and  held
           at this temperature until most of the  moisture  is removed from
           the sample.  The  carrier  gas flow rates  will  be reduced during
           this drying period to compensate for the increased flow rate due
                                      2-9
2140E

-------
          to the water vapor.  This adjustment is necessary  to  maintain  the
          desired residence time of the gases through the secondary furnace.

8-15.  Identical to Soil Tests (2.3.1).

     (Note:   A condensate  trap will  be  placed between  the particulate
              filter and the  sorbant  traps  in the sampling train to remove
              the high load  of  moisture.  The moisture in the trap will be
              analyzed for POHCs).

     2.3.3  Liquid Tests

     Unlike the soils and sludges which would be batch fed,  the liquid waste
     would be  continuously  fed  through a probe  into the  primary furnace
     barrel.   The  desired temperatures  and carrier  gas flows would  be
     established in both the  primary  and secondary  furnace prior  to feeding
     the  liquid  waste.   The  liquid  waste  systems would  consist  of  a
     reservoir and peristaltic pump.   For a  300-gram  liquid sample fed into
     the primary furnace over a 1-hour period,  the sample volume flow rate
     in the secondary furnace would be approximately  30% of  the total  sample
     flow  rate.   This percentage  can be reduced by  slower feed  rates
     occuring over longer periods.
                                     2-10

-------
                         3.0   FEEDSTOCK CONSIDERATIONS
3.1  INTRODUCTION

The  success of  the  bench-scale incineration  test program depends  upon
obtaining samples  containing  the  chemicals to be incinerated in sufficient
quantity  to provide for  the  detection of  very low concentrations  (.01
percent not  destroyed  by incineration).   Such samples  must be obtained for
liquids, sludges, and soils.

The success  of the bench-scale  testing program  depends on the development of
an  adequate database concerning  the soils,  sludges,  and liquids to  be
incinerated.   Furthermore, the success  of  incineration depends  upon
obtaining sufficient  information  concerning the feedstocks to  ensure  safe
and complete destruction.   Feedstock  characterization must be performed with
respect to  physical,  chemical,  and thermodynamic  properties  of the  soils,
sludges,  liquids,  and selected major compounds found  at Basin F.  Of the
materials to be incinerated,  information exists  concerning  most of the
contaminated chemicals themselves  (Table  3.1-1).   However,  this data set is
insufficient to  ensure success, and  data  concerning the  soils,  sludges, and
liquids as a whole are virtually nonexistent.

3.2  SAMPLE CONSIDERATIONS

The  principal  material  to  be incinerated  is  contaminated  soil found  at
Basin F.  Soils  include  both  the  overburden and the soil beneath the 9.5-mm
(3/8-inch)  asphalt liner.   As a  practical  matter, the  soils  to  be
incinerated  will include  the  asphalt liner  as well.   Liquid and sludge
materials exist  in significant  quantities,  but  relative  to  the  soils, are  of
less consequence.

The hazardous chemicals  identified in Table 1.1-1  and  1.1-2 exist in various
concentrations  in  the soils  at Basin F.  Basin  F liquid, however,  is
considered  to be homogeneous.  Similarly, the  sludges are  considered to be
relatively homogeneous.  The concentrations of  chemicals  in soils vary as a
                                      3-1
2140E

-------
          TABLE 3.1-1




PROPERTIES OF SELECTED COMPOUNDS
Chemical Compound
1 Chloropane
1,1 Dichloroethylene
1,2 Dichloroethylene
2 Chloropane
Acetophenone
Aldrin
Arsenic
Benzaldehyde
Benzene
Benzole Acid
Bromo Dichloromethane
Carbon Disulfide
Carbon Tetrachloride
Chlorobenzene
1-Chlorobutane
Chloroform
Chlorohexane
Copper
Cyclohexane
Dieldrin
Dihydroxybenzoic acid (methyl ester)
Dimethyl Disulfide
D imethy loxyethane
DIMP (diisopropylmethylphophonate)
Empirical
Formula

CH2C12
C1CHCHC1
CHjCHClCHj
CHgCOC6H5
C12H8C16
As
f* LJ pi in
i* Ji |JL*nu
C6H6
C g. Hq COOH
PhRrPl
CS2
cci4
C6H5C1
CH3(CH2)2CH2C1
CHC13
C6H13C1
Cu
C6H12
C12H8C16°
W*
CHj-S-S-CHj
CHjOCH^OCHj
C^K-PO,
Molecular
Weight

97
97
79
120
365
75
106
78
122
164
76
154
113
93
119
121
64
84
381
154
94
90
193
Specific State
Gravity (at 25°C)

Liquid
Liquid
Liquid
Liquid
Solid
Solid
Liquid
0.880 Liquid
Solid
Liquid
Liquid
1.590 Liquid
1.100 Liquid
Liquid
1.490 Liquid
Liquid
Solid
Liquid
Solid
Solid
1.060 Liquid
Liquid
0.980 Liquid
Melting
Point (C)


-50

19.7
104 - 105
814
-26
5.5
121.7

-111
-22.6
-45
-123.1
-63.5

1,083
6.5
150
199-200



Boiling
Point (C)

31.6
48
35.3
202.3

615
179
80.1
249
89.2 - 90.6
46.5
76.8
131.7
78
61.26
134
2,324
80.7
175 - 176

109.7 - 115
83
174
Flash
Point (C)

-17.8
2.2
-32.2
82.2


64.4
-11.1
121.1

-30
None
29.4
-9.4
None
35

-20



40

Auto Ignition
Temp (C)

570
460
599.3
571.1


191.7
562.2
571.1

90

638.3
460



245






-------
      TABLE 3.1-1 (Continued)




PROPERTIES OF SELECTED COMPOUNDS
Chemical Compound
Diphenylethane
Dithiane
DMMP (Dimethylmethylphosphonate)
Endrin
Ethoxyethylene
Fluoride
Heptane
He xachlorobenzene
Hexane
Iron
Isodrin
Magnesium
Mercury
Methyl Acetate
Methylacetophenone
Naphthalene
Pentachlorobenzene
Pentachloroethane
Phenol
Phosphorus
Sodium Acetate
Sodium Fluoride
Sodium Hydroxide
Sodium Methyl Phosphonate
Sodium Sulfate
Sodium Sulfate
Empirical
Formula
(C^CHCHj
C4H8S2
W°3
C12H8C16°

F2
CH3(CH2)5CH3
C6C16

Fe
C12H8C16
Mg
Hg
CHjCOgCH,

C10H8
C6HC15
p| y i r*^l
l^rB^irtU'Lii^
C H OH
P
NaC2H^02
NaF
NaOH


Na-SO.
Molecular
Weight
182
120
124
381

38
100
285
86
56
365
24
200
74

128
250
202
94
31
82





Specific State
Gravity (at 25°C)
Liquid
Solid
1.140 Liquid
1.645 Solid

Liquid
Liquid

Liquid
Solid
Solid
Solid
Liquid
Liquid

Solid

Liquid
Solid
Solid
Solid





Melting
Point (C)
-20
108 - 113

235

-218

230

1,535
241 - 242
651
-38.89
-98.7

80.1

-29
40.6
44.1
324





Boiling
Point (C)
272
199 - 200
181


-187
98.5
326
68.7
3,000

1,107
356.9
57.8

217.9

162
181.9
280






Flash Auto Ignition
Point (C) Temp (C)
128.9 440





-3.9 215
242.2
-21.7 225




-10 501.7

78.9 526.1


79.4 715
Spont AI 30
607.2






-------
     TABLE 3.1-1 (Continued)





PROPERTIES OF SELECTED COMPOUNDS
Chemical Compound
Sulfur (Flowers of Sulfur)
Tetrachlorobenzene
Tet rachloroethylene
Toluene
Trlchlorobenzene
Xylene (Ortho, Meta, and Para)
Empirical
Formula
S8
CCljCClj
C6H3C13
CfiH (CHj).
Molecular
Weight
256
216
166
92
181
106.2
Specific
Gravity
2.07
1.73
1.63
0.866

0.861-0.88
State
(at 25°C)
Solid
Liquid
Liquid
Liquid
Solid
Liquid
Melting
Point (C)
119
138
-23.4
-95
63.4
-47.9
Boiling
Point (C)
444.6
245
121.2
110.4
208.5
138.8 - 144.4
Flash
Point (C)
207
155
None
4.4
107
27.2 - 32.2
Auto Ignition
Temp (C)
232
480
—
465 - 530

-------
function  of  borehole location and  depth  (see Appendix C  of the Task 17
Technical Plan).   Most  concentrations are in  the  parts per billion (ppb)
range, although some concentrations are in the parts per million (ppm)  range.

It  is  not essential  that the samples  of soil used  in the bench-scale
incineration  testing  program contain  a representative average  of waste
concentrations.  Average  conditions  may never be encountered in the actual
program.  Rather,  it is  essential  that  the severe  problems  be tested
explicitly.   For this reason, soils  from the area  of  Borehole No. 01 will be
used to test  the  adequacy of the incineration regimes available.  The area
of  Borehole  No.  01 has been chosen because it has not lost its asphalt
liner.  The overburden  is particularly contaminated, and the soils beneath
the. liner also exhibit  significant  levels of contamination.  Borehole No. 01
is  located  in the area known  as "Little F,"  the  area dyked in 1962 and
apparently containing the most problematical  soils and potential sludges as
well as liquids (See Figure 3.1-1).*

3.3  SAMPLE TESTING

Sample testing includes physical,  chemical,  and  thermodynamic properties of
the liquids, potential sludges,  and  soils as well  as  screening for potential
POHCs.  Sample testing, therefore, will occur  in two  phases.  All samples to
be subjected to the bench-scale  incineration system will be  homogenized  and
then  characterized  for  physical,   chemical,  and  thermodynamic (PCT)
properties and potential  POHCs.  Samples  will  be obtained in 15 kg
quantities in  order to provide  sufficient material  for the bench-scale
process plus all characterization studies which must precede it.
 *Note:  Under Task Order No. 6, Environmental Sciences and Engineering (ESE)
  is developing  the  contamination profile  of Basin F  and  soon will send
  Ebasco a copy of the  draft report.   This report will define the locations
  and magnitude of contaminants presently existing in  and  around Basin F.
  Upon evaluation  of the  report, Ebasco  may change  the soil  sampling
  location.
                                      3-2
  /,nc

-------
                                                                          A ALDRIN
                                                                          B DIELDRIN
                                                                          C ARSENIC
                                                                          D ENDRIN
                                                                            ISODRIN
                                                                            FLUORIDE
                                                                          G SULFURS
                                                                          H DBCP
                                                                          X ACTION LEVELS NOT EXCEEDED
                                                                         NO SAMPLE NOT ANALYZED
                                                                          * INDICATES CONCENTRATION
                                                                            EXCEEDS 100X THE ACTION LEVEL
                                                                                    NUMBERS IN PARENTHESIS
                                                                                    DENOTE INTERVALS BELOW
                                                                                    LINER AS FOLLOWS:
                                                                                    (1) = 0.0-1.0 FT
                                                                                    (2) = 1.0-2.0 FT
                                                                                    (3) = 2.0 - 3.0 FT
                                                                                    (4) = 3.0 • 4.0 FT
                                                               X(2)
                                                              NO (3)
                                                              NO (4)
   *— APPROXIMATED^
                                                                      A, B, D (2)
                                                                     31  F(3)
WATER LEVEL
     1982
                    X(2)
                   B, C(3)
                   NO (4)
                                                                       32   X(2)
                                                                            X(3)
                                                                          NO (4)
                                                                                    AD(1)
                                                                                     X(2)
                                                                                    NO (3)
                                                                                    NO (4)
                                   C(2)
                                 A,D(3)
                                   X(4)
                                                               X(D 22
                                                               X(2)
                                                               X(3)
                                                             NO (4)
                                                                               A.B.C. D, E(1)
                                                                                 A, C, D, F (2)
                                                                               A, B, C. D, f (3)
                                                                               A, B, C, D, F (4)
                                                                            A*B*C, D*E*F, G,
                                                                              A, B*C. D, E, F, G (2) 02
                                                                                A, B, C, D, F, G (3) •
                                                                                  A, C, D, F, G (4)
                                               C(2)
                                              NO (3)
                                              NO (4)
  LIQUID
  BORING LOCATIONS
                                              Figure 3.1-1
                                       SOIL SAMPLING LOCATION
SOURCE: MYERS AND THOMPSON. 1982

-------
     3.3.1  Feedstock Characterization

     The feedstock characterization program is designed to define  those  PCT
     properties essential for understanding the bench-scale program  and  for
     contributing to  the larger-scale operations.  Such  characterizations
     are not intended to provide a complete listing of  properties, but only
     such a listing as is essential for safe and cost-effective operation of
     the system.

     Certain physical and  chemical properties have already been  partially
     determined for the  hazardous  chemicals to be destroyed and removed by
     incineration.  Some  of these  properties include  chemical formula,
     molecular weight,  melting point,  boiling point,  flash  point,  and
     autoignition temperature.   Heats  of combustion  either have been
     determined or calculated,  as will be shown in Chapter 4.

     Critical parameters  are those describing the matrix containing the
     hazardous  chemicals.    Those  parameters  requiring  definition   are
     identified below:
     Material
Parameters to be Determined
     Soils (including
     overburden and liner)
Specific heat
Heat capacity
Thermal conductivity
Moisture content
Ash fusion temperature
     Sludges
Viscosity
Moisture content
Ash fusion temperature
Distillation curve
     Liquids
Viscosity
Corrosivity (with respect to refractory)
2140E
                                   3-3

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     These  parameters  will  be  determined, to  the greatest  extent
     possible, in  the  evaluation of the samples prior  to  bench-scale
     incineration testing.

     3.3.2  Analytical Screening for Potential POHCs

     Samples collected for test incineration from Basin F will include:

     o  Soil;
     o  Sludge; and
     o  Liquid.

     Nonhomogeneity of  the collected samples is  expected  due to the
     wide variability in  soil type and multi-phase characteristics of
     the  liquid/sludge  in Basin  F.   As the  lagoon evaporates, the
     liquid/sludge portion of the basin becomes more concentrated with
     organic  and  inorganic  constituents.   As  a  result,  the
     concentrations of  these compounds  can be expected to vary widely
     across the basin area.   Therefore, the samples taken and delivered
     to the laboratory will not be homogeneous.

     An initial screen  of the samples may be performed on aliquots of
     each matrix  that   has been made as homogeneous  as possible by
     mixing.   Enough  sample   of  each matrix type  will  be  collected,
     homogenized,  and stored at  the  Hittman/Ebasco laboratory at 4°C  or
     less to use for all  incineration tests.  Chemical  characterization
     of waste  samples  is critical to  evaluating the destruction and
     removal efficiency (ORE) of incineration  tests.   The most effi-
     cient and cost effective means of characterizing the waste is to:

         1.  Combine all samples received by matrix into one bulk sample.

         2.  Homogenize by mixing or agitating the bulk sample.*

* The effectiveness of this process will be evaluated.  If found to be
  unsatisfactory,  alternate procedures will be investigated.
                                       3-4

-------
         3.  Prepare aliquots from each bulk matrix for analytical screen.

         4.  Ship aliquots to appropriate laboratory.

         5.  Determine the constituent concentration.

    Soil, sludge, and liquid  samples  will be assayed  semiquantitatively by gas
    chromatography/mass  spectrometry  (GC/MS)  for  volatile and  semivolatile
    organic target analytes.  An  attempt will  be made to identify other major
    unknown peaks present  in  the  GC/MS  total  ion current profiles.  Potential
    unknown analytes will  be  tentatively identified, if possible.   Collected
    samples will  also  be  assayed  quantitatively by graphite furnace  atomic
    absorption  spectroscopy for  arsenic,  by cold  vapor atomic  absorption
    spectroscopy  for  mercury, and  for  other  target  metals by  inductively
    coupled argon  plasma  (ICP) emission spectroscopy.   Soils,   sludges,  and
    liquids will  be  characterized in terms of ignitability, corrosivity,  and
    reactivity.
                                       3-5
2140E

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                       4.0  SELECTION OF TEST PARAMETERS
4.1   INTRODUCTION

The  planned  bench-scale  test  consists  of  20  test  burns,  largely on
contaminated  soils but  also  including sludges and liquid from Basin F.  The
20 test  burns are  necessary  due to the multiple runs required to adequately
test  for all  major contaminants regardless  of concentration.  Such  testing
will  lead  to  the ultimate selection of POHCs for pilot-scale and full-scale
operations.

A bench-scale test matrix was  developed  recognizing the typical operating
parameters  for hazardous  waste incinerators capable  of  handling  chemically
contaminated  solids.  These  representative parameters are as follows  (from
Frankel, Sanders, and Vogel 1983).

                       	Type of Incinerator	
Parameter              Rotary Kiln     Fluid          Hearth

Temperature of
Primary Chamber (°C)   280-1,280        750           560-900

Temperature of
Afterburner (°C)       900-1,600        N/A           1,000-1,600

Residence Time
in Primary Chamber     2 hrs           0.75-2.5 sec   10-30 min

Residence Time
in Afterburner         1.3 sec         N/A            2 sec

The parameters shown by  Frankel  et  al.  are not the only ones utilized in or
reported for  incineration.   Other authors have shown afterburner  residence
times of up  to  5 seconds for  gases evolved in primary incinerators.   For
example, Bonner et al. (1981) report that

-------
afterburner  residence  time requirements may  be  0.2-6.0 seconds depending
upon  the  waste being destroyed.   Bonner  also reports varying temperature
regimes  depending  upon  technology.   The temperatures  reported for  a
fluidized bed  in  Bonner  et al. (1981) are 450-980°C.  These are consistent
with, but broader than,  the  temperatures  previously  mentioned.  Dellinger et
al.  (1984)  gives  typical afterburner conditions of  2-4 seconds (out of a
potential range of 1-12 seconds) and bulk gas temperatures of 600-1,100°C.

The  basis for  the  parameters also  includes optimal  fuel combustion
conditions as  discussed  in Kramlich et al.  (1984),  focusing on excess 0_
in the stack gas  at  5.4  percent (35 percent excess air), and an upper bound
of approximately  7  percent  0_ in  the  stack (corresponding to  about 50
percent excess  air).  The basis of the parameters includes  the  limitations
of the laboratory equipment, identified as follows:

     1.  Maximum primary chamber temperature, 800-1,000°C
     2.  Maximum practical afterburner temperature, 1,250°C

The  basis of the  test matrix  also  includes the goals  of:  1) obtaining
sufficient  spread in  the parameters  to  develop  first  order  kinetic
approximations of destructive  mechanisms  (a  problem  with the residence times
of the MRI  experiments);  and  2)  obtaining at least  one regime where ORE
levels of 99.99 percent are reasonably assured.

4.2  TEST MATRIX PARAMETERS

The  test matrix  parameters  involve  varying residence time  in  the
afterburner, temperature  in  the afterburner,  and  0_ concentration  in the
carrier gas.  These  parameters  are summarized as follows:

                        	Value
Parameter

Time (sec)
Temp (°C)
Minimum
2
900
5.4
Maximum
5
1,250
7.0
                                      4-2
2140E

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         Additional runs will  be made at  65Q°C,  as discussed below,  in  order to
\,        ensure that some regimes will be  tested  that  will  not succeed.   These runs
         will be at 2 and 5  seconds  residence  time  in  the afterburner, but will only
         be at 5.4% 0. concentration.

         The basis for each parameter is  summarized  below.

              A.2.1  Selection of Time Parameter

              The variation  in residence  time  is based upon  the values in  the
              literature.   The minimum value of 2 seconds  appears in  virtually all
              scientific and  engineering  materials concerning  hazardous  waste
              incineration.   Dellinger et  al.  (1984),  for  example,  reports  the
              temperature  to achieve destruction  of a compound  at a ORE of  99.99
              percent in 2  seconds  (see Table 1.1-3).  The  residence time  of 2
              seconds is also  consistent with  the data presented by Frankel  et al.
              (1983) for afterburners being operated commercially,  as shown above.

•-.             The maximum value  of 5 seconds  appears to be a  practical upper limit
              based upon the bench-scale apparatus  and the  need for firing 300-500
              grams of contaminated  materials  per test to  fairly simulate  larger-
              scale operations.  The 5-second value appears near the upper end of the
              scale presented by Bonner  et al.  (1981).   Further, the spread between
              2 seconds  and  5  seconds provides sufficient range  to  achieve  a fair
              extrapolation  to  6 seconds  should such an extrapolation be necessary.

              4.2.2  Selection  of Temperature Parameter

              The laboratory-scale operations  will  use  a  primary chamber  (Linder
              furnace)  temperature of 1,000°C,  or  as close to  that  as  can  be
              achieved.   It is expected  that the  actual  temperature reached will be
              between 800  and 1,000°C, rather than the peak  value.  This  temperature
              is consistent with the values reported by Frankel  et  al.  (1983) for
              rotary kilns  and hearth type furnaces and the values reported by Bonner
              et al.  (1981)  for  fluidized bed furnaces.   The  final  temperature
              selected  could well be limited by the feedstock tests concerning  ash
              fusion temperatures of  the  soils  to  be fed.

                                              4-3
         21AHF

-------
The first temperature in the afterburner, 900°C, is consistent with the
minimum afterburner  temperature  reported  by Frankel et al. (1984) for
afterburners associated with rotary kilns.   Further,  it is consistent
with the  literature  concerning temperatures required to achieve 99.99
percent destruction  (see,  for  example,  Dellinger et al. 1984 as shown
in Table  1.1-3).   It presents  a minimum temperature below which 99.99
percent ORE is probably not achievable.

The maximum temperature in  the afterburner,  1,250°C,  represents a
practical upper limit of the bench-scale  equipment.   Further,  it is in
the middle  of the  range for  afterburners  as reported by Frankel et al.
(1984).  Because there  is  a 350 Centigrade degrees spread between the
minimum and maximum temperatures,  there  is  considerable  reason for
confidence  in extrapolating  the results to higher temperatures  (e.g.,
1,500°C) should such extrapolation prove necessary.

A third temperature, 650°C, has  been chosen as  a minimum value for test
purposes.    This temperature  is consistent with the low end  of values
shown for afterburners.  Further,  it is at  the low end of temperatures
where 99.99 percent  ORE for hazardous organics is  achieved as shown in
Dellinger et  al.   (1984).   The temperature of  650°C  is designed to
provide a failure  to achieve 99.99 percent ORE for some (but not all)
compounds in  order  to  provide the most  effective data for kinetic
calculations.  Tests run at 650°C  will  be at  2 and 5 seconds, but will
only be at 5.4 percent 0_ in the carrier gas.

The third  temperature  provides a matrix  of six points  for the
establishment of time and temperature  requirements  to incinerate the
soils.  The matrix appears as follows:
                              4-4

-------
Minimum
650°C
650°C
Intermediate
900°C
900°C
Maximum
1,250°C
1,250°C
                        	Temperature
         Time

         2 seconds
         5 seconds

A.2.3  Oxygen Concentration

Oxygen concentration is  a  parameter chosen to determine the  level  of
excess air  which is optimal  in firing  of the  supplementary fuel.
Oxygen concentration is  varied  in  the  carrier  gas as a means of making
the bench-scale  tests  most representative of  the postflame oxidation
regions  as   well as the pyrolysis  region.    Oxygen  concentration
influences not only  the  temperatures achieved in the  flame (see,  for
example,  Babcock and Wilcox (1978)  for  a correlation between excess
0   and  flame  temperature),  but  also influences  the degree  of
completeness of  combustion  and  the minimization  of PIC formation.   The
correlation  between  excess  air  and excess 0_  in  the dry  stack gas is
shown in the following equation (Babcock and Wilcox 1978):
    XEA = 100 x (02 - 0.5 CO)/(.264N2 - (02 - 0.5 CO)           (1)

Where %EA is  percent  excess air,  0_ is percent oxygen in the  dry
stack gas, CO is  percent  carbon monoxide  in the dry  stack gas,  and
N_  is percent  nitrogen  in the  dry stack  gas.   For  these
calculations, the CO  term can be  ignored  because  proper combustion
reduces CO to  less  than  .002-.005% at an absolute maximum  (20-50
ppmv  CO).   Nitrogen  concentration  can  be taken  at  79 percent.
Consequently, the expression can be simplified to the following:
    %EA = 100 x 02/(20.856-02)                                  (2)

Solving this  equation for various levels  of  excess air provides
the following values:
                              4-5

-------
           SEA    %02
25
30
35
40
50
75
4.2
A. 8
5.4
6.0
7.0
8.9
     The research by Kramlich  et  al.  (1984) previously cited demonstrates
     that PICs are minimized and DREs are maximized with  excess  air  in the
     30 to 40 percent range.  Below and above  that range,  PICs  increase in
     dramatic quantities,  as is shown  in Figure 4.2-1.

     The minimum concentration of 02  in the stack gas is  selected at 5.4
     percent, corresponding  to  the  apparent  optimal  value shown  in
     Figure 4.2-1.   This  level  can be set  for the  carrier gas  in  the
     experiment.   It corresponds to a C02  level of  15.6 percent.  Further,
     because 5.4 percent 02  is  an apparent  minimum point,  selection  of any
     value below this depiction of 35 percent excess  air would seriously
     distort efforts at limited extrapolation.  Such distortions  would make
     the results of excess  air  levels greater  than  35-50 percent appear to
     be more favorable than would be expected under actual operations.

     The maximum concentration  of 0_  is  set at 7.0 percent,  corresponding
     to common firing practices  of  many combustion  systems.  Further, this
     representation of 50  percent  excess  air represents a  practical upper
     bound beyond which ORE  levels of 99.99 percent could not practically be
     expected (see, for example, Figure 4.2-1).  Finally, the spread  between
     35 and  50 percent excess  air  does  provide sufficient data for  limited
     extrapolation to levels between 50  percent and  75 percent.

     It should be  noted  that  the  values  of 5.4  percent  and 7.0 percent
     represent oxygen  concentrations  expected  for  the postflame region.
     Should it become necessary in order to demonstrate 99.99 percent ORE,
                                      4-6
21AOE

-------
     ^2000

     (U
     0>
     >»
     X
     o

     I/I
     I/I
     0)


     5 1500
o

o
4->


V
     o
     o>
       1000
     •o
     c
     03

     l/t
     c
     o
     o
     o

     •o
  500
             O  co

             A  Hydrocarbons as CH^

             Q  Test Compound (Average of four)
         100
                                     0.02
                                           0.02
                                              
-------
     one experiment will be  run  at  5 seconds and 1,250°C with  air  as the
     carrier gas in  order  to more  closely  approximate flame mode  oxygen
     concentrations.

     4.2.A  Test Execution

     The regimes established above will be tested on the contaminated soils
     fractions.   Two runs will be made per sample in selected cases in order
     to ensure  adequate  data on all  hazardous  organics identified.  Such
     tests will be run  at  1,250°C for 5 seconds at 5.4% 02,  1,250°C  for  2
     seconds at 5.4% CL, 900°C  for  5 seconds at 5.4%  02>  and 900°C for 2
     seconds at 5.4% 0  .   POHCs  will be selected for  single run tests at
     7% 0   in the carrier  gas,  and  for  tests  at 650°C.   Once a rough
     optimum regime has  been determined for contaminated soils, it will be
     tested on  the  liquids  (where two  runs  are contemplated),  on sludges
     (two runs), and on  a  proportionate mixture of all materials found at
     Basin F.   The two  runs on the proportionate mixture  of all materials
     will  be  at  5 second  residence time  and  at  900°C  and  1,250°C
     temperatures in the afterburner.

4.3  SELECTION OF PRINCIPAL ORGANIC  HAZARDOUS COMPOUNDS (POHCs)

POHCs are  used  as compounds  that can measure  the  fate of all  hazardous
chemicals to be destroyed.   They are  chosen based upon thermal  stability  and
concentration.  Various  ranking  schemes commonly proposed  for the selection
of POHCs include:

     o  Heat of combustion of the hazardous chemical;
     o  Autoignition temperature;
     o  Theoretical kinetics; and
     o  Thermal decomposition data.

Each methodology  has its  strengths and  weaknesses.   Heat  of  combustion
permits  evaluation  of all  compounds either  by experimentally  determined
values  in  kcal/g,  or by calculated values.   Heat of  combustion,  however,
does not deal with the issue of thermal stability.  Autoignition
                                      4-7

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temperature,  theoretical  kinetics,  and thermal  decomposition  data provide
additional  insights.   Unfortunately,  the database  is  incomplete for such
properties with respect to the compounds found in Basin F.

The U.S.  Environmental Protection Agency (EPA) utilizes heat of combustion
for selection of POHCs according to the following formula:

    POHC rank = (%C) + 100/Hc                                        (3)

Where %C represents percentage of concentration  in  the waste and He is
heat of combustion in  kcal/g.  This formula  is used here  in  the  absence
of more analytically  precise kinetics and thermal  decomposition data.
It is  used  to recognize that He  and  thermal stability are not neces-
sarily  correlated.   This  formula is more  sensitive  to  He than
concentration with respect to Basin F wastes due to the low concentra-
tions of materials (typically in the ppb and ppm ranges).

Table 4.3-1  is  a  compilation of heats of combustion for the hazardous
organics in  the soils  sampled at  Boring No.  1 and in the liquids found
in Basin F.   Of these,  aldrin has an  He of 3.75 kcal/g and endrin, has
an He  of  3.46 kcal/g  (Dellinger et al. 1984).  These  chemicals, along
with dieldrin,  can  be classified as  POHCs.   Because of the critical
nature of these tests,  however,  and the lack of absolute precision  in
using  the  He value to determine appropriateness  of  any  POHC with
respect to  incinerability,   the  bench-scale  tests  will  be performed
initially for all identified compounds in  the  soils obtained  from
Basin F Borehole No.  01.   This  testing for all  compounds necessitates
multiple (4)  runs.  Based on these runs, the POHCs  will be  determined
for the remaining tests.
                                   4-8

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                                 TABLE 4.3-1
                                                           I/
                 HEATS  OF  COMBUSTION  FOR  HAZARDOUS  WASTES -
Compound
VOLATILE HALO ORGANICS
Chloroform (trichloromethane)
1,1 - Dichloroethane
(ethylidene chloride)
1,2 - Dichlorethane
(ethylene chloride)
1,1,1 - Trichloroethane
(methylchloroform)
1,1,2 - Trichloroethane
(vinyltrichloride)
Tetrachloroethylene
(perchloroethylene )
Carbon tetrachloride
(tetrachloromethane)
1,2 - Trans-dichloroethylene
(acetylene dichloride)
Dichloromethane
(methylene chloride)
Hexachlorobutadiene
Hexachloroethane
VOLATILE AROMATICS
Benzene (benzol)
Toluene (methylbenzene)
Xylene (0-Xylol)
Ethyl benzene (phenylethane)
Formula

CHC13
CH3CHC12
C1CH2CH2C1
CH3CC13
C12CHCH2C1
C12CCC12
CCl,
C1CHCHC1
CH2C12
C«C16
C2C16

C6H6
C6H3CH3
C6H^(CH3)2
C6H5C2H5
Btu/lb

1,350
5,405
5,405
3,585
3,585
2,145
430
4,865
3,065
3,820
830

18,070
18,270
18,450
18,500 2/
Kcal/gram

0.75
3.00
3.00
1.99
1.99
1.19
0.24
2.70
1.70
2.12
0.46

10.03
10.14
10.24
10.27
2140E

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                           TABLE A.3-1 (Continued)



                 HEATS OF COBUSTION FOR HAZARDOUS WASTES
Compound
CHLORINATED AROMATICS
Chlorobenzene (phenyl chloride)
Hexachlorobenzene
(perchlorobenzene)
1,2,3,4 - Tetrachlorobenzene
1,2,4 - Trichlorobenzene
1,2 - Dichlorobenzene
ORGANOCHLORINE PESTICIDES
Aldrin "kl
Endrin 4/
Dieldrin ^J
Isodrin &
Chlordane ~U
Malathion &/
Parathion 2/
Azodrin (monocrotophos)
Vapona (DDVP) iS/
Hexachlorocyclopentadiene
Atrazine il/
DDTI2/
DDE13/
Oxathiane
Formula

C6H5C1
C6C16
C6H2Cl4
C6H3C13
C6H4C12

C12H8C16
C12H8C160
C12H8C160
C12H8C16
C10H6C18
C10H1906PS2
C10H1AN05PS
C6HU05NP
C4H7C12O^P
C5C16
C8H1AN5C1
(C1C6H^,)2CHCC13
C14H8C14
N/A
Btu/lb

11,890
3,225
4,700
6,125
8,235

6,755
6,235
10,200
N/A
4,880
N/A
6,505
N/A
N/A
3,785
N/A
8,125
9,100
N/A
Kcal/gram

6.60
1.79
2.61
3.40
4.57

3.75
3.46
5.66
N/A
2.71
N/A
3.61
N/A
N/A
2.10
N/A
4.51
5.05
N/A
2140E

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                           TABLE 4.3-1 (Continued)
                 HEATS OF COtffiUSTION FOR HAZARDOUS  WASTES I7
       Compound                 Formula                 Btu/lb     Kcal/gram
Dithiane                        N/A                        N/A         N/A
Nabam M/                       C^H^NaS^
Maneb il                        C^H6MnN2S4
Zineb ii/                       C4H6MnN2S4Zn
NONCHLORINATED ALIPHATIC SOLVENTS
Methylethyl Ketone (butanone)   C4H80                   14,538        8.07
Acetone (propanone,             C3HgO                   13,300 27     7.38
dimethyl ketone)
Methylisobutyl Ketone (hexone)
Dimethyldisulfide
(2,3,-dithiabutane)
OTHERS
Acetonitrite (methyl cyanide)
Acrylonitrile (vinyle cyanide)
Methane
Pyridine
Ethane
Aniline (phenylamine)
Nitrobenzene
(CH2)2CHCH2COCH3
CH3-S-S-SH3

CH3CN
CH2CHCN
CHA
NCHCHCHCHCH
C2H6
C6H5NH2
C6H502N
N/A
N/A

13,280
14,285
23,879 2/
14,105
22,320 U
15,730
10,810 2/
N/A
N/A

7.37
7.93
13.25
7.83
12.39
8.73
6.00
I/  All heat  contents from  determination  of the  thermal decomposition
    properties of 20  selected  hazardous  organic  compounds Dellinger  et  al.
    1984.
2/  Chemical Processes.  Felder and Rousseau.  1978.
3/  l,2,3,4,10,10-hexachloro-l,4,4a,5,8,8a-hexahydro-l,4,5,8-dimethanon
    aphthalene
2140E

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                           TABLE A.3-1 (Continued)
                 HEATS OF COMBUSTION FOR HAZARDOUS  WASTES I/
4/  l,2,3,4,10,10-hexachloro-6,7-epoxy,l,4,4a,5,6,7,8,8a-octahydro
    1,4,5,8-endo-endo,dimethanonaphthalene)
5/  l,2,3,4,10,10-hexachloro-6,7-epoxy-l,4,4a,5,6,7,8,8a-octahydro-l,4,5,8-
    dimethanonaphthalene
6/  1,2,3,4,10,10-hexachloro-l,4,4a,8,8a hexahydro-1,A,5,8-endo-
    dimethanonaphthalene
7/  1,2,4,5,6,7,8,8-octachloro-A,7,methano-3a,4,7,7a-tetrahydroindane
8/  S - (1-2 dicarbethoryethyl) 0,0-dimethyldithiophosphate
9/  0,0-dietlyl 0-P-nitrophenylphosphorothioate
10/ 0,0-dimethyl 0-(2,2-dichlorovinyl phosphate)
ll/ 2-chloro-4-ethylamino-6-isopropyl amino-s-triazine
12/ l,l,l-trichloro-2,2-bis(p-chlorophenyl) ethane
137 l,l-dichloro-2,2-bis-(p-chlorophenyl)ethylene
14/ Ethylenebis (dithiocarbamic acid) disodium salt
15/ Manganous ethylenebis (dithiocarbonate)
16/ Zinc ethylenebis (dithiocarbamate)
2140E

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4.4  SELECTION OF ANALYTICAL PARAMETERS

The analyses that will be  performed  to achieve  the objectives of the waste
incineration tests were selected to meet the following  criteria:

     o  Maximize the information;
     o  Minimize number of analytical procedures;
     o  Utilize current laboratory certification;  and
     o  Minimize certification efforts.

The analytical program will support four (4) phases of  testing:

     o  Initial screen of waste feedstock;
     o  POHC evaluation tests;
     o  Incinerator optimization tests; and
     o  Incineration under optimum conditions.

The complete  organic  analysis will  be performed  for  four  (4)  test burns
which will  cover the  full  range  of  test  conditions  to establish the
appropriate POHCs.  The  initial screen  of  the  feedstock wastes  has been
discussed in  Section 3.2.2.   Optimization of  the incinerator operating
conditions  requires rapid  analytical  response  to  guide  subsequent test
burns.   To  achieve a  rapid  turn-around  of the results  during  the
optimization phase, only POHCs will be tested  for  in the  feedstock,  the
solid residue  fraction,  and the  off-gas.   These analyses  will  not be
certified but  will be performed using approved  methods.   However, while
certification may not  be necessary,  some demonstration of  the  laboratory's
ability to detect the required levels will be required.

The 99.99% ORE  level in  the optimization phase  and optimum conditions phase
will  be  determined from  the initial  feedstock screening  analyses.  The
99.99% ORE level, will be  used to determine the analytical detection limit.
The actual  DREs will  be calculated  for the POHC  from the  analysis of  the
individual feed sample.
                                      4-9
2140E

-------
         A table of  99.99% ORE  levels will be calculated from the initial feedstock
v        screening data  for all POHCs  that  are selected for  analysis  during the
         optimum conditions  phase.   After the  optimum  conditions  for incineration
         have been established, the  following analytical procedures will be performed
         at HEAI on the feedstock and the incineration by-products:

              o  Chlorinated Hydrocarbon Analysis (GC/ECD)
              o  Organosulfur Compound Analysis (GC/FPD)
              o  Organophosphorous Compound Analysis (GC/NPO)
              o  Volatile Organic Analysis (GC/PID and GC/Hall detector)
              o  Hydrogen Halides (F~ & Cl")
              o  Cyanide (Distillation/Colorimetric)
              o  Metals (Arsenic by  furnace AA, Mercury  by  cold vapor AA, general
                 metals by ICP)
              o  GC/MS Screen

         Furthermore, the above procedures will be  used to analyze data for feedstock
         at the time of each optimum conditions burn.   Because HEAI  has not proposed
         to certify  the  above methods,  the  data resulting  from the analysis can
         provide only a rough estimate  of the quantity of analyte present.  This will
         be necessary to establish the  best  estimate of POHC concentration at time of
         the burn.   The  incineration off-gas and residues will be tested to  acquire
         quantitative data  to better estimate  the destruction and removal efficiency
         at optimum conditions.

         A more detailed  discussion  of the  procedures  is  described  in Section 5.2.
         The methods were  selected based upon the  ideal instrument  detection limits
         that each  procedure is  capable of producing  under optimized analytical
         preparatory conditions.

         A GC/MS  screen  of  the  organic fraction of the  incineration gas sampling
         train and of  the solid residues  will  be performed on  selected test runs.
         This screen will  not continue  to be utilized  if  the desired detection  limits
         cannot be  achieved.  However,  through a GC/MS  screen,  more data may  be
         aquired about compounds which  are detected but  not  identified by  the GC/EPD,
Vs-k
         NPD, FPD, or Hall detector  analyses.
                                              4-10

-------
                            5.0  ANALYTICAL  DETAILS
5.1  SAMPLE HANDLING AND SAMPLE FLOW

Hittman/Ebasco Associates Inc. (HEAI) will be  the  lead laboratory on sample
handling and processing.  Samples  shipped from the field will be  homogenized
and properly stored under refrigerated  conditions  by  HEAI  until analysis or
incineration testing.   For  initial feedstock  analysis, the  sample will be
shipped  by  overnight  express  to  the approved laboratory.  Figure  5.1-1
illustrates the flow of the sample from RMA to the laboratories for analysis.

The soil sample collected will be  from  a known area of high  contamination  to
facilitate the bulk homogenization and storage of one sample.   Sludge and
liquid  samples  should be of  a more consistent  contaminant  concentration
range, although "hot" spots can be expected.   After aliquoting  for feedstock
analysis, the samples will then be aliquoted into  separate bottles for each
test  incineration  run.   The samples will be maintained in  tightly  sealed
glass containers under  refrigerated  conditions.   The  lid  of each container
will be wrapped with  Teflon tape and then a  layer  of  parafilm around that  to
prevent loss of volatiles.  However, it can  be assumed that  some  contaminant
concentration  levels  will  drop  during this  period  of optimizing the
incinerator burns.

The laboratories performing analyses will be CAL,  UBTL, and  HEAI.  HEAI will
have the lead on sample  preparation  and shipment for feedstock analyses.  A
full  set of  organic  and metal analyses will be  performed on each initial
soil, sludge, and  liquid feedstock sample.   HEAI will be responsible for all
incinerator  test   burn  sample analysis.   The solid   and  gas   fractions
collected from  the test burns will  be analyzed by  methods developed  at
HEAI.   Table  5.1-1 summarizes in  tabular  form,  the  tests which  will  be
performed and Table 5.1-2 summarizes the number of analyses  to  be performed.
                                      5-1
91 />or

-------
VGA/Matrix
 to CAL
                    Sample Shipped
                       from RMA
                         I
                     Received by
                        HEAI
                   Samples combined
                    by Matrix type
                         I
                     Bulk  sample
                     Homogenized
                         I
              Analytical and  Incineration
                 Test Aliquots Prepared
                         I
semi-volatile/matrix
   to HEAI
                   Results to HEAI
                  Incineration tests
                         I
                       Analysis
metal/matrix
 to  UBTL
                  FIGURE 5.1-1
      SAMPLE ANALYTICAL  FLOW

-------
     TABLE 5.1-1



ANALYTICAL METHODOLOGY
Analysis/Matrlx/Analytes
Volatile Organlcs/Sollds
1,1-Oichloroethane
Dlchl o row thane
1 , 2-Olchloroethane
1,1, 1-Trichloroethane
1,1, 2-Trichloroethane
Carton tetrachloride
Chloroform
Tetrachloroethylene
Trichloroethylene
Trans-1 , 2-Oichloroethylene
Benzene
Toluene
Xylene (3 isomers)
Ethylbenzene
Chlorobenzene
Methylisooutyl ketone
Dlmethyldisulfide
Blcycloneptadiene
Dlcyclopentadiene
Semi-Volatile Organics/Solids
Aldrin
Endrln
Oieldrin
Isodrln
p.p'-OOT
p.p'-OC
Chlorophenylmethyl sulfide
Chlorophenylmethyl suUoxide
Chlorophenylmethyl sulfone
Detection
Limit*

o.s ug/g
O.Sug/g
0.5 ug/g
0.5ug/g
0.5 ug/g
0.5 ug/g
0.5 ug/g
0.5 ug/g
0.5 ug/g
0.5 ug/g
0.5 ug/g
0.5 ug/g
o.s ug/g
0.5 ug/g
0.5ug/g
0.5 uq/9
0.5 ug/g
o.s ug/g
0.5ug/g

0.5 ug/g
0.5 ug/g
o.s ug/g
O.Sug/g
0.5 pg/g
0.5ug/g
0.5 ug/g
o.s ug/g
0.5 ug/g
High Range Level of
Concentration Hold Time Certification Reference Methods
7 days for Semi- EPA 624 (2)
25 u g/g the solid Quantitative (A) EPA 8240 with
25ug/q and 40 days EPA 5030
25 ug/g for the extraction (1)
25 ug/g extract (1) CAL-K9
25 ug/g
25 ug/g
25 ug/g
25 ug/g
25 u g/g
25 ug/g
25 ug/g
25 ug/g
25 ug/g
25 ug/g
25 ug/g
25 ug/g
25 ug/g
25 ug/g
25 yg/g
7 days for Semi- EPA 8270 with
100 ug/g the solid ft Quantitative (A) EPA 3540
100 ug/g 40 days for extraction (1)
100 ug/g the extract HIAI-X9-A
loo ug/g (l)
50 ug/g
100 ug/g
loo ug/g
50 uo/cj
100 ug/g
Principle of Method
A 10 gram portion of the sample is obtained with
a minimum of handling. The sample is shaken for
4 hours with 10 ml methanol. An aliquot of the
methanol extract Is Injected into 5 ml of water
and analyzed by purge-trap GC/MS using a packed
column. Surrogates and internal standards are
used. Unknowns are identified.

Surrogates are:
d2 - Methylene chloride
1 ,2-Oichloroethane-d4
djQ - Ethylbenzene


The internal standard will be
1 , 2-dibromoethane-d^ .




A 15 aram portion of the sample is obtained with
a minimum of handling and mixed with 30 grams of
anhydrous sodium sulfate. The sample is soxhlet
extracted for 8 hours with 300 ml of methylene
chloride. The extract is reduced to a final
voline of 10 •! In a K-0 aparatus. An aliquot
of the extract is analyzed by fused silica
capillary colim GC/MS. Surrogates and internal
standards are used. Unknowns are identified.


-------
                                                                              TABLE 5.1-1 (Continued)
Analysls/Matrlx/Analytes
Hexachlorocyclopentadlene
Oxathlane
Olthlane
Malathion
Parathlon
Chlordane
Azodrin
Vapona
Supona
OIMP
Atrazlne
ICP Metal Screen/Solids
Cadmium
Chromium
Copper
Lead
Zinc
Aluminum
Iron
Detection
Limit*
0.5 ug/g
0.5 ug/g
0.5 pg/g
0.5 \ig/g
0.5 ug/g
0.5 ug/g
0.5|ig/g
0.5 ug/g
0.5 ug/g
0.5 ug/g
0.5uq/g

0.5 ug/g
5 ug/g
5 ug/g
5 ug/g
5 ug/g
Interelement
Interelement
High Range Level of
Concentration Hold Time Certification Reference Methods
100 ug/g
100 ug/g
100 u g/g
loo ug/g
100 ug/g
100 y g/g
100 u g/g
100 ug/g
100 ug/g
so ug/g
loo ug/g
6 mos (5) Quantitative (B) USATHAMA 7S
500 ug/g UBTL-P9
500 ug/g
500 ug/g
500 ug/g
500 ug/g
Correction
Correction
Principle of Method
Surrogates are:
d^-1 , 3-Oichlorobenzene
d^-Diethylphthalate
d^-2-Chlorophenol
d4 Di-n-Octyl Phthalate
The internal standard will be d,0 Phenanthrene



A 1 gram portion is digested with 3 ml repeated
portions of KNO? and finished with HC1. The
sample is filtered to a final volume of 50 ml.
The sample Is analyzed by ICP.

•


Arsenic/Solids
10 ug/g     6 mas       Quantitative  (B)  EPA 7060 with
                                          EPA 3050
                                          extraction (2)
                                          UBTL-B9
A one gram portion of the  sample Is digested with
       HN03.   The digest is analyzed by GF/AA.

-------
                                                                  TABLE  5.1-1  (Continued)
Analysis/Matrix/Analytes
Detection    High Range                   Level of
  Limit*    Concentration  Hold Time    Certification     Reference Methods
                                                                                                                                           Principle of Method
Mercury/Solids
O.lgg/g        1 gg/g     28 days (5)   Quantitative (B)   EPA 245.5 (5)
                                                          UBTL-Y9
                                A one gram portion is weighed out  and treated
                                with aqua regla followed by potassium perman-
                                ganate.  Excess permanganate is reduced with
                                hydroxylamlne sulfate.  The mercury  is reduced
                                with stamous chloride and determined using the
                                cold vapor technique.
Extraction Procedure Toxiclty
Incinerator Residues/Solids
                           7 days
                                        None
EPA 1310(1)
EPA Method C004 (6)
HEA1
A 100 gram portion of incinerator residues is
extracted for 24 hours with 1.6 liters  of
deionlzed water which is maintained at  pH
5-0.2 using acetic acid.  The extract is
analyzed by USATHAMA certified liquid methods
shown in Table 6.1-2 for the eight elements,
four pesticides and two herbicides listed in
40 CFR 261.24.
Ignltablllty/Sollds
                           7 days
                                        None
Corrosivity/Solids
                           7 days
                                                                           None
EPA 1010(1)
EPA Method COO2 (6)
ASTM Method
093-77
HEAI
EPA 1110(1)
EPA Method C002(6)
NACE Standard
TM-10-69
HEAI
A sample is heated at a slow constant  rate with
continual stirring in a cup.  A small  flame is
directed into the cup at regular Intervals with
simultaneous interruption of stirring.  The
flash point is the lowest temperature  at which
application of the flame ignites the vapor above
the sample.

Coupons of SAE Type 1020 steel are exposed to
the sample and by measuring the degree to which
the coupon has been eroded, determines the
corroslvity of the sample.

-------
                                                                  TABLE 5.1-1 (Continued)
Analysis/Matrix/Analytes
Detection
Limit*
High Range
Concentration Hold Time
Level of
Certification Reference Methods
Principle of Method
Reactivity (Total
and Amenable
Cyanide; and Sulfides)/SolIds
7 days
                                                                           None
EPA 9010 and
EPA 9030(1)
EPA Method C003(6)
HEAI
Total and Amenable Cyanides:   Two 100 gm samples
are hrought to a 500 ml volume in ASTM type  II
water. Each sample is then distilled to remove
interferences.  During distillation cyanide  is
converted to HCN which is trapped in a scrubber
containing 50 ml 1.25 N NaOH.  10-12 drops of
rhodamine indicator are added to the scrubber
contents.  The solution is titrated with
standard silver nitrate solution to the first
change in color from yellow to brownish pink
against an ASTM type II water blank.
                                                                                                                             Sulfides  Excess iodine is added to a  50 om
                                                                                                                             sample which has been treated with  zinc acetate
                                                                                                                             to produce zinc sulfide and suspended  in 200 ml
                                                                                                                             distilled water.  Two ml of 6 N HC1 is added to
                                                                                                                             the sample.  The iodine oxidizes the sulfide to
                                                                                                                             sulfur under acidic conditions.  Excess iodine
                                                                                                                             is back trltrated with sodium thlosulfate using
                                                                                                                             the starch indicator, until the blue color
                                                                                                                             disappears.

-------
                                                                  TABLE  5.1-1  (Continued)
Analysis/Hatrlx/Analytes
                                   Detection    High Range                   Level of
                                     Limit*    Concentration  Hold Time    Certification
                               Reference Methods
                                              Principle of Method
Proximate Analysis:
    Moisture/Solids
7 days
                                                                           None
EPA Method
AOOla (6)
HEAI
Ash (Loss on Ignition)/Solids
7 days
                                                                           None
Elemental Composition/Solids
7 days
                                                                           None
EPA Method
AOOlb  (6)
HEAI
EPA Method
A003  (6)
A 10 gm soil or 25 gm sludge aliquot is
transferred to a tared porcelain evaporating
dish.  The sample and dish are weighed, then
heated on a hot plate to evaporate the sample to
near dryness without boiling.  The sample and
dish are then transferred to a 103°C oven to
complete evaporation.  Periodically the sample
is removed from the oven, cooled in a desiccator
and weighed.  Dryness is considered complete
when weight loss is<4« of previous weight.

After removing a 50 mg aliquot for elemental
analysis, the weighed solids from the moisture
analysis and porcelain dish are ignited  for 30
minutes at 600°C.  The ash is cooled in  a
desiccator and weighed.

A  50 mg sample of dried solids are analyzed to
determine the percent concentration of the
following elements:  carbon, nitrogen,
phosphorus, sulfur, and halogens (i.e. iodine,
chlorine, fluorine, bromine).
Heating Value of  the Waste/Solids
                                                              7 days
                                                                           None
                               EPA Method
                               A006  (6)
                                 A 1  gm sample  is placed in a bomb calorimgrer
                                 and  ignited.   The amount of heat released by the
                                 burning waste, the activation energy, is
                                 expressed  as Btu/lb.

-------
TABLE 5.1-1 (Continued)
Analysls/Matrlx/Analytes
Volatile Halo Organlcs/Mater
Chlorobenzene
Chloroform
1 , 1-Olchloroethane
1 , 2-Olchloroethane
1,1, 1-Trlchloroethane
1 , 1 ,2-Trichloroethane
Tet rachlo roct hy lene
Trlchloroethylene
1 , 2-trans-Olchloroethy lene
Dichloromethane
Carbon tetrachlorlde
Volatile Arom. Organlcs/Water
Benzene
Toluene
Xylenes
Ethyl benzene
Organochlorlne Pesticides/Water
Aldrln
Endrin
Dieldrln
Isodrln
Chlordane
Hexachlorocyclopentadlene
p.p'-OOT
p.p'-OOE
Detection
Limit*

Ipg/L
1 yg/L
1 wg/L
lpg/L
1 pg/L
1 wg/L
1 ug/L
1 pg/L
1 pg/L
1 pg/L
1 ug/L

lug/L
l ug/L
l wg/L
lpg/L

0.1 ug/L
0.1 pg/L
0.1 pg/L
0.1 pg/L
0.1 ug/L
0.1 pg/L
0.1 pg/L
0.1 pg/L
High Range Level of
Concentration Hold Time Certification Reference Methods
14 days (2) Quantitative EPA 601 (2)
50Mg/La
50pg/La
50pg/La
50 u g/La
50 p g/La
50Mg/La
50ug/La
50pg/La
50ug/La
50yg/La
50 u g/La
7 days (2) Quantitative EPA 602 (2)
50wg/La
50gg/La
50pg/La
50pg/La
7 days for Quantitative EPA 608 (2)
10pg/La the water
10pg/La and 40 days
10gg/La for the
10pg/La extract (2)
10pg/La
10ug/La
10pg/La
10pg/La
Principle of Method
Purge and Trap GC/Hall Detector with a packed
column (1% SP-1000 on Carbopack B) 1,2-dibromo-
ethane or other suitable internal standard will
be used based on Phase I experience to monitor
purge efficiency.







Purge and Trap/GC/PID with a packed column (IX
SP-1000 on Carbopack B, to permit runs in
conjunction with EPA 601). A suitable internal
standard will be used based on Phase I experi-
^
ence to monitor purge efficiency.
An 800 ml portion of water is extracted with 3 x
50 ml methylene chloride. The extract is reduced
in volume and exchanged with iso-octane. The
final volume Is 10 ml or less. The concentrated
extract is analyzed by GC/EC using a fused silica
capillary column. Cleanup procedure will be
f ?)
applied as required. A suitable Internal
standard will be selected based on Phase I
Q
experience to monitor purge efficiency.

-------
                                                               TABLE 5.1-1 (Continued)
Detection
Analysls/Matrlx/Analytes Limit*
Dicyclopentadiene and 0.3 pg/L
Bicycloheptadienc/Water




Organosulfur Compounds/Water
Chlorophenylmethyl sulfide 2 pg/L
Chlorophenylmethyl sulf oxide 2 pg/L
Chlorophenylmethyl sulf one 2pg/L
1,4 oxathlane 2 pg/L
dithiane 2 pg/L


Phosphorates /Water
Oil sopropylmethylphosphonate 2 p g/L

Olmethylmethylphosphonate 2 pg/L





Organophosphorous Pesticides/Water
Malathlon 0.1 pg/L
Parathion 0.1 pg/L
High Range
Concentration
25 ug/L






50 pg/L
50 pg/L
50 pg/L
50 pg/L
50 ug/L



100 pg/L

100 pg/L






5 pg/L
5 pg/L
Level of
Hold Time Certification Reference Methods
Extract Quantitative Developed by MRI
within 7 for USATHAMA
days, Certification
analyze
within 40.
See 4 (1)
Extract Quantitative USATHAMA 4P
within 7
days,
analyze
within 30.
See EPA 625
(1)

7 days Quantitative USATHAMA 4S for
See EPA 625 DIMP
(1)
ESE will develop
method for DMMP




7 days Quantitative EPA 8140(2)
See EPA modified for
625 (1) water
Principle of Method
A 100 ml portion of sample is extracted with 5
ml of methylene chloride. The extract is
analyzed by GC/FID using a fused silica
capillary column. A suitable internal standard
will be specified based on Phase I experience to
monitor purge efficiency.
An 800 ml portion is extracted three times with
50 ml methylene chloride. The volume is reduced
in a K-0 apparatus and exchanged for Isooctane.
The Isooctane extract is analyzed by GC/FPD-S
using a packed column (5X SP-1000 on Chromosorb).
A suitable internal standard will be specified
based on Phase I experience to monitor purge
efficiency.
An 800 ml portion of the sample Is extracted
three time with 500 ml methylene chloride. The
extract is reduced in volume and exchanged with
Isoctane. The final volume is 5 ml. The
extract is analyzed bya GC/NPD using a fused
silica capillary column. Vapona will be added
if indicated by Phase I experience. A suitable
internal standard will be specified based on
Phase 1 experience to monitor purge efficiency.
An 800 ml portion of the samples is extracted
three times with 50 ml methylene chloride. The
extract Is reduced In volume and exchanged with
Azodrin
Supona
Vapona
0.1 ug/L
0.1 pg/L
0.1
5
5 ug/L
5 pg/L
isooctane.  The final volume is  5 ml.  The
extract is analyzed by GC/NPD using a fused
silica capillary column.   A suitable internal
standrd will be specified based  on Phase 1
experience to monitor purge efficiency.

-------
                                                                  TABLE 5.1-1 (Continued)
Analysis/Matrix/Analytes
Detection    High Range                   Level of
  Limit*    Concentration  Hold Time    Certification    Reference Methods
                                                                                                                                           Principle of Method
Metals by AA/Hater
  Arsenic

  Mercury
 lOgg/L      100Mg/L      6 mos  (5)     Quantitative      EPA 206.2  (A)

O.lug/L        lOyg/L    28 days  (5)   Quantitative      EPA 245.1  (4)
                                                  A 100 ml  aliquot of sample is digested with H20,
                                                  and HMO,.  The digest is analysed by GF/AA.b
                                                                                                                            A 100 ml aliquot is treated with H2S04,  HNOj,
                                                                                                                            KMn04, KjSjOg.  Excess KMn04 is destroyed with
                                                                                                                            hydroxylamine sulfate.  The mercury is reduced
                                                                                                                            with stannous sulfate and analyzed by CV/AA.b
Metals by ICP/Kater
Chromium
Cadmium
Lead
Zinc
Copper
Magnesium
Calcium
Sodium

50(i g/L
50 p g/L
50 pg/L
50gg/L
50 \t g/L
10 mg/L
100 mg/L
100 mg/L

5000 Mg/L
5000 g g/L
5000 y g/L
5000 yg/L
5000 v g/L
1000 g g/L
1000 g g/L
1000 y g/L
                                                              6 mos  (5)     Quantitative
                                                         EPA 200.7  (4)
                                                                                                                            All samples will be treated by adding HNO?  + Ha
                                                                                                                            and heating before analysis to dissolve precipi-
                                                                                                                            tates that may have formed after sampling.
                                                                                                                            Magnesium, calcium and sodium may be certified
                                                                                                                            at lower levels if required.
Ignltabllity/Water
                           7 days
None
EPA 1010 (2)
ASTM Method
D93-77 and
EPA Method
C001(6)
A liquid sample is heated at a  slow constant
rate with continual stirring in a cup.  A small
flame is directed into the cup  at regular
Intervals with simultaneous Interruption of
stirring.  The flash point is the lowest
temperature at which application of the flame
ignites the vapor above the sample.
Corroslvity/Water
                           7 days
                                       None
                  EPA 1110 (2)
                  NACE Standard
                  TM-01-69 and
                  EPA Method C002 (6)
                                Coupons of SAE Type 1020 steel are exposed to
                                the sample and by measuring the degree to which
                                the coupon has been eroded, determines the
                                corrosivity of the  sample.

-------
                                                                  TABLE 5.1-1 (Continued)
Analysis/Matrix/Analytes
                                   Detection    High Range
                                     Limit"    Concentration  Hold Time
               Level of
             Certification
                               Reference Methods
                                              Principle of Method
Reactivity (Total and
Amenable Cyanide, and
Sulfide)/Water
7 days
                                                                           None
EPA 9010
EPA 9030 (2):
and EPA Method
C003 (6)
Proximate Analysis:
Moisture/Mater
7 Days
                                                                           None
EPA Method
A001a(6)
Total and Amenable Cyanides:   Two 500 ml samples
preserved with 2 ml IN NaOH are prepared.  One
is chlorinated to destroy succeptable
complexes.  Each sample is then distilled to
remove interferences.  During distillation,
cyanide is converted to HCN which Is trapped  In
a scrubber containing 50 ml 1.25N NaOH.  Ten  to
twelve drops of rhodamlne Indicator are added to
the scrubber contents.  This solution is
titrated with standard silver nitrate solution
to the first change in color from yellow to
brownish pink against an ASTM Type II water
blank.
Sulfides;  Excess iodine is added to a 200 ml
sample which is treated with zinc acetate to
produce zinc sulfide.  Two ml of 6N HC1 is added
to the liquid.  The iodine, oxidizes the sulfide
to sulfur under acidic conditions.  Excess
iodine is back titrated with sodium thiosulfate,
using the starch Indicator, until the blue color
disappears.

A 100 ml  liquid aliquot is transferred to a
tared procelain evaporating dish.  The sample
and dish  are weighed, then heated on a hot plate
to evaporate the sample to near dryness without
boiling .  The sample and dish are then
transferred to a 103°C oven to complete
evaporation.  Periodically the sample Is removed
from the oven, cooled in a desiccator and
weighed.  Dryness is considered complete when
weight loss is < « of previous weight.

-------
                                                                  TABLE 5.1-1 (Continued)
Analysis/Matrlx/Analytes
Detection    High Range                  Level of
  Limit*    Concentration  Hold Time    Certification     Reference  Methods
                                                                                                                                           Principle of Method
Ash (Loss on Ignition)
                           7 days
None
Elemental Composition/Mater
                           7 days
None
Heating Value of the Haste/Water
                           7 days
                                       None
Viscosity/Water
                           7 days
                                       None
                  EPA Method
                  A00lb(6)
                  EPA Method
                  A003C6)
                  EPA Method
                  A006(6)
                  EPA Method
                  A005(
-------
                                                                 TABLE 5.1-1 (Continued)
Analysis/Matrlx/Analytes
Detection    High Range                  Level of
  Limit*    Concentration  Hold Time    Certification
                                                                                            Reference Methods
                                                                                        Principle of Method
Volatile Organics/Off-Gas
                           4 weeks In   None
                           freezer
                                                                          The front and back sections of the Tenax tubes
                                                                          are combined and thermally desorbed.  The
                                                                          desorbed organics are analyzed by GC Hall using
                                                                          a fused silica capillary column.
Acid Gases/Off-Gas
                           28 days     None
                                                                          The O.ln NaOH sorbent from the stack gas
                                                                          impinger is assayed by specific ion probe for
                                                                          chloride.
Volatile Metals/Off-Gas
   Chromium
   Cadmium
   Lead
   Zinc
   Cooper
                                                              6 mos
                                                                          None
                                                                                            EPA 200.7(5)
50 ug
50 ug
50 ug
50 yg
50 ug
500 ug
500 vg
500 yg
500 yg
SOOyg
                                                             An aliquot of silver catalyzed ammonium
                                                             persulfate sorbent is treated with HNOj + HC1
                                                             and heated before analysis to dissolve
                                                             precipitates and analyzed by ICP.
Volatile Metals/Off-Gas
   Arsenic
 1 yg
10 yg
                                                              6 mos
                                        None
                                                         EPA 206.2 (5)
                                                             An aliquot of silver catalyzed ammonium
                                                             persulfate sorbent is treated with H^O, and
                                                             HNO-.  The digest is assayed by GF/AA.
Volatile Metals/Off-Gas
   Mercury
 0.1 ug
lOyg
28 days     None
                                                         EPA 245.1 (5)
An aliquot of silver catalyzed ammonium
persulfate sorbent is treated with H^O^
                                                                                                                            HMO,
                                                                                                                                       and
                                                                                                                                                    Excess
                                                                                                                            KMN04 is destroyed with hydroxylamine
                                                                                                                            sulfate.  The mercury is reduced with  stannous
                                                                                                                            sulfate and analyzed by cold vapor AA.b

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                                                                  TABLE 5.1-1 (Continued)
Analysis/Matrlx/Analytes
Detection      High Range
  Limit*      Concentration
                                 Hold  Time
  Level of
Certification     Reference Methods
                                                                                                                                         Principle of Method
Organophosphorous Compounds/
Off-Gas

Organosulfur Compounds/Off-Gas

Organochlorlne Compounds/Off-Gas
                                              Qualitative        Developed by HEAI


                                              Qualitative        Developed by HEAI

                                              Qualitative        Developed by HEAI
                                         XAD-2 sorbent, incinerator residues,  fly ash,
                                         and water extracted (if necessary).  All
                                         extracts combined to one sample concentrate.
                                         Solvent exchanged as necessary to perform
                                         instrumental analysis.  Analyses by GC with
                                         specific detectors as described under liquid
                                         matrix.
•Actual detection limits for certified methods are Identified  in Volume IV of the RMA Procedures Manual (Project Specific Analytical Methods Manual)  for
 each laboratory.  Detection limits for uncertified methods  and methods to be certified are desired detection limits.

a Reflects an estimate of the linear range of the method and is proposed to minimize dilutions.
b To be developed during USATHAMA Phase II certification.

References:
(1)  EPA SW-846, 2nd ed., "Test Methods for Evaluating Solid Waste".
(2)  EPA-«X)/4-82-057, July 1982 "Methods for Organic  Chemical Analysis of Principal and Industrial Wastewater".
(3)  Personal Communication from Chris Weathington, Ebasco QA  Manager.
(4)  ESE-AMP^-UD-HjO.l, July 22, 1982.
(5)  EPA-600/4-79-020, Revised March 1983, "Methods for Chemical Analysis of Water and Wastes".
(6)  EPA-600/8-M-OO2, February 1984, Sampling and Analysis  Methods for Hazardous Waste Combustion.

Notes:
     (A)  Semi-Quantitative:  See Section III of the Litigation Technical Support and Services Rocky Mountain Arsenal Procedures Manual,  Seciton  11.2.2.1.
     (B)  Quantitative:  See Section III of the Litigation Technical Support and Services Rocky Mountain Arsenal Procedures Manual,  Section 11.2.2.1.

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Table 5.1-2
Number of Analyses
	 Feedstock 	

Test Phase
Initial Screen of
Waste Feedstock

POHC Evaluation Tests





Optimization Tests

Test of Optimum
Conditions
•





Analysis
VOA-GC/MS1
Semi vol. -GC/MS2
Metals3
VOA-GC/MS
Semi vol. -GC/MS
GC/ECD4
GC/FPD5
GC/NPD6
GC/PIO7
GC/ECD
GC/78
VOA-GC/MS
Semi vol. -GC/MS
GC/ECD
GC/FPD
GC/NPD
GC/PID
Metals

Solid
1
1
1
4
4

—
—
-
12
12
1
1
_
_
-
-
1

Liquid^
1
1
1
—
_
_
—
—
-
<•»
-
1
1
_
_
-
-
1

Sludge
1
1
1
—
—
—
_
_
-
_
-
1
1
_
_
_
_
1
Residual
Ash

—
-
—
_
4
4
4
4
12
12
—
_
3
3
3
3
3
Off-
Gas

—
-
_
_
4
4
4
4
12
12
^
_
3
3
3
3
3
1.  VOA-GC/MS:  Volatile Organic Analyses by Gas  Chromatography/Mass Spectrometer.
2.  Semivol. - GC/MS:  Semivolatile Organic Analyses by Gas Chromatography/Mass
    Spectrometer
3.  Metals:  Selected metals by inductively coupled plasma and atomic absorption.
4.  GC/ECD:  Chlorinated Hydrocarbons by Gas Chromatography with Electron Capture
    Detector.
5.  GC/FPD:  Organosulfur Compounds by Gas Chromatography, with Flame Photometric
    Detector.
6.  GC/NPD:  OrganoPhosphorous Compounds by Gas Chromatography with Nitrogen Phosphorous
    Detector.
7.  GC/PID:  Volatile Organic Analysis by Gas Chromatography with Photolonlzation
    Detector.
8.  Detector depends on  selected POHCs.

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5.2  ANALYTICAL PROTOCOL SUMMARY

The  following is a  summary of  the  analytical procedures which  will  be
followed  to  support  the Task  17 objectives.   All soil, sludge,  sediment,
incineration  residue,  and  solid matrices were  considered as  soils  for
analytical  purposes.   Analytical  methods,  target analytes,  and desired
target  detection  limits for liquid matrix analytes  are discussed in this
section as well.

The  off-gas  analytical  procedures have not been  developed in  detail  but a
summary of the analytical approaches  and  procedures  that may be expected to
meet the requirement of Task 17 are listed.

     5.2.1  Volatile  Organics  in  Soil  and   Solid  Samples   by  Gas
            Chromatography/Mass Spectrometry (GC/MS)

     The  volatile organics  method for solids was based on EPA Method 8240
     (EPA SW-846).  This method was PMO certified for  soils  and solids at
     the  semiquantitative level  for the Task  17  Program (USATHAMA Method N9
     for UBTL and K9 for CAL).

     In this  method, a  10-gram portion of the sample will be  obtained  with
     minimum  of handling and placed into 10 ml  of  methanol  in a volatile
     organic  acid (VOA) septum vial,  spiked  with the surrogates:  methylene
     chloride-d2; 1,2  Dichloroethane-d.;  and ethyl  benzene-d.Q> capped
     with a teflon lined lid,  and shaken  for four hours.   A 20-ug aliquot of
     the  methanol extract  will  be  removed,  spiked with 200  ug of
     1,2-dibromoethane-d.  as  an internal standard,  and injected  into  5 ml
     of organics-free water and  contained  in a syringe.  The contents of the
     syringe  will then  be  injected into  a  purging device,  purged,  and
     analyzed on a packed column (1%  SP-1000 on  Carbopack B) by GC/MS.   Each
     sample  will  be assayed  for  target  compounds  at  detection  limits
     identified in Table 5.1-1.
                                      5-2
2140E

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 In addition, the total  ion  current profile will be screened  for  all
 major unknown peaks.  An attempt will be made  to  identify  the largest
 of these major unknown peaks which are present  in  excess of ten percent
 of the area of the internal standard peak.   Each of these major unknown
 peaks will be reported as the purity, fit and  probability  to  match the
 three most likely candidate  compounds from  the  Environmental Protection
 Agency/National  Bureau  of  Standards/National  Institute of  Health
 (EPA/NBS/NIH) Mass Spectral  library computer program.

 5.2.2  Semivolatile  Organics  in  Soil  and  Solid  Samples  bv  Gas
        Chromotography/Mass Spectrometry (GC/MS)

 This  analytical  technique was based on EPA  Method 8270 for  solids (EPA
 SW-8A6)  and  was  PMO certified  for  soils and solids  at  the
 semiquantitative  level for the Task 17 program (USATHAMA Method L9 for
 UBTL,  X9 for CAL, and  X9-A for HEAI).

 Using  this method,  a  15-gram portion  of  the sample will be obtained
 with   a  minimum  of   handling and  spiked  with the surrogates:
 2-chlorophenol-d^,   1,3-dichloro-benzene-d^,  diethyl   phthalate-d ,
 and  di-n-octyl  phtalate-d^.   The sample will be mixed with anhydrous
 sodium sulfate  (30 grams or  more  depending  on sample moisture  content)
 then  the  soxhelet  extracted  for  8  hours  with 300 ml  methylene
 chloride.   The  extract  is reduced  to a final  volume  of 10 ml in a
 Kuderna-Danish (K-D)  apparatus.   An aliquot of  this concentrate will be
 spiked with phenanthrenerd._ as an internal standard  and analysed on
 a  fused  silica capillary column by GC/MS.   Samples will be  assayed for
 target analytes  at  the  detection  limits shown in Table 5.1-1.   In
 addition,  the  total  ion current  profile will  be  scanned  for major
 unknown peaks.  As discussed for  volatile organics, an attempt will be
made to identify these unknown major peaks.

5.2.3  Metals in  Soil and Solid Samples by Inductively Coupled Argon
       Plasma (ICP) Emission  Soectrometrv

The ICP method,  based on USATHAMA  Method 7S,  is PMO certified at the
quantitative level (USATHAMA Method P9 for UBTL and A9 for  CAL).
                                 5-3

-------
     In this procedure, a one-gram portion of  sample  will  be  digested  in a
     watch glass covered  Griffin  beaker with 3 ml  of concentrated nitric
     acid.  Contents  of the beaker  will be heated to near dryness and
     repeated portions of concentrated  nitric  acid  will be added until the
     sample is completely digested.  The digestion  process  is  finished  with
     two ml  of  1:1 nitric acid and  2 ml of 1:1  hydrochloric  acid.  The
     sample digest will be filtered, the beaker and watch  glass  rinsed  with
     deionized water,  and the  rinsate passed through the filter.  The
     digestate is brought to a final volume  of  50  ml and assayed  by ICP.

     The  sample  will be  assayed  for target metals at  detection  limits
     identified in Table 5.1-1.

     5.2.A  Arsenic in Soil  and Solid Samples  by Graphite  Furnace Atomic
            Absorption (AA)  Spectroscopy

     The arsenic method  for  soils  and solids was  developed from EPA Method
     7060  (EPA-SE-846).   Using this  method, a one-gram sample will  be
     digested with  hydrogen peroxide  and  concentrated  nitric acid.   The
     digest  will be  filtered and  assayed  by  graphite furnace  atomic
     absorption  spectroscopy.  The target  detection limit for arsenic  will
     be 1  ug/g.   This method is  PMO certified at  the quantitative level
     (USATHAMA Method B9 for UBTL and G9 for CAL).

     5.2.5  Mercury  in  Soil  and  Solid  Samples  by Cold  Vapor  Atomic
            Absorption (CVAA) Spectroscopy

     This  mercury  method,   developed  from EPA  Method  245.5  (EPA
     600/4-82-057), is  PMO  certified at the quantitative level (USATHAMA
     Method Y9 for  UBTL  and  J9  for CAL).  In the method, a one-gram sample
     portion will  be  digested with  aqua regia followed by treatment with
     potassium permanganate.   Excess  permanganate  will  be reduced with
     hydroxylamine  sulfate.  Mercury  will  be reduced with stannous chloride
     and assayed by CVAA.   The target detection  limit for mercury will  be
     0.1 ug/g.
                                      5-4
2140E

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     5.2.6  Extraction  Procedure  (EP)  Toxicity  Protocol   for  Soils.
            Incineration Residues, and Solids

            This  extraction  procedure  is  based upon  EPA   Method  1310
            (EPA-SW-846)  and EPA Method  C004  (EPA-600/8-84-002).   The
            procedure  will  not  be  PMO  certified.   In the extraction
            procedure, a  100-gram portion  of the sample is  extracted for a
            period  of 24 hours  with 1.6  1  of deionized water  which is
            maintained at pH  5.0  +0.2 using 0.5 N acetic acid and monitored
            throughout the  course of the extraction.  The sample slurry is
            allowed to  stand to permit the solid  phase to  settle and  the
            liquid  portion  to be  decanted for  filtration.   The filtered
            liquid  is the extract.   This liquid will be assayed using PMO
            certified methods for arsenic,  cadmium,  chromium, endrin, lead,
            and mercury,  and  approved methods  for  selenium,  silver,  barium,
            lindane,  methoxychlor,  toxaphene,  2,4-dichlorophenoxy acetic
            acid, and 2,4,5-trichlorophenoxy propionic acid.

     5.2.7  Ignitability in Soil and Solid Samples

     This method  is based  on EPA Method 1010  (SW-846).   Ignitability is
     determined by  heating  a  sample  at a slow, constant rate with continual
     stirring  in  a Pensky-Martin closed-cup  tester.   A small  flame is
     directed  into  the  cup  at  regular intervals  with a  simultaneous
     interruption at  which the  test flame ignites  the vapor  above  the
     sample.  This method will not be PMO certified.

     5.2.8  Corrosivity Toward Steel in Soil and Solid Samples

     The corrosivity  method is  based on EPA Method  1110 (SW-846).  In the
     method, coupons  of SAE Type  1020 steel are exposed to  the  waste  to be
     evaluated and, by  measuring the degree to which the  coupon has  been
     dissolved, the corrosivity  of the  waste  is determined.  This method
     will not be PMO certified.
                                      5-5
21AOE

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     5.2.9  Reactivity in Soils and Solid Samples

     Reactivity for soils and  solids  in this task is defined  in  terms of
     cyanide or sulfate concentrations.   The assay employs  EPA  Method 9010
     (EPA-SW-846) for  total and  amenable cyanide  and  EPA method  9030
     (EPA-SW-846) for  sulfide.   For cyanide, a sample will be split  into
     two, 100-gram aliquots, each brought to a 500 ml volume with ASTM Type
     II water in  a  1-liter  boiling flask.   One  aliquot  is  chlorinated with
     calcium hypochlorite to destroy susceptable complexes.  Each aliquot is
     distilled to remove  interferences  and  25 ml of concentrated sulfuric
     acid is slowly added to  each flask.  During distillation, cyanide  is
     converted to HCN  which is  then trapped in  a  scrubber  containing  50 ml
     1.25 N NaOH.  Ten  to twelve  drops  of rhodamine indicator  are added to
     the scrubber contents.   This  solution  is titrated with standard  silver
     nitrate solution  to the  first change in color from yellow to brownish
     pink against an ASTM Type II water  blank.

     Sulfides are determined  by adding  excess iodine to a 50-gram sample
     suspended in 200  ml  distilled water which has been treated  with  zinc
     acetate to  produce zinc  sulfide.   Two  ml of 6N  hydrochloric acid is
     added to the sample.   The iodine  oxidizes  the sulfide to  elemental
     sulfur under acidic  conditions.  Excess iodine is back titrated  with
     sodium  thiosulfate using  starch  indicator  until the  blue  color
     disappears.   These methods will not be  PMO certified.

     5.2.10  Proximate Analysis of Soils and Solid Samples

     The proximate analysis provides  data relating to the  physical form of
     the  sample  and  provides  an  approximate mass  balance  as  to  its
     composition.  This analysis  is  based  upon EPA  Method   AOOla  for
     particulate and moisture, EPA  Method AOOlb for ash  (loss  on ignition),
     EPA Method A003 for elemental  composition, and EPA Method A006 for the
     heating value  of the  sample  (EPA-600/8-84-002).   Proximate analyses
     procedures will not be  PMO certified.

     In the particulate  and moisture  method (EPA AOOla),  10  grams  of soil
     and 25 grams of sludge  are placed in a  tared porcelain evaporation

                                     5-6
2140E

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2140E
     dish.  The sample and  the  dish  are  weighed,  then heated on a hot plate
     to  evaporate  the sample to the  near  dryness without scorching.  The
     sample and  dish are then  transferred to  a  103°C oven  to complete
     evaporation.  Periodically, the  sample and dish are removed  from the
     oven,  cooled  in a  desiccator and  weighed.   Dryness is considered
     complete when weight loss is less than 4% of the previous weight.

     Ash  (loss on  ignition)  content (EPA AOOlb) is determined on the  weighed
     solids from the moisture analysis.  After  removing a 50-mg aliquot for
     elemental analysis, the solids  and  procelain dish are  ignited  for 30
     minutes at 600°C.  The  resultant ash and porcelain dish  are cooled  in a
     desiccator and weighed.

     The  elemental composition method (EPA  A003)  uses 50  mg  of dried solids
     to  determine  the  percent  concentrations  of  carbon,   nitrogen,
     phosphorous,  sulfur,  and halogens  (iodine,  chlorine,   fluorine, and
     bromine).  Carbon is determined  by  measuring carbon dioxide and water
     upon  combustion (ASTMD-3178-73).   Nitrogen  is determined  by   the
     Kjeldahl  digestion  method  (ASTM D-3179-73),   and  oxygen  by the
     difference method  (ASTMD-3176-74).   Phosphorous is  determined  by the
     spectroscopic  method  (ASTMD-2795),   sulfur  by sulfate  titration
     (ASTMD-3177),  and halides by halide  titration (ASTMD-2361-66).

     Heating value of the sample will be  determined using  the ASTMD-2015
     method.  In the method, a one-gram sample is  placed in a calibrated
     isothermal  jacket  bomb calorimeter  under  controlled   conditions.
     Calorific values (Btu)  will be  computed from temperature  observations
     made before,  during,  and after combustion of the sample.

     5.2.11  Unknown  Identification in Soil.  Solid,  and Sludge Samples  by
             Gas Chromatography/Mass Spectrometry (GC/MS)

     The total ion current  profile will  be screened for  all major unknown
     peaks.  The laboratories will report  (RT Code,  estimated concentrations
     and print MS traces) all unknowns with peaks  greater than  10  percent  of
     the  internal  standard   response.  Each of these major  unknown   peaks
     greater than  10 percent of the  internal  standard response (excluding
     obviously meaningless peaks,  e.g.,  column bleeds) will be reported  as
                                      5-7

-------
     the  purity,  fit,  and probability  to  match the  three  most likely
     candidate  compounds  from the Environmental Protection Agency/National
     Bureau  of Standards/National Institute  of  Health (EPA/NBS/NIH) Mass
     Spectral library computer program.

     5.2.12  Volatile Halogenated Organics in Liquid Samples

     The analytical method for volatile halogenated organics in water will
     be  based  on EPA Method  601 (EPA  60074-82-057).   This analytical
     procedure will be  a  purge and trap method,  assayed on a packed column
     (1% SP-1000  on  Carbopack B) by GC  equipped with a Hall electrolytic
     conductivity  detector.   Water   samples  will   be  spiked  with
     1,2-dibromethane,  or another  suitable  internal standard  based  on
     project experience, to monitor purge efficiency.

     Volatile halogenated  organic analyses  and desired detection limits are
     identified in Table 5.1-1.

     5.2.13  Volatile Aromatic Organics in Liquid Samples

     The volatile aromatic hydrocarbon methods will be based on EPA Method
     602 (EPA 660/4-82-057)  for  water  and EPA Method 8020 (EPA-SW-846)  for
     soil and  solids.   Analysis  of volatile  aromatics  in  water will be a
     purge and trap method, analyzed by  GC   equipped with  a photoionization
     detector using a packed column (1% SP-1000 on Carbopack B).

     Table 5.1-1 lists the volatile aromatic  organic  constituents and target
     detection limits.

     5.2.14  Organochlorine Pesticides  in Liquid Samples

     The analytical methodology  for organochlorine  pesticides will be based
     on  EPA  Method  608  (EPA  600/4-82-057)  and EPA Method  8080  (EPA
     600/4-82-057) for water  and EPA Method 8080 (EPA-SW-846) for  soil  and
     solid samples.   An  800-ml portion  of  water will be  extracted three
     times with 50 ml of methylene chloride.  The extract shall be reduced
                                      5-8
2140E

-------
in  volume  and exchanged with  hexane to a  final  volume  of 10 ml or
less.  The concentrated extract  will be  analyzed  by GC with an electron
capture detector using a fused silica capillary column.

Organochlorine pesticides  and  their target detection limts are listed
in Table 5.1-1.

5.2.15  Organosulfur Compounds in Liquid Samples

The  organosulfur  compounds that  will be target analytes are  listed in
Table 5.1-1.  Methodologies  for  organosulfur  analyses will be developed
from USATHAMA Method 4P for  water.   In a water matrix, an 800-ml  sample
will be extracted three  times with  50 ml  of  methylene chloride.   The
extract volume shall  be  reduced  in a K-D apparatus and exchanged with
isooctane.  The isooctane  extract will be  assayed on  a  packed column
(5%  SP-1000  on Chromosorb)  by GC with  a flame photometric detector.
The target detection limit for organosulfur compounds  in water will be
2 ug/1.

5.2.16  Organophosphorous Pesticides in Liquid Samples

Organophosphorous compounds  targeted for analysis are listed in  Table
5.1-1.  Analytical  methods for  these compounds  are derived  from EPA
Method 8140 (EPA-SW-846) for water.

In  a water matrix,  the five  Organophosphorous  compounds  will  be
extracted from an  800-ml  sample  with three 50-ml volumes of  methylene
chloride.   The extract  will  be concentrated  and exchanged with
isooctane to a final volume  of 5 ml.  An aliquot  of the  extract will be
assayed on a packed column 6 feet by 2mm ID 1.5% OV17 + 1.95% QF-1 by
GC equipped  with  a nitrogen/phosphorous detector.  Target detection
limits for the five Organophosphorous pesticides in water will be 0.1
ug/1.
                                 5-9

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     5.2.17  Phosphonates in Liquid Samples

     The  phosphonates   Include  diisopropylmethylphosphonate  (DIMP)  and
     dimethylmethylphosphonate (DMMP).   Specific analytical  methodologies
     for phosphonates will be developed from USATHAMA Method 4S for water.

     The sample will be analyzed  on a fused silica  capillary  column  by GC
     equipped with a  nitrogen/phosphorous detector.   The  target  detection
     limit for phosphonates in water will be 2  ug/1.

     5.2.18  Metals in Liquid Samples

     Ten metals  will be  assayed   in  liquid matrices.   The metals  and
     principal analytical method will be as follows:  arsenic and mercury by
     atomic  absorption;  and  cadmium,  calcium,  chromium,   copper,  lead,
     magnesium,  sodium,  and zinc by ICP.

     The method for arsenic  analysis will be derived from EPA Method 206.2
     (EPA  600/4-79-020)  for  water.   Using  EPA  Method  206.2  (EPA
     600/4-79-020), a 100-ml sample of water will be digested with hydrogen
     peroxide and  concentrated nitric  acid.  The digest will be assayed by
     graphite furnace  atomic absorption  spectroscopy.   Target  detection
     limits for arsenic in water will be 10 ug/1.

     The mercury  methods  will  be  derived from EPA Method  245.1 (EPA
     600/4-79-020) for water.  In  the water method,  a 100-ml sample will be
     treated with  sulfuric acid,  nitric acid,  potassium permanganate,  and
     potassium pursulfate.   Excess  permanganate will  be  destroyed  with
     hydroxylamine sulfate.  Mercury  will  be reduced with  stannous sulfate
     and assayed by cold  vapor atomic absorption spectroscopy.  The  target
     detection limit  for mercury in water will be 0.1 ug/1.

     The method for  ICP metals in water was derived from EPA Method 200.7
     (EPA 600/4-79-020).   Target  analytes  and  desired  detection limits for
     ICP metals in the liquid matrix is shown in Table 5.1-1.
                                     5-10
2140E

-------
     All Mater samples for ICP metals will be digested by adding nitric and
     hydrochloric acid  and  heating before  analyses  to dissolve  any
     precipitates that may have  formed  after sampling.  The sample digest
     will be filtered, brought to  a final volume of 50 ml, and assayed by
     inductively coupled  argon plasma emission spectrometry.

     5.2.19  lonitabilitv in  Liquid Samples

     This method is  based on EPA  Method  1010  (SW-846).   Ignitability is
     determined by heating a sample at a  slow, constant  rate with  continual
     stirring  in  a  Pensky-Martin  closed-cup tester.  A  small flame  is
     directed  into  the  cup  at  regular  intervals  with  a  simultaneous
     interruption of  stirring.   The flash point is  defined as the lowest
     temperature at  which the test flame ignites  the vapor  above the
     sample.  This method will not  be PMO  certified.

     5.2.20  Corrosivity  Toward Steel in Liquid  Samples

     The corrosivity method  is based on EPA Method  1110  (SW-846).   In the
     method, coupons of SAE  Type 1020 steel  are  exposed  to  the waste to be
     evaluated and,  by measuring the degree to  which  the  coupon has been
     dissolved, the corrosivity  of the waste is determined.   This method
     will not be PMO certified.

     5.2.21  Reactivity in Soils  and Solid Samples

     Reactivity in soils  and solids for this task  is  defined  in terms of
     cyanide or sulfide  concentrations.   The assay employs EPA Method 9010
     (EPA-SW-846) for  total  and  amenable cyanide  and EPA  Method 9030
     (EPA-SW-846) for sulfide.   For cyanide, a  sample will be split  into
     two, 500-ml  aliquots in  a  1-liter  boiling flask.   One  aliquot  is
     chlorinated  with  calcium  hypochlorite  to  destroy  susceptable
     complexes.  Each aliquot is distilled to remove interferences  and 25 ml
     of concentrated sulfuric  acid is  slowly added  to each flank.  During
     distillation,  cyanide  is converted  to HCN which is  trapped in a
     scrubber containing  50 ml 1.25 N NaOH.   Ten to twelve drops of
                                     5-11
2140E

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     rhodamine indicator are added to the scrubber contents.  This solutions
     is titrated with  standard  silver  nitrate  solution to the first change
     in color from yellow  to brownish  pink against an  ASTM Type  II water
     flask.

     Sulfides are determined by adding excess  iodine  to a  200-ml  sample
     which has been treated  with zinc acetate  to  produce zinc sulfide.   Two
     ml of 6N hydrochloric acid is added to the sample.  The iodine oxidizes
     the sulfide to elemental sulfur under acidic conditions.  Excess iodine
     is back titrated  with  sodium  thiosulfate  using starch indicator until
     the blue color disappears.   These  methods  will not be PMO certified.

     5.2.22  Proximate Analysis  of Liquid Samples

     The proximate analysis  provides data relating to the physical form  of
     the  sample  and  provides an  approximate  mass  balance as  to its
     composition.  This analysis  is  based  upon EPA  Method  AOOla  for
     moisture, EPA Method AOOlb for ash  (loss  on  ignition), EPA Method A003
     for elemental composition,  and EPA Method A006 for  the  heating value of
     the sample  (EPA-600/8-84-002).  Proximate analyses procedures will not
     be PMO certified.

     In the moisture method  (EPA AOOla), a 100-ml liquid sample is placed in
     a tared  porcelain evaporation dish.   The sample  and the dish  are
     weighed, then heated  on a  hot plate to evaporate the sample to near
     dryness without scorching.   The sample and dish are then  transferred to
     a 103°C  oven  to complete evaporation.  Periodically, the sample and
     dish are removed  from the  oven,  cooled in  a desiccator, and weighed.
     Dryness is considered complete when weight  loss  is less than 4% of the
     previous weight.

     Ash (loss on ignition)  content (EPA AOOlb) is determined on  the weighed
     solids from the moisture analysis.  After removing a 50-mg aliquot  for
     elemental analyses, the solids  and procelain dish  are ignited for  30
     minutes at 600°C.  The  resultant ash and  procelain dish are  cooled  in  a
     desiccator and weighed.
                                     5-12
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 The elemental composition method (EPA A003) uses 50 mg of dried solids
 to  determine the  percent  concentrations  of  carbon,  nitrogen,
 phosporous,  sulfur,  and  halogens  (iodine,  chlorine,  fluorine,  and
 bromine).   Carbon is determined by measuring  carbon dioxide  and  water
 upon combustion  (ASTMD-3178-73).   Nitrogen  is  determined  by the
 Kjeldahl  digestion method (ASTM D-3179-73),  oxygen by the difference
 method  (ASTMD-2795), sulfur  by sulfate  titration  (ASTMD-3177),  and
 halides by  halide titration (ASTMD-2361-66).

 Heating  value of the sample  will  be determined  using the ASTMD-2015
 method.   In the  method,  a one-gram sample is placed in a calibrated
 isothermal  jacket  bomb  calorimeter  under  controlled  conditions.
 Calorific values  (Btu)  will be computed  from  temperature  observations
 made before,  during,  and  after  combustion  of the  sample.

 Viscosity of liquid  samples  will  be determined  using  the ASTMD-445
 method  utilizing  a kinematic viscometer  and  a thermometer.   The time
 will be measured  for the  flow of a fixed  volume  of liquid through the
 viscometer.

 5.2.23  Volatile  Organics in  Incineration Off-Gas  Samples  bv  Gas
        Choromatography Mass/Spectrometry  (GC/MS)

 Due  to  their volatility, analysis for  these  compounds  will be
 restricted  to incineration  off-gas samples collected on Tenax/Charcoal
 tubes.   In   this  method,  the  front  and  back  portions  of  the
 Tenax/Charcoal tubes  are  thermally desorbed.  These desorbed  organics
 are  analyzed  by a GC Hall detector using  a packed column (1%  SP-1000 on
 Carbopack B).  This  procedure  will  analyze  for the  volatile halo
 organics.  This method will not be certified by PMO, but demonstration
 will be required  to show the detection level that can be achieved.

Other test burns  may  be used  to collect the volatile aromatic organics
 for  analysis,  since the  tenax  traps  will permit only one analytical
run.  The volatile  aromatics  will  be analysed by GC/PID upon  the same
packed column as  described above.
                                5-13

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     GC/MS  will not  be  used  because  it  does  not  have the  required
     sensitivity to achieve the Task 17 action levels.

     5.2.24  Acid Gases in Incineration Off-Gas Samples

     This method was developed.by UBTL  for the analysis of hydrogen chloride
     (EPA-600/8-84-001) in incineration off-gases.   The method will not be
     PMO certified.

     In the  method,  0.2 N sodium  hydroxide  sorbent  from an incineration
     off-gas impinger  is  assayed  by specific ion probe for the presence of
     chloride.

     5.2.25  Volatile  Metals  bv  Inductively  Coupled Argon Plasma  (ICP)
             Emission Spectrometry in Incineration Off-Gas Samples

     This ICP method,  based  on EPA method 200.7 (EPA-600M-79-020), is  not
     PMO certified  at  the quantitative level.   The  ICP  method has been
     certified only for soils and waters, not volatile metals.

     In this procedure, an  aliquot  of  silver catalyzed ammonium persulfate
     sorbent is placed in a  beaker, treated  with  concentrated nitric  acid
     and 1:1 hydrochloric acid, and heated to dissolve precipitates that may
     have formed.  The acidified aliquot will be filtered, the beaker  rinsed
     with deionized water, and the  rinsate passed through the  filter.   The
     digestate is brought to a final volume of 5 ml and assayed by ICP.

     5.2.26  Volatile  Metals/Arsenic  in Incineration Off-Gas  Samples bv
             Graphite Furnace Atomic Absorption (AA) Spectrometry

     The arsenic method  for  soils and  solids will  be  developed  from EPA
     Method 7060  (EPA-SW-846).  Using  this  method,  an aliquot of silver
     catalyzed ammonium persulfate  sorbent will be  digested with hydrogen
     peroxide and concentrated nitric acid.  The digest will be filtered and
     assayed by graphite furnace atomic absorption Spectrometry.   The  target
     detection limit for arsenic will be 1 ug/g.
                                     5-14
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      5.2.27  Volatile Metals/Mercury  in  Incineration Off-Gas Samples bv Cold
              Vapor Atomic Absorption  (CVAA)  Spectrometrv

      This mercury  method  was developed  from  EPA Method  245.5  (EPA
      600/4-82-057).   In the method, an aliquot of  silver catalyzed ammonium
      persulfate  sorbent  will  be  digested  with aqua  regia followed  by
      treatment  with  potassium  permanganate.  Excess permanganate  will be
      reduced  with  hydroxylamine  sulfate.    Mercury  will  be reduced  with
      stannous chloride and assayed by CVAA.   The target detection  limit  for
      mercury  will  be  0.1  ug/g.

      5.2.28   Moisture Content  in  Incineration Off-Gas Samples

      The  moisture  content determinations will not  be PMO  certified.  In this
      method,  the weight of the  condensate collected in the trap is  measured.

      5.2.29   Organophosphorous.  Orgonosulfur.  and Organochlorine Compounds
              in Incineration Off-Gas Samples by GC/Selective Detectors

      After  incineration  the bottom residue  and  fly ash,  the XAD-2 sorbent
      are  sohxlet extracted with methylene  chloride and  the  condensate  in  the
      liquid trap  is extracted  with methylene chloride.  The extracts are
      concentrated  by  Kuderna  Danish.   The  concentrates  are then  solvent
      exchanged to  isooctane.   The  final volume  will vary from 0.25 ml to
      0.50 ml  to meet  the  sensitivity  and action levels required of Task  17.
      This method will not be PMO certified.   Demonstration will be required
      to show the detection  level that can be achieved.

      The  concentrate  is  analyzed for organochlorine, Organophosphorous and
      organosulfur  compounds.   The instrumental conditions  are  the  same  as
      those described  under the  respective  sections in Table 5.1-1 for  liquid
      samples.
                                     5-15
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         5.3  ANALYTICAL RESULTS
X,
              5.3.1  System Performance Parameters

              A run log will be maintained  for  the  bench-scale test unit.   This log
              will note  the purpose  of  a  particular  test  run,  the  set  test
              conditions,  and any  abnormalities encountered during  the  test.   The
              operating parameters such  as  temperatures,  pressures, and flow  rates
              will be  recorded  on a  data sheet.   Measurements  will be made  at
              appropriate intervals to insure a continuous  picture of the operating
              conditions.

              5.3.2  Analytical  Results

              The concentrations of the  constituents measured in the off-gases and
              solid residues will  be  analyzed  for  the  original  sample  volume  (for
              liquids) or  weight   (for  soils).    For  sludge,  the  data  would  be
              presented based on a dry weight  basis.
v,
         5.4  CERTIFICATION

         The initial feedstock analyses  will  be performed by PMO  certified methods
         and laboratories for those methods which are currently certified.  To  reduce
         the intralaboratory analytical variations  and  provide the  rapid  turn  around
         of analyses, HEAI will perform  all of the  analyses of  the individual feed
         wastes and incineration  products except for the physical characterization
         analyses.  No new methods will  be  certified for this task. However, some
         methods demonstration will be required.   Hittman/Ebasco  will  use methods
         approved by PMO but will not  perform additional  certification  analyses.  If
         required to  determine the   validity   of analytical  data, qualitative
         certification would be  recommended.

         5.5  QA/QC

         For Task 17, the sample handling and analytical  activities will comply with
         the established QA requirements  stated  in the RMA Procedures Manual except
                                              5-16
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as noted  in this  test  plan.  The  bench-scale test conditions  such as
temperature, gas flow rates, pressures, and oxygen levels will be measured
using industry-acceptable  methods and  equipment.   These methods  will  be
based on the equipment manufacturers calibration and established procedures.

The analytical  procedures for feedstock  and solid residues  will use QC
procedures  outlined  in the  RMA  Procedures  Manual (Ebasco,  1985).   All
chemical analyses will include:

     o   Calibration standard;
     o   Blank; and
     o   Matrix spike.

During development of procedures  for  off-gas and residue chemical analysis,
it will be  necessary to  document the steps used  to achieve  the required
detection limits.  The documented procedure will include:

     o   Summary of method;
     o   Instrumentation and operating conditions;
     o   Reagents and materials;
     o   Analytes and analytes standard concentration;
     o   Details of sample preparation;
     o   Calculation; and
     o   QC.

For all analyses where the  detection  or action  level is  critical,  there  will
be one standard  run  at  two times the required detection  limit.   The matrix
spike also will  be at two times  the detection level or two times  the found
analyte concentration.
                                     5-17
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                             6.0  EXPECTED RESULTS
6.1  INTRODUCTION

The test  program  outlined in the preceding sections is designed to develop
data  at  the  bench-scale  that  will  ensure  success  of  a full-scale
incineration program.  It will provide  a  basis  for selecting  an appropriate
incineration regime and will  therefore  contribute  to the confirmation of the
selection of the most  desirable  technology  for waste destruction to a ORE of
99.99 percent.  Details of these expected results are outlined below.

6.2  EXPECTED DRE RESULTS

The tests identified above  will  provide detailed information  concerning the
ability to remove hazardous organic chemicals from the soils by heating them
to temperatures in  the 800-1,000°C region.  They will determine the extent
to which  such chemicals as  aldrin,  endrin, dieldrin, isodrin,  and other
contaminants can be  removed from the soils matrix and  put into the vapor
state in order to ensure their destruction in an afterburner.

The tests identified  above will  provide  sufficient  analytical data  to
determine the DRE for  all organics found  in the  soils as a function of time,
temperature, and oxygen concentration.  Specific plots will be as follows:

       o  DRE as a function of temperature with a residence time of 2 seconds;

       o  DRE as a function of temperature with a residence time of 5 seconds;

       o  DRE  as  a  function  of  time  with  a  temperature of  1,250°C
          (afterburner);

       o  DRE as a function of time with  a  temperature of  900°C  (afterburner);
          and
                                       6-1

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v
                o  ORE of certain  selected POHCs  (e.g.,  aldrin as a function  of
                   oxygen concentration  for constant  time  and temperature values.

         From these data a rough optimal (most cost effective)  regime for destruction
         of hazardous  organics can  be  developed.   This  regime will incorporate
         thermodynamic data  concerning  the  soils (e.g.,   heat  capacity, thermal
         conductivity, specific heat) plus regime results  into  conceptual evaluations
         of fuel  consumption (temperature) and  equipment volume  (residence  time)
         requirements.

         ORE values will  also  be determined  for liquid,  sludge, and a mixture  of
         wastes at  a  successful regime associated with soils  incineration  (e.g.,
         1,250°C,  2 seconds, 5.4% 02).  Such  ORE values will confirm the utility of
         a selected regime for  the entire  waste feedstock  associated with Basin  F.

         6.3  EXPECTED TECHNOLOGY SELECTION CONFIRMATION RESULTS

         The data  above  will provide a method for conceptual  optimization  of  the
         incineration  regime to  be  scaled  up from  the bench-scale operations  to
         either pilot  plant or full-scale operation.  These data can then be compared
         to typical  regimes for existing  incinerator designs from among  the
         technologies  of countercurrent and cocurrent rotating  kilns, fluidized beds,
         and multiple  and single hearth  furnaces.

         In addition to  the  ORE  data described  above,  the PCT  data concerning the
         soils, sludge,  and  liquid also will be factored  into the evaluation of
         technologies.  Specific  issues will include ash  fusion temperature of the
         soils.  Such  data will be used to  determine whether a  given technology does
         or does not have a "fatal flaw" with respect to the wastes found at Basin F.
         Such data could be  used  to  rule  out a given technology if it cannot provide
         sufficient temperature or residence time to ensure 99.99 percent ORE.
                                               6-2

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                                  APPENDIX 1





                                  REFERENCES
2140E

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          6.4  OTHER EXPECTED RESULTS
v
          The tests  described  in preceding  sections  will contribute by determining
          initial  regimes  to  be  tested either  at the pilot-scale  or full-scale
          operation.   Further,  they  will  be useful  in  determining conceptual
          parameters of a full-scale operation including the following:

          Technology               Parameter

          Rotary Kiln              Capacity (volume)
                                   Direction (countercurrent vs.  cocurrent)
                                   Angle and rotational speed for residence time
                                   Optimal fuel and combustion regime

          Fluidized Bed            Capacity (volume)
                                   Optimal fuel and combustion regime
                                   Maximum operating temperature
i
"**N,
          Afterburner              Capacity (volume)
                                   Optimal fuel and combustion regime

          These  expected resulted  will  be essential  in  developing a cost-effective
          incineration  program  for the complete and safe  destruction  of the hazardous
          chemicals in  Basin  F  at  RMA.
                                               6-3

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                                  REFERENCES
Babcock and Wilcox.  1978.  Steam:   Its Generation and Use.   The  Babcock  and
    Wilcox Company, New York, NY.

Bonner, T. et al.  1981.  Hazardous Waste Incineration Engineering.  Noyes
    Data Corporation, Park Ridge,  NJ.

Dellinger, B.  Determination of the Thermal Decomposition Properites of
    20 Selected  Hazardous Organic  Compounds.   Prepared by  University of
    Dayton, Research Institute, Environmental Sciences Group, Dayton, OH.
    Prepared for Environmental Protection Agency,  EPA-600/2-84-138,
    August 1984, 204 pp.

Felder, R. and R. Rousseau.  1978.   Elementary Principles of Chemical
    Processes.  John Wiley and Sons.,  Inc., New York, NY.

Frankel, I., N. Sanders, and G. Vogel.  1983.  Survey of the Incinerator
    Manufacturing Industry.  Chemical Engineering Process 79(3):44-55.

Kramlich, J. et al.  Laboratory-Scale Flame-Mode Hazardous Waste Thermal
    Destruction  Research.   Prepared by  Energy  and Environmental Research
    Corp.,  Irvine,  CA.   Prepared  for Environmental  Protection Agency,
    EPA-600/2-84-086, April 1984,  155 p.
                                      A-l
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