ENVIROSCIENCE
                   MOBILE  INCINERATION SYSTEM SOLIDS TRIAL  BURN PLAN
                                       Prepared By

                                      IT Corporation
                                Edison,  New Jersey  08837
                                 EPA Contract 68-03-3069
                                           For
                          U.S.  Environmental Protection Agency
                      Municipal Environmental Research Laboratory
                      Solid and Hazardous Waste Research Division
                       Oil and  Hazardous Materials Spills Branch
                                Edison,  New Jersey  08837
                                    February 24, 1983
                      312 Directors Drive • Knoxville. Tennessee 37923 • (61 5) 690-3211
                                     Division of IT Corporation

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                            TABLE OF CONTENTS
                                                                     Page
  I.   PROJECT DESCRIPTION                                            1-1
      A.   Introduction                                               !_]_
      B.   Solids Incineration Scope                                  1-2
      C.   Proposed Trial Burn Dates                                  1-3

 II.   ENGINEERING DESCRIPTION OF THE MOBILE INCINERATOR              II-l
      A.   Process Description                                        II-l
      B.   Manufacturer's Name and Model Number                       II-l
      C.   Type of Incinerator                                        II-4
      D.   Linear Dimensions                                          II-4
      E.   Auxiliary Fuel Systems                      '               II-4
      F.   Solids Handling and Feed System                            II-7
      G.   Prime Mover Capacity                                       II-8
      H.   Automatic Waste Feed Cut-Off                               II-8
      I.   Stack Gas and Pollution Control Monitoring System          11-11
      J.   Nozzle and Burner Design                                   11-16
      K.   Water Injection                                            11-17
      L.   Materials of Construction                                  11-17
      M.   Location and Description of Indicating and Control  Devices  11-17

III.   TRIAL BURN PROCEDURES                                          III-l
      A.   POHC Selection Rationale                                   III-l
      B.   Waste Preparation                                          III-2
      C.   Solids Handling and Feed                                   III-6
      D.   Sampling Analysis and Monitoring Procedures                III-6
      E.   Detailed Test Burn Protocol                                111-15
      F.   Emission Control Equipment Description and Operating
          Conditions                                                 111-24
      G.   Procedures During Equipment Malfunction                    III-26
      H.   Trial Burn Inspections                                     111-29
      I.   Trial Burn Recordkeeping                                   111-33
      J.   Trial Burn Schedule                                        111-33
      K.   Site Cleanup                                               111-38
      L.   Quality Assurance Project Plan                             111-38

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                                  TABLES
Table
 No.                                                               Page
  1     Safety Interlock System                                     II-9
  2     Interlock Set-Points                                        11-10
  3     Continuous Stack Monitoring Analyses                        11-15
  4     Materials of Construction for Mobile Incinerator            11-18
  5     Pentachlorophenol Physical Properties                      III-3
  6     Stack Gas Analytical Methods                               III-ll
  7     Trial Burn Analytical Summary                              111-12
  8     Oxygen Analysis Method                                     111-16
  9     Carbon Dioxide Analysis Method                             111-17
 10     Carbon Monoxide Analysis Method                            111-18
 11     Oxides of Nitrogen Analysis Method                         111-19
 12     Sulfur Dioxide Analysis Method                             111-20
 13     Total Hydrocarbon Analysis Method                          111-21
 14     Trial Burn Operating Conditions                            111-22
 15     Operating Conditions for APC Equipment                     111-28
 16     Trial Burn Schedule                                        111-37

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                                  FIGURES

Figure
  No.                                                             Page
   1    EPA Mobile Incineration System                            II-2
   2    Block Flow Diagram of Mobile Incinerator                  II-3
   3    Dimensional Sketch of Rotary Kiln                         II-5
   4    Dimensional Sketch of Secondary Combustion Chamber        II-6
   5    Thermocouple Probe Detail                                 11-19
   6    Stack Gas Sampling Locations                             III-7
   7    Air Pollution Control  (APC) Equipment)                   111-25
   8    Dimensional Sketch of APC Equipment                      111-27
   9    RK/SCC Operating Log Sheet                               III-34
  10    APC Equipment Operating Log Sheet                        111-35
  11    Utility Operating Log Sheet                              111-36

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                                         1-1

                                      SECTION  I
                                 PROJECT DESCRIPTION

A.  INTRODUCTION
    This project  covers  the  solids  incineration  trial  burn  of  the  Environmental
    Protection Agency's  Office  of Research and Development's Mobile  Incinerator
    System by the Environmental Emergency Response Unit  (EERU)  at  the  Kin-Buc  land-
    fill site in  Edison,  New Jersey.   The system consists> of a rotary  kiln,  a  secon-
    dary combustion  chamber,  and an air pollution control train, each  mounted  on  a
    heavy duty over-the-road semitrailer.  The system  is  designed  for  field  use  to
    destroy/detoxify hazardous  and  toxic organic substances that have  contaminated
    soil or water at spill sites or at "orphaned" dump sites.   Liquids,  sludges,  and
    contaminated  debris  that have been shredded  or otherwise prepared  for  processing
    can be introduced into the  system.

    The system has previously undergone a rigorous three-phase trial burn  liquid
    incineration  program which  was  designed to minimize  the risk of  any  undesirable
    emissions to  the environment.   The three-phase program  involved  the  incineration
    of the following liquids:

         Phase I     -  Diesel oil only
         Phase II   -  A blend  of 20 to 23% carbon tetrachloride  (CC14), and
                        25-31% o-dichlorobenzene  (ODCB) dissolved in  diesel oil
         Phase III  -  A blend  of 2% tetrachlorobenzene,  11% trichlorobenzene, and
                        18-22% PCBs  as Arochlor  1260, dissolved in  diesel oil

    The Phase II  evaluations were completed and  showed destruction removal efficien-
    cies  (DREs) for  all principal organic hazardous  constituents  (POHCs) well  above
    99.99%.  The  Phase III evaluations are not yet completed but preliminary indica-
    tions show that  the DREs for the PCBs were acceptable.

    If, as expected,  the Phase  III  Toxic Substances  Control Act (TSCA) trial burn is
    successful, and  the mobile  incinerator obtains both  TSCA and RCRA  permits, a
    demonstration test of the mobile incinerator is  scheduled  for  August 1983  at the
    Kin-Buc  landfill in Edison,  New Jersey.

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                                         1-2

    During the Kin-Buc demonstration  test, oily  leachate  from  the  Kin-Buc  landfill
    will be incinerated.  During  the  Kin-Buc  demonstration,  EERU is  also proposing  a
    three-phase program of  solids incineration.

B.  SOLIDS INCINERATION SCOPE
    The scope of  the  three-phase  solids  incineration program would be as follows.

1.  Phase I
    During Phase  I, clean soil will be fed to the incinerator while  burning oily
    leachate.  The purpose  of this phase would be to determine practical operational
    ranges for the solids handling system, the inicnerator  ram feed  system, the
    rotary kiln  (inclination and  rpm), and the rotary kiln  ash handling system.
    Phase I will  not  be either a  RCRA or TSCA solids trial  burn since the  soil used
    will be certified as nonhazardous.

2.  Phase II
    During Phase  II a soil  contaminated  with  less than  50 ppm of PCBs will be fed to
    the mobile incinerator.  During this phase diesel fuel  will be used as auxiliary
    fuel rather than  the Kin-Buc  oily leachate.  The PCB  contaminated soil will be
    either a clean, artifically contaminated  soil,  or an  actual PCB  contaminated
    soil from an  existing site.   Phase II will be a RCRA  trial burn, but not a TSCA
    trial burn because the  PCB soil concentration will  be <50 ppm.   The purpose of
    this phase is to  demonstrate  the  mobile incinerator's capabilities for
    detoxifying contaminated soil.

3.  Phase III
    During Phase  III  a mixture of pentachlorophenol (PCP) and sand will be fed to
    the mobile incinerator.  During this phase diesel fuel  will be used as auxiliary
    fuel rather than  the Kin-Buc  oily leachate.  The PCP  will be fed as a  50% mix-
    ture of PCP in sand to  prevent the formation of pools of molten  PCP in the
    rotary kiln.  Phase III will  be a RCRA solids trial burn.  The purpose of this
    phase is to obtain a flexible solids RCRA permit for  the mobile  incinerator.

    The purpose of the trial burn is  to  evaluate and demonstrate the mobile
    incinerator's ability to safely destroy hazardous and toxic solid materials in

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                                         1-3

    accordance with the requirements of the Resource Conservation and Recovery Act
    (RCRA).  This objective will be met by:   (1) measuring the destruction and
    removal efficiencies  (DRE) for the specified test materials/  (2) determining
    particulate and acid gas removal efficiencies for the air pollution control
    equipment, and  (3) continuously monitoring the system's operating conditions and
    emissions.  In addition to defining the performance capability of the system,
    the data generated will furnish background information for subsequent permitting
    associated with the on-going use of the mobile incineration system for cleaning
    up spill and dump sites.  As such, the data quality level objective for this
    project is Level  2, requiring a high degree of quality coverage.

    The trial burn will consist of 2 tests each having three runs.  This trial burn
    plan covers all 6 runs.  The waste feed rates and trial burn protocol are
    discussed in Section  III-E.

C.  PROPOSED TRIAL BURN DATES
    The solids trial burn  for the mobile incinerator is planned for the last 7 days
    of the 30-day Kin-Buc  demonstration which is scheduled to start in mid-August.

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                                         II-l

                                      SECTION II
                  ENGINEERING DESCRIPTION OF THE MOBILE INCINERATOR

A.  PROCESS  DESCRIPTION
    The mobile  incineration system has  been designed and built to provide a mobile
    facility for  on-site  thermal  destruction/detoxification of hazardous and toxic
    organic  substances.   The total system consists  of:   (1) major incineration and
    air pollution control (APC) equipment mounted on three  heavy duty,  over-the-
    road, semi-trailers;  (2) combustion and stack gas monitoring equipment housed
    within a fourth  trailer; (3)  ancillary support  equipment.   As illustrated in
    Fig.  1,  the mobile  incineration system consists principally of a:   (1) rotary
    kiln;  (2) secondary combustion chamber (SCC);  (3) wetted-throat venturi elbow
    and quench  elbow sump;  (4) cleanable high  efficiency air filter (CHEAF);  (5)  MX
    (mass transfer)  scrubber; and (6) an induced draft (ID) fan.   Auxiliary equip-
    ment  consists of bulk fuel storage,  waste  blending and  feed equipment,  scrubber
    solution feed equipment,  ash  receiving drums, and an auxiliary diesel power
    generator.  A block flow diagram of the system  is shown in Fig.  2.

    The mobile  incineration system is controlled and monitored via electrical relay
    logic and conventional  industrial process  instrumentation  and hardware.   Safety
    interlocks  and shutdown features  comprise  a  major portion  of  the control  system.
    Fuel, waste,  and combustion air feed rates,  combustion  temperatures,  and  stack
    gas concentration of  carbon monoxide (CO), carbon dioxide  (C02), and oxygen (02)
    are continuously monitored, thus  assuring  compliance with  regulatory
    requirements.

B.  MANUFACTURER'S NAME AND MODEL  NUMBER
    The design  and procurement of  the mobile incineration system  was sponsored  by
    the Oil  and Hazardous Material  Spills  Branch (OHMSB) of the EPA's Municipal
    Environmental Research  Laboratory (MERL-Ci).  The initial  design was  developed
    by MB Associates.   Subsequent  design,  assembly,  and  modification was  performed
    by EERU's operating contractors  —  Mason and Hanger-Silas  Mason Company,  and  IT
    Corporation.  IT Corporation is  the  current  operating contractor for  EERU and is
    responsible for  final assembly,  inspection,  and  testing the system and  its  sub-

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                    BURNERS
                                      KIIM-SCC DUCT
   SOLIDS HAM
  FEED SYSTEM
       COMBUSTION GAS ANALYSIS
            (Oj. CO. C02)
                                                       SECONDARY
                                                       COMBUSTION
                                                        CHAMBER
                                                         COOLING
                                                         SHROUD
                                                           FAN
                                                                               .QUENCH ELBOW
                                                                                      CHEAF
                                                                                            REFLO DUCf
                                                        /STACK OAS ANALYSIS
                                                        (THC. NO,. SO], Oj. CO. COj)
                                                   7—IX-
                                                   t— I.D. FAM      I
   DESCniPTION
                                                                               KILN
                                                 SCC
                                   APC
OVERALL WIDTH: 2.4m
OVERALL LENGTH: 45.7 m
STACK HEIGHT. 9.1 m
OVERALL HEAT DUTY: 15 MILLION BTU/hr
ELECTRICAL REQUIREMENTS: 100 kW

WEIGHT TRAILER 1 - 42.000 Ib (19.051 kfl)
WEIGHT TRAILER 2 - 67.000 Ib (25,855 kg)
WEIGHT TRAILER 3 - 36.000 Ib (16.329 kg)
TEMPERATURE:
PRESSURE:
GAS RESIDENCE TIME:
EXCESS OXYGEN:
1.000C
- 1.000 Pa
2 sec
4 percent
FEED RATES (AT 20 PERCENT XS AIR)
AIR:                         aS
FUEL OIL:                    285 L/hr
WASTE SOLIDS:               68 kg/min
WASTE OIL:                   227 L/hr
WATER:                      680 L/hr
                                                DISCHARGES
                                                ASH:
                                                WASTE WATER:
                             NONE
1,200 C
- 1,500 Pa +
2 sec
4 percent
                   34m'/min
                   150 L/hr
                   NONE
                   NONE
                   NONE


                   NONE
                   NONE
80 C
- 10K Pa

4 percent
                NONE
                NONE
                NONE
                NONE
                                                                PARTICULATE FILTER MEDIA
H
to
                                                + 1.000 PASCAL « 4 in H, O
                                                * DEPENDENT UPON FEED MATERIAL
                                          FIG. 1  EPA MOBILE INCINERATION SYSTEM - DESIGN SUMMARY

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                       SAMPLE
AIR
                                                       OFF QAS
                                  LI   i_J
                                                                                  H
                                                                                  I
                                                                                  U)
           FIG. 2 BLOCK FLOW DIAGRAM OF MOBILE INCINERATION SYSTEM

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                                        II-4

    sequent  field  operations  as  a mobile  hazardous and toxic material destruction
    system.   The system,  being one-of-a-kind and custom designed,  has no model
    number.

C.  TYPE OF  INCINERATOR
    The mobile  incinerator is a  rotary kiln (RK) incinerator with  secondary com-
    bustion  of  the kiln  combustion gases  in a fuel oil fired secondary combustion
    chamber  (SCC)  (see Fig.  1).

D.  LINEAR DIMENSIONS AND CROSS  SECTIONAL AREA OF THE MOBILE INCINERATOR

1.  Rotary Kiln
    The rotary  kiln  is a carbon  steel  shell lined with 6 inches  of castable refrac-
    tory.  The  RK  is a cylindrical shell  which is 16 ft long and has  a 4 ft-4 in.
                                                               2
    inside diameter  (ID).   The cross sectional area  is 14.75 ft  and  the RK volume
              3
    is 236 ft .  Figure  3 is  a dimensional sketch of the rotary  kiln.

               \
2.  Secondary Combustion Chamber
    The secondary  combustion  chamber  (SCC)  is  a carbon steel cylindrical shell lined
    with 6 in. of castable  refractory.  The SCC  is  36  ft  long and has a  4 ft-4  in.
                                               2
    I.D.  The cross sectional area is  14.75 ft
    Figure 4 is a dimensional sketch of the SCC.
                                          2                             3
I.D.  The cross sectional area is 14.75 ft  and the SCC volume is 531 ft •
E.  AUXILIARY FUEL SYSTEMS
    Both the RK and the SCC have fuel oil-fired auxiliary fuel systems.

1.  Rotary Kiln
    The RK is fired by two 4-in. Maxon burners, each of which is  capable of a  12:1
    turn down and close fuel/air ratio compliance throughout this range.  These bur-
    ners have high-turbulence and short flames which result in high intensity  com-
    bustion.  Each Maxon burner is rated at about 4 MM Btuh.

2.  SCC
    The SCC auxiliary fuel system consists of two tangentially fired fuel oil  bur-

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                     • WATER INJECTION PORT
    SOLIDS RAM
   FEED SYSTEM
RAtA FCCO { (If*V»»«*.'
               ROTARY KILN
                                                                                     H
                                                                                     I
                                                                                     01
           Fig.  3.   Rotary Kiln  Sketch
                  with Dimensions

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I III
r 1 1





* *
3=
c— V
,' O '
\ v-' '
\^ ^/
1





L


a
i
                            SECONDARY

                            COMBUSTION

                             CHAMBER"
                                                                            i
                                                                           en
SECONDARY COMBUSTION CHAMBER AND QUENCH
           Fig.  4.  Secondary Combustion Chamber

                 Sketch with Dimensions

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                                         II-7

    ners which are used  to  increase  the temperature of the incoming RK combustion
    gas.  The incoming RK gas  enters the SCC  axially through spin vanes which impact
    a swirling and mixing action  to  these gases.   The RK gases are mixed and con-
    tacted with  the hot  gases  from the two SCC burners because of the design of the
    inlet spin vane and  the tangentially fired burners.   Sach burner is rated at
    about 2.8 MM Btuh.

F.  SOLIDS HANDLING AND  FEED SYSTEM
    The solids materials to be incinerated during the trial burn will be contained
    in drums and will be fed to the  ram feed  hopper either by a drum handling
    vehicle or by a drum loading  mechanism.   The  ram feed hopper will have  a dust
    cover and seal which will  allow  dumping of the drum  but prevent fugitive dust
    emissions.   The hopper  will also be connected to the combustion air blower  air
    inlet and therefore  under  a slight negative pressure which will also prevent
    fugitive dust emissions from  the hopper.

    A ram feeder processes  all solid wastes into  the kiln.   The ram feeder  is
    hydraulically operated  with a 31/4-in.  diameter by 121-in.  stroke cylinder.   It
    has the capacity of  ramming up to 2 ft in 30 seconds as well as partial volumes
    over longer  periods.  The  rate of ram  feed will be determined by the charac-
    teristics of the material  being  destroyed  and will be easily field controlled
    for both volume and  speed.  The  leading edge  of the  ram will have  a shearing
    edge to further reduce  potential ram jam-ups.

    The solids volume feed  control will be effected by controlling the ram  pullback
    position so  that the  kiln  can be charged frequently  with partial loads  and
    thereby reduce combustion  transients  or localized starved  air conditions  to  the
    kiln.   Swing-up gates have  been  incorporated  in the  trough bottom to isolate the
    shredder from the kiln  atmosphere.   Each swing gate  functions  sequentially as
    the ram advances and  retracts.   Swing  gates were chosen in order to avoid slots
    and slide grooves which can be easily  fouled  with sand,  dirt,  oil,  or debris.
    Gate postion switches control and limit ram movement in order to prevent the
    possibility  of uncontrolled air  entering the  kiln.

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                                         II-8

G.  PRIME MOVER CAPACITY
    The mobile incinerator  has  three  main fans:  a RK combustion air blower,  a SCC
    combustion air  blower,  and  a  single-stage  induced draft fan.   The induced draft
    fan is the system prime mover.  The  capacities of the three fans are as  follows:
              RK  combustion  air  blower
              SCC combustion air blower
              Induced draft  fan
2200 acfm at 30 in.  w.c.
1760 acfm at 28 in.  w.c.
9,100 acfm at 42 in.  w.c.  at 175°F
  inlet
    The induced draft fan  is  connected  to  a  variable  speed motor.   The  volumetric
    flow rate to the fan is controlled  by  adjusting the  variable  speed  motor which
    drives the fan.  The fan  is  driven  by  a  155-hp diesel  engine  and  operates  at a
    nominal speed of 3,350 rpm.

H.  AUTOMATIC WASTE FEED CUT-OFF
    The mobile incineration system uses  electrical relay logic  and  conventional
    industrial process  instrumentation  and hardware.   Instrumentation is designed to
    monitor process conditions,  provide  data for assuring  compliance with regulatory
    requirements, and assure  appropriate process response  and control,  operational
    flexibility, and safety interlocking and shutdown  features.   The safety
    interlocks and shutdown features comprise a major  portion of  the control system.

    Safety shutdown responses identified in  Tables 1 and 2 are  relayed  to various
    equipment items when certain process limits are reached or  not  met.  In general,
    the process parameters that  alert and  initiate responses to alarm conditions
    are:
    1.    High and low kiln temperature
    2.    High and low secondary combustion chamber  temperature
    3.    Low secondary combustion chamber outlet oxygen  (O2)  level
    4.    Low flow in the quench, particulate scrubber, or mass  transfer scrubber
         sumps
    5.    Very low level in the quench, particulate  scrubber,  or mass  transfer
         scrubber sumps

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                                TABLE 1 SAFETY INTERLOCK SYSTEM
                                 KILN
SCC
QUENCH
CHEAP I MX SCRUBBER
KILN BURNERS
SCC BURNERS
EMERGENCY VENT
ID FAN
CAUSTIC FEED PUMP
QUENCH SUMP PUMP
KILN RAM FEED
WASTE OIL FEED
X





X
X
X





X
X






X
X






X
X
X
X




X
X
X
X

X


X
X






X
X






X
X
X
X




X
X
















X
X



X
X
X
X
X
o



X
X
X
X




X
X






X
X






















X
X
X
X




X
X












s









X
X
X
X
0
X


X
X



X




                 KEY:
                 X -TURNS OFF
                 S - STARTS
                 0 - OPENS
                D- BLANK INDICATES EQUIPMENT STAYS ON. ALARM BUZZER SOUNDS
                                                             H
                                                             H

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                                   11-10
                                  TABLE 2
                       SAFETY INTERLOCK ACTION VALUES
Kiln
    High Gas Temperature
    Low Gas Temperature
SCC
 >1900°F
 <1400°F
    High Gas Temperature
    Low Gas Temperature
    Low Oxygen Concentration
Quench
    Low Recycle Water Flow to Nozzles
    Low Low Water Level in Sump
    Low Make-up Water Flow to Nozzles
 >2400°F
 < 2060°F
 < 40 gpm
 < 5 in.
 < 5 gpm
CHEAF
    Low Water Flow to Nozzles
    Low Low Water Level in Sump
    High Gas Temperature

MX Scrubber

    Low Water Flow to Nozzles
    Low Low Water Level in Sump
< 8 gpm
< 4 in.
>240°F
< 100 gpm
< 6 in.
ID Fan
    Loss of Vacuum
    Excess Fan Vibration
>-20 in.  W.C.
>0.003 in.  amplitude

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                                     11-11

 6.   High gas temperature or pressure in the quench  section
 7.   High pressure at the induced-draft inlet
 8.   High vibration of the induced-draft fan
 9.   Insufficient burner air or fuel supply

 The fuel oil burner system includes an internal interlock system that shuts down
 the burner system (i.e.,  fuel oil flow) if:  a flame is detected during
 pre-ignition,  the pilot fails to ignite,  the burners fail to ignite, or there is
 a  loss  of flame  after ignition.   A shutdown of the burners automatically stops
 waste feeds.

 During  an alarm  condition,  waste and fuel oil feeds are immediately stopped.
 When  required  the induced-draft  fan shuts down and the emergency vent located
 between the  quench sump and CHEAP opens.   All recycle and makeup water flows  are
 maintained,  if possible,  to prevent over-heating in the mass  transfer scrubber.
 The safety interlock  system is designed to provide protection both  for operating
 personnel and  for the incineration equipment.

 During-  the solids trial burn, the ram  feed mechanism  will  be  interlocked with
 the carbon monoxide  (CO)  stack monitor.  If,  during solids  feeding,  the CO  con-
 centration in  the stack exceeds  150 ppmv-dry gas basis,  the ram feeding mecha-
 nism will be shut down and  an alarm will  sound.  The  fuel  oil burners  in the RK
 and SCC,  however,  will continue  to operate  since a volume  of  unburned  solid
waste which  requires  secondary combustion will  still  remain in the  kiln.   The
 interlock system will prevent any  operation  of  the ram  feed until the CO stack
 concentration  drops below 150 ppmv-dry basis.

 STACK GAS AND  POLLUTION CONTROL  MONITORING SYSTEM
Since the mobile  incineration system was designed  to  safely destroy or detoxify
a wide  range of hazardous wastes,  an important  aspect of the  design was to pro-
vide a  monitoring system which would analyze the flue and  stack  gases for  com-
bution  components  [carbon monoxide  (CO), carbon dioxide  (C02),  and  oxygen  (02)]
and emission components [(oxides of  nitrogen  (NOX), sulfur dioxide  (SO2),  and

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                                    11-12

 total  hydrocarbons  (THC)].   The stack monitoring system principally serves two
 critical functions:   (1)  it provides  the operators with current data on the per-
 formance of  the  incineration and gas  cleaning processes; and (2) it generates
 and  records  accurate  data on the gas  emissions from the process.  This ensures
 operator safety  and compliance  with operating permit requirements.   Functional
 requirements were met by  the selection of a dual gas chromatograph (GC) system
 that possesses a high level of  reliability and versatility,  and conforms to the
 mobile nature of the  incineration system.

 The  selection of a process  GC over other available monitoring systems  was  based
 on the ability of a single  vendor to  provide a complete analytical  system  that
 could withstand  the extreme operating conditions of the mobile  incinerator.   The
 previously cited conditions,  in conjunction with the very  nature of chemical
 waste, incineraiton, produce an  extremely difficult gas  sampling environment  —
 hot  (2,200°F), wet  (50 volume % water),  and dirty (1-2  gr/scf).   The stack gas
 monitoring system selected  consists of  three subsystems:

       •  Gas sampling/conditioning
       •  Gas analysis/analyzer calibration
       »  System control/results  reporting

 Gas  Sampling and Conditioning
 The  gas  sampling conditions  in  the mobile  incinerator present the most  difficult
 (hot, corrosive, wet,  and dirty)  aspect  of the  gas  analysis.  In order  to
 reliably  and accurately extract,  condition,  cool,  and dry  gas samples under
 these conditions, two Bendix  Model  8901C Stack  Prove/Conditioning Assemblies
were selected.   Several favorable  characteristics  of this  model are that the
 materials of construction are highly  resistant  to corrosion  and the assembly  is
 able to  cool and dry  gas  samples with very little  loss  of  sample components.

Two  gas  sampling/conditioning assemblies are used to provide separate gas
 samples  for the  measurement of  combustion  parameters and emission levels.  The
 qas  sampling/conditioning subsystem consists  of  two identical assemblies;  one
assembly  is mounted on the exit duct from  the SCC  before gas quenching  and the
second assembly  is mounted on the incinerator stack.  The  need  for  separate

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                                     11-13

 samples  for each analysis arises from the desire to optimize the combustion gas
 analysis (CO,  C02/  and O2) by extracting the sample as close to the incineration
 process  as  possible.   These assemblies,feed conditioned gas samples through
 umbilical tubes to the gas analyzer and control units which are housed in a
 fourth trailer that is dedicated to analytical support.

 Since  the combustion gas  sampler/conditioner assembly will collect a sample at
 the  SCC  exhaust before gas quenching,  the gas sampled:  (a) will be relatively
 dry  which minimizes potential problems in the gas sampling/conditioning unit;
 and  (b)  has not been diluted with ambient air from in-leakage through openings
 in the negatively pressured air pollution control equipment.

 The  second  stack probe/conditioning assembly is located  on the incinerator stack
 to collect  gas samples for emission measurement.   Construction and operation of
 these  assemblies is identical.

 Gas  sampling is done  with a corrosion  and  temperature resistant ceramic probe
 which  extracts gas  samples from the center of the process  duct.   The extracted
 sample passes  through a ceramic inertial filter,  located inside the probe,  to
 remove particulate  ir^terial (5pm) from the gas  sample.   Next,  the filtered gas
 sample is partially cooled in an air-air heat exchanger  to lower the temperature
 to 212-248°F (100-120°C);  entrained liquids  are collected  in  a liquid trap at
 the  bottom  of  the exchanger.   The gas  sample then passes through a vaporizer
 248°F  (120°C)  to ensure that all entrained liquids  from  process or instrument
upsets are  vaporized  before the gas drying process.   Gas drying is accomplished
in a Perma  Pure  dryer which removes water  vapor from the gas  sample without
using  a  condensation  process that often  scrubs  key gas components from the
sample.  The drying process transfers  the  water vapor from the gas sample
through  a tubular plastic  membrane  to  clean,  dry [110°F  (43.3°C) dew point],
sweep  air on the  outside  of the dryer.   The  filtered,  cooled,  and dried gas
sample is then transported to the analyzers  (discussed in  the next section)
through  Teflon tubing.  Pressure switches  in the stack probe/conditioning
assembly monitor  gas  sampling and conditioning operation for  particulate build-
up or  plugging.   When appropriate,  the unit  automatically  back-purges itself
with steam  or  compressed air to maintain reliable,  long-term  untended operation.

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                                        11-14

2.   Gas Analysis/Analyzer Calibration
    The cleaned gas sample, from the combustion  gas  and  stack  sampler/conditioning
    assemblies, enters the analyzer section  of the system through  a Bendix
    Model 890B Dual Steam Transport Assembly.  The transport assembly  delivers  the
    gas samples from either gas sampling  location to the appropriate analyzer.   The
    analyzer section operates in conjunction with the monitoring system controller
    to divert gas samples:  (1) to the thermal conductivity detector GC for  analysis
    of C02, 02/ and SO2;  (2) through a methanizer to a flame ionization detector GC
    for analysis of CO;  (3) to the flame  ionization  detector GC  for analysis  of  THC;
    and (4) a chemiluminescent detector for  analysis  of  NOX.   The  analyzer section
    also introduces calibration gas (from cylinders)  through the sampling/condition-
    ing units to the appropriate analyzer.   The  analyses  conducted by  the  continuous
    analyzers are summarized in Table 3.

    The decision was made to use process gas chromatographs to perform the majority
    of the analyses for the following reasons:    (1) The  expensive  analyzer detectors
    would be protected from corrosive gases  or submicron particulate,  which may  be
    present due to process upsets or failure of  the sample conditioning system,  by  a
    relatively inexpensive GC column;  (2) The front end  components  of  a GC system,
    such as tubing and sampling valves,  are  readily available in the corrosion
    resistant materials that are required to transport gas samples;  (3)  The ver-
    satility of a thermal conductivity/flame ionization  GC system permits  simple and
    inexpensive modifications  to the gas analysis to  include additional  or very  spe-
    cific components;  (4) Gas  chromatography offers the  ability to  more  readily
    remove interfering components from a gas sample before reaching  the  analyzers
    than do spectrometric analyzers;  and  (5) The components of the  analyzers are
    more resistant to problems associated with a mobile  field system,  e.g., vibra-
    tion.   Calibration of the  analyzers  is accomplished using cylinder  gas standards
    which  are injected into the monitoring system at  the sample probes.  This
    calibration method not only calibrates the analyzers but accounts  for  component
    losses that are related with sample  conditioning  and transportation.
    Calibration of the analyzers is directed by the monitoring system  controller on
    a  repeated,  specified basis.

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                      11-15
Table 3.  Continuous Stack Monitoring Analyses
Analysis
Combustion
Gas
Combustion'
Gas
Combustion
Gas
Stack Gas
Suck Gas
Stack Gas
Component
CO
CO,
o,
NO,
SO,
THC
Sample
Location
sec
sec
Stack
Stack
Stack
Stack
Analyisr
Mathanizar-GC/FlO
3endix .Modet 9220
GC/TC
Sandix Model 9120
GC/TC
Sendix Model 91 20
Chemiluminescsncs
Sandix Modal 3102
GC/TC
Sandix Modal 9120
GC/FtO
3«ndix Modal 9220
Anaiysia
Range
0-3SO ppm
0-10 parcsnt
0-3 peccant
0-200 ppm
0-2000 ppm
0-200 ppm
Analysis
Tima
S min
S min
S min
on line
S min
5 min

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                                        11-16
3.  System Control/Results Reporting
    Two microprocessors control:   (1) the  two  gas  sampling/conditioning assemblies;
    (2) the sample transport and calibration systems;  and (3)  the  gas  analyzers.
    One of the microprocessors is  dedicated to controlling the flame  ionization GC.
    The second microprocessor controls  the thermal conductivity GC, collects  data
    from the chemiluminescence detector, and generates  analytical  reports  on  a
    remote computer terminal.

    In addition to controlling GC  functions, the microprocessors continuously:
    (1) control analyzer calibration  (zero, span,  and  drift) and sequencing of
    sampling probe back flush; and (2)  monitor for low  flow of calibration gases,
    for low flow of gas sample, for high component concentration,  and  for  system
    utilities.  The ability of the microprocessor  to completely monitor  and operate
    the samplers and analyzers permits  operation of the mobile incinerator in remote
    locations with a minimum technical  staff.   As  well  as  controlling  the  entire
    analytical system, the microprocessors perform another important task.  That
    task is the generation of calibration  reports, analytical  result reports,  time-
    weighted average reports, analytical system alarm conditions,  and  incinerator
    excess emission reports.

J.  NOZZLE AND BURNER DESIGN

1.  Rotary KiIn
    The RK incinerator includes three burners  — a waste oil burner which  will  not
    be used during the solids trial burn,   and  two  identical Maxon  Multifire II
    burner assemblies.  The two Maxon burner assemblies will be fired  with deisel
    oil during the solids trial burn.   Each burner is a 4-in.  model No.  31534 and is
    rated at up to 3.9 MM Btuh.   The diesel oil is air atomized at a combustion air
    pressure of about 14 ounces per square inch.   The combustion air is  supplied by
    the combustion air blower described in Section III-G.  Maxon bulletin  4200-77,
    which describes the nozzle and burner  design of these  burner assemblies,  is
    included in Appendix B.  The RK burner locations are shown in  Fig.  3.

2.   Secondary Combustion Chamber
    The two secondary combustion burner assemblies are also Maxon  Multifire II  bur-

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                                        11-17

    ners.  Each burner  is  rated  at about  2.8 MM Btuh of diesel oil.   The diesel oil
    is air atomized at  a combustion air pressure of about 14 ounces  per square inch.
    The combustion air  is  supplied by  the SCC combustion air blower  described in
    Section III-G.  Maxon  bulletin 4200-77,  which describes the nozzle and burner
    design of these burner assemblies,  is included in Appendix B.  The  SCC burner
    locations are shown in Fig.  4.

K.  WATER INJECTION
    During liquids only feed  to  the RK, clean atomized water at 1  to 2 gpm is
    injected into the RK for  temperature  control.   During the solids trial burn
    while water injection  will probably still be done,  the rate of water injection
    will be lower than  1 to 2 gpm  because of the moisture present  in the soil.   The
    actual rate of water injection during the solids trial burn will depend on  the
    moisture content of the soil that  is  incinerated during the trial burn.

L.  MATERIALS OF CONSTRUCTION
    The materials of construction  of the  major mobile  incinerator  components  are
    summarized in Table 4.

M.  LOCATION AND DESCRIPTION  OF  TEMPERATURE,  PRESSURE,  AND FLOW INDICATING AND
    CONTROL DEVICES
    The location of the mobile incinerator sensors  can  be found in the  P&IDs
    included in Appendix C.   A description of  the  various  sensors  is  as  follows.

1.  Kiln and Secondary  Combustion  Chamber Combustion  Temperature
    The combustion gas  temperatures of  the rotary kiln  and secondary  combustion
    chamber are measured with a  type S  (platinum/10% rhodium)  thermocouple.
    Thermocouple accuracy is ±0.5%  from 540  to 1480°C.  The  thermocouples  are
    located within a special thermowell designed to  measure  the  combustion  gas tem-
    perature while avoiding the  influence of radiant heat from the flame envelope
    (see Fig.  5).   This is achieved by aspirating the combustion gases  through the
    thermowell assembly and over the surface of  the  shielded  thermocouple.  The hot
    gases  are  then returned to the  combustion  chambers.   The  output  of  the  ther-
    mocouple is  converted and transmitted as a current  signal  to an  analog process

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                                          11-18
                         Table 4.  Materials of Construction
                                  Mobile Incinerator
          Component
          Materials of Construction
Rotary kiln

RK/SCC transition duct
Secondary combustion chamber
Quench elbow
Quench elbow sump
Duct, sump to cheaf
CHEAP
MX scrubber
ID fan

Stack
Carbon steel (A-36) lined with A.P. Green
  Kast-0-Lite 30
Inconel 601
Carbon steel (A-36) lined with Kast-O-Lite 30
Inconel 625
Inconel 625
Inconel 625
Inconel 625
Fiber reinforced plastic (FRP)
Housing (347 stainless steel), shaft and
  impeller  (Inconel 625)
304 stainless steel

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    11-19
Fig. 5
                                      PIPE

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                                        11-20

    controller.  A change from setpoint causes  the  controller to adjust the com-
    bustion air flow in the kiln by  means  of a  flow control  valve.   In the secondary
    combustion chamber, however, a change  in setpoint causes this controller to
    adjust both tuyere  (over fire) air and combustion air.   In both cases  a change
    in combustion air flow causes a  change in back  pressure  in the  air lines to the
    burners.  This pressure change causes  a change  in fuel oil feed to the burners
    by means of flow control valves, which are  set  to feed fuel oil to the burners
    in the correct proportion based  on the air  feed back pressure.

    The output from the controller is also sent to  a recorder with  high and low
    alarm functions.  A high or low  temperature will activate an alarm at  the
    appropriate control panel.  A high or  low temperature in the kiln  or secondary
    combustion chamber will also shut down the  waste liquid  and solids  feed by  means
    of an. electric signal from these alarms.  This  electric  signal  will close double
    electric solenoid valves on the waste  liquid feed  line and deactivate  the con-
    veyor motor and timer/sequencer  for the waste solids feed system.   In  addition,
    a high temperature will also cause the  shut off  of auxiliary fuel  to the auxi-
    liary fuel burners.

2.  Waste Liquid Flow
    Waste liquid flow is measured by a micro-motion, gyroscopic/coriolis mass flow
    meter.   Optical measurements are processed  electronically  and the output is
    displayed digitally.  The waste  liquid  flow is  controlled  manually  by  a needle
    valve located before the meter flow.   Accuracy  of  the flow  meter is  ±0.4% from
    0.68 kg/min (1.5 Ib/min) to 13.6 kg/min (30 Ib/min).

3.  Waste Solids Feed
    The feed rate of waste solids to the rotary kiln is controlled  by a  mechanical
    timer/sequencer that cycles the positions of a hydraulically operated  hopper
    door,  a hydraulic feed ram,  and a pneumatically  operated kiln entrance  door.
    The hopper door and feed ram are positioned by  solenoid  controlled hydraulic
    valves.   The kiln entrance door is positioned by a solenoid  controlled  ph'eumatic
    valve.   Positions are  verified through electrical signals  sent  by position
    switches.   These position switches also provide  lockout  functions to ensure

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                                        11-21

    proper sequencing of the individual units.   The desired feed rate is obtained by
    adjusting of the cycle time and pull back position  of  the ram feeder (volume).
    Manual switches for each of the three units  are available for manual operation.

    If a high pressure condition is met in  the ram  hydraulic system (ram feed jam)  a
    pressure switch will activate a panel mounted alarm.   Solid feed stops  and must
    be reset manually.  High CO stack concentrations will  also activate  an  alarm and
    stop the solid feed until reset manually.

4.  Air Pollution Control Equipment Pressure Drop
    Pressure drop is controlled across  the  filter medium in the CHEAP (cleanable
    high efficiency air filter) by means  of  a differential pressure switch.   When
    the loading of particulate on the filter causes a pressure drop exceeding a set-
    point, the differential pressure switch will activate  and transmit an electric
    signal to the filter advance motor.   This motor will start and  advance  clean
    medium until the pressure drop returns  to normal, then the differential pressure
    switch will de-energize and turn off  the filter advance  motor.

    Pressure is also monitored at the exit  from the mass transfer scrubber.   Upon
    detection of a loss of vacuum (high negative pressure)  a pressure switch  will
    activate an alarm at the appropriate  control panel and also shut  down the  waste
    feeds.

5.  Combustion Gas Flow
    Measurement of combustion air flow is performed by a (Annubar)  differential
    pressure cell located at the inlet to the kiln air blower.  Accuracy of the
    measurement is dependent on the geometry near the sensor  and can  be determined
    through field calibration.   Output from the differential  pressure transmitter in
    the form of a current signal is sent to a square root  converter and subsequently
    to an analog process controller.   The combustion air flow to the kiln supplies
    combustion and atomizing air to the burners,  air to the pilot burners,  and purge
    air to the burner flame detectors.   These air usages are  at set rates or  are
    controlled by other systems.   The residual air flow is  then sent  to the kiln
    tuyere (over fire).   This kiln tuyere air flow is controlled at a constant rate

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                                        11-22

    by the kiln air process controller through a flow control  valve.   Therefore,
    adjusting the tuyere air will maintain a constant total air  flow when  slight
    changes occur in air usage by other systems.  Additional air leaks into  the kiln
    through the front and rear kiln seals and the hot ash discharge.

    Total air flow to the secondary combustion chamber is similar to the kiln.
    However, tuyere air to the combustion chamber is held constant, thereby  allowing
    the total air flow to the combustion chamber to vary as other systems  require
    air.  These systems are identical to the air-using systems in the  kiln.

    The total flow of combustion gases is the sum of kiln air  flow, secondary com-
    bustion air flow, combustion products, and any infiltration  air.

6.   Burner Control System
    The combustion chamber pressure is used to regulate the fuel to air ratio for
    the auxiliary fuel burners.   Fuel is controlled by a pneumatic control valve
    that uses as pneumatic inputs the combustion chamber pressure and  the blower air
    pressure.  Therefore,  a change in these pressures will cause a corresponding
    change in the amount of fuel feed to the burners.

    Fuel feed to the burners is monitored by a pressure switch.  Upon detection of a
    low fuel pressure to the burners,  an electric signal will be sent to a normally
    open solenoid valve to shut off fuel flow.

    The differential pressure between the blower outlet and the combustion chamber
    is monitored by a differential pressure switch.   When a low differential
    pressure is detected an alarm will sound in the appropriate control panel and
    the fuel to the auxiliary fuel burners will be shut off.   This is  accomplished
    by means of an electric signal from the differential pressure switch to the fuel
    shut-off solenoid valves.

    The presence of a flame is monitored by an ultraviolet flame detector.   The
    detector is  purged with air  to maintain a clear line of sight to the flame enve-
    lope.   Upon  detection  of  no  flame  an alarm will sound at the appropriate control

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                                        11-23

    panel and the fuel to the auxiliary  fuel burners  will  be  shut off  by means of
    the fuel shut-off solenoid valves.

    A second low-level sensor is used to monitor  very low  water  levels in the  recir-
    culation sumps.  Upon detection of a very low level  the differential pressure
    switch will transmit an electrical signal to  activate  an  alarm and to shut off
    waste liquid and solid feed streams.   In addition a  very  low level in the  quench
    sump will shut off auxiliary fuel to the burners  by  means  of the auxiliary fuel
    solenoid valves.

    Each of the sumps has provisions for gravity  drains  for high sump  water  levels.
    These sumps are also equipped with high  level  sensors.  Upon detection of  a high
    level above the drain outlet the differential  pressure switch  will transmit an
    electric signal to an alarm at the appropriate control panel,

7.   Scrubber Water Flow
    Water is supplied to the air pollution control system by three  separate  cir-
    culation systems.  These are the quench, CHEAF, and  mass transfer  water  cir-
    culation systems, each of which has a dedicated recycle pump.   Flow  is measured
    and indicated by rotometers for each system.   Flow is assured  by maintaining  a
    minimum water level in each of the sumps supplying each pump.   Water  levels are
    measured by differential pressure level  sensors using instrument air.  Upon
    detection of a low level,  the differential pressure  switch will transmit a
    current signal to open a normally closed solenoid valve and  allow  makeup water
    into the sump.   In the quench system, however, a  low level in  the  quench sump
    will allow  additional makeup water to be added to cool and saturate the com-
    bustion  gas  stream.

    Each of  the  rotometers,  indicating flow for the three water  circulation systems,
    contain  magnetic switches  that will activate alarms under low flow conditions.
    Upon detection of low flow,  these switches will transmit an  electric signal to
    activate an  alarm and to shut off waste feed.   In addition,  a  low  flow in the
    recirculated quench water  systems will also shut down all burners.

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                                          11-24

 8«  pH  of  the  Scrubber Water
     The pH of  the  scrubber water in each of the three water circulation systems is
     measured by  a  pH electrode system.   The system consists of three electrodes,  a
     reference  electrode (silver/silver  chloride),  a thermal compensator,  and the  pH
     electrode.   Accuracy  of the electrodes  is ±0.02 PH units from a pH of 2 to 12
     from 0°c to  110°C.  The potentials  from the electrodes  are amplified,  processed
     and transmitted  as  a  current signal to  an analog process controller.   The
     controller,  upon detection of a PH  below setpoint,  will open  a normally closed
     solenoid valve and  allow instrument air to activate a pneumatic control valve.
     This then  allows  caustic solution to be pumped  into the water circulation
     system.  Detection  of  normal operating  conditions will  deactivate  these sole-
     noids  and  subsequently  close the control  valves.

 9.  Miscellaneous Control  Instrumentation

 a.  Hydraulic Systems — The hydraulic  systems  for  the  solid waste  feed and  the kiln
     rotation are monitored for high hydraulic pressure.  Upon detection of  a high
     hydraulic presure in either  system,  a pressure  switch will transmit an electrical
     signal to activate an alarm on the appropriate  control panel.

 b.  Kiln and Secondary Combution Chamber Oxygen Analyzers (See Section I)

 c.  Kiln Ash Discharge — Ash discharged from the rotary kiln is controlled by a
     mechanical  timer/sequencer that alternates the opening of a double door
     discharge  chute.   The  timer transmits an electric signal to activate a solenoid-
     controlled  pneumatic,  rotary actuator on each door.   Instrument air is used for
     the  pneumatic actuators.   Manual switches are available  for manual operation of
     the  ash discharge system.  Manual operation is required  for waste liquids only
     feeding, but  can  be  automatic when solid wastes  are  fed.

d.   Kiln Process  Water —  The addition of process water  to the kiln is  controlled  by
     the kiln oxygen analyzer.   Flow is indicated by  a rotometer.

e.   Emergency Vent  — An emergency vent  is located before the combustion gas inlet
     to the  CHEAF  to protect against high temperatures  caused by loss of quench

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                                      III-l

                                     SECTION III
                                TRIAL BURN  PROCEDURES

A.  POHC SELECTION RATIONALE

1.  Polychlorinated Biphenyls  (PCS)  in  Soil at <50 ppm
    One of the main uses  of the mobile  incinerator will be to incinerate soils con-
    taining low  levels  of hazardous  and toxic  organics such as those caused by chem-
    ical spills  or those  occurring at inactive sites.   It is therefore important to
    test the mobile incinerator capabilities for  desorbing and destructing a low
    concentration of a  test chemical from  a soil.

    Two soil alternates are presently being considered for the trial burn;  clean
    soil which is artifically  contaminated with Arochlor 1260,  or actual PCS con-
    taminated soil from a spill clean-up.   The actual  contaminated soil needs to
    contain only PCBs at  <50 ppm.

    PCBs were selected  as the  test chemical for the  following reasons:

    a.   High adsorption  to soil  - chlorinated organics  such as  PCBs are highly
         adsorbed to soils as  evidenced by high soil adsorption  coefficients (KOC).

    b.   Wide range of  KOCs -  different PCB isomers  have a wide  range of KOCs.
         Analysis for PCBs in  the stack  gas  and RK ash will therefore result in
         data which will  indicate the importance  of  KOC  for many different  chemicals
         as a function  of KOC.

    c.   Existing PCB data base  - In  January 1983, EERU  completed a TSCA PCB trial
         burn in which diesel  oil containing 18 to 22% Arochlor  1260 was incinerated
         by the mobile system.  Preliminary  indications  are that all TSCA require-
         ments were met or exceeded  durng  this  testing.

2.  Pentachlorphenol/RCRA Permitting
    Another use of the mobile  incinerator  will  be  the  disposal of solid chemical

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                                       III-2

    wastes either in  drums  or  in  bulk.   In  order to do this it will be necessary to
    obtain a national RCRA  solids  permit through the trial burn process.   In order
    to obtain a. flexible RCRA  permit  which  will require a minimum of new trial burns,
    an Appendix VIII  solids  constituent  should  be selected which is high up on the
    EPA's Incinerability Ranking  List.   In  selecting pentachlorophenol (PGP),  the
    following criteria were  evaluated:

      •  Location on  ranking list
      •  Melting point
      •  Boiling point
      *  Ambient vapor pressure
      •  Heat of combustion
      «  Analytical requirements
      •  Commercial availability  in large quantities
      •  Toxicity
      «  Relevance of the chemical to actual past spill/clean-ups  and contaminated
         soils

    Based on these criteria, PCP was  selected as  the  trial burn Appendix  VIII
    constituent/principal organic  hazardous constituent (POHC).  Table  5  summarizes
    physical property data relative to waste analysis  and gives an approximate  pre-
    liminary composition of  the PCP/sand mixture  that  will be  used during the  trial
    burn.

    The PCP will be fed to the mobile incinerator  as  a mixture of  about 50%  by
    weight PCP and 50% sand.   The  sand is necessary  to reduce  refractory  damage
    caused by pools of molten  PCP  burning on the RK's  refractory surface.

B.  WASTE PREPARATION

1.  PCBs in Soil (Artificial Mixture)
    When a chemical spill occurs on a soil, two adsorption processes  become  impor-
    tant.  The first  is true adsorption where the  contaminant  actually  is  adsorbed
    by the organic and inorganic matter in the soil.   Sometimes  this  component  has
    been called the "soil-bound" fraction.  The organic matter offers a matrix  in
    which the contaminant molecules are physically captured.   The  inorganic  com-
    ponents  provide surfaces for adsorption.  The  second  process normally  included

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                                   III-3
             Table 5.  Pentachlorophenol Physical Properties
Structure                                      C Cl OH
Molecular weight                               266.5
Heat of combustion  (Btu/lb)                    3760
Melting point  (°C)                             188
Boiling point  (°C)                             310
                                                       -4
Vapor pressure @ 20°C  (mm Hg)                  1.1 x 10
Chlorine  (wt %)                                66.6
Approximate Trial Burn Composition:
                          wt. %
     Carbon                13.5
     Hydrogen               0.2
     Oxyg en                 3.0
     Chlorine              33.3
     Water                 10.0
     Ash (sand)            40.0
                          100.0
     Btu/lb               1,880

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                                  III-4

as soil adsorption  is  in  reality  the  holding of the bulk contaminant phase be-
tween soil particles.   Although  this  effect is  normally considered together with
the adsorption  component,  it is  in  reality  an adsorption process and will be
called such  in  this plan.

Since little chemical  energy is  involved  in the adsorption compenent,  this
material  is  relatively easily removed from  soil and would rapidly volatilize and
be combusted in an  incinerator.   However, the soil-bound component is  held by
powerful  bonding forces and  the  rates of  desorption of  this soil-bound fraction
in an incinerator would be expected to be slower than the adsorbed fraction.

A soil preparation  procedure is presented that  focuses  on maximizing the  organic
and inorganic adsorption  process  so as to more  closely  simulate  actual
"weathered"  contaminated  soil.  This  procedure  is  comprised of a preclassifica-
tion step, a PCS addition step, and a storage and  aging step.  These procedures
are as follows:

a.   Preclassification — The existing EPA  water knife  unit will be  used  to
     preclassify the soil.   The soil  will be  fed into the unit and broken up  by
     the water knife action.   The slurry  produced  will   be allowed to  settle  and
     then spread under a  rain cover to air  dry.  Since  clean soil will be used
     for  this test, the soil  fractions  rejected from the  water knife and  the
     wash water  will be discarded in  a conventional  fashion.

b.   PCS Addition — Arochlor 1260  will be  dissolved in a methylene  chloride/
     isopropanol  mixture.   This mixture will  be fomulated so as  to minimize any
     flammability hazards.   This mixture  will be sprayed  onto the soil while
     undergoing  mixing in  a  double  arm sigma  type  mixer.   The dry soil will be
     weighed before addition  to the mixer and the  solvent will be added in quan-
     tities so as to achieve  40 to  45  mg/kg of  total PCBs  in the  soil.  The
     mixer will be operated  for sufficient  time to assure full mixing.  The mixer
     will be equipped  with a  steam  jacket and a pressure  cover and the solvent
     will be evaporated from  the soil while the soil remains in  the  mixer.  The
     solvent will be recovered with a water cooled condenser and  reused to

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                                       III-5

         dissolve  more  PCBs  for  subsequent batches.   Solvent recovery will also
         reduce  the  air pollution  impact of an organic solvent.

    c-   Storage-Aging  — The  solvent-dry soil will  be transferred manually into
         sealed  55-gallon drums  for  dry  storage.   These drums will be allowed to set
         for several months, thus  allowing the adsorption process to approach
         equilibrium.

    d.   Sampling-Analytical —  Several  soil  samples  per drum will be obtained and
         composited.  This composite sample will  be  split with a suitable solvent,
         and analyzed for PCBs  (see  Section III-D).   Analytically it may be
         necessary to use a soil digestion process for the PCBs  in soil  in order to
         quantitatively determine  PCBs since  the  soil-bound PCBs may not quan-
         titatively  extract from the soil.

    e.   Process Development —  All  of the above  steps will be tested in a small-
         scale laboratory program  to determine the optimal process conditions  and
         the effectivenes  of the approach.  After  development,  those specific  proce-
         dures will  be  used for  soil preparation.

2.  Actual PCB Spill  Clean-up Soil
    If an actual PCB  spill clean-up  contaminated  soil can be located,  the soil will
    need to be shipped  to Edison and/or  the Kin-Buc site where it will need to be
    stored and analyzed. The soil, if shipped  in  bulk,  will be analyzed,  placed in
    drums,  and sealed until the  Kin-Buc  trial  burn.

3.  PGP/Sand Mixture
    The PCP used for  the  trial burns will  be commercial grade  PCP manufactured
    either  by Vulcan Chemicals or Reichold  Chemical Company.   The sand will be ana-
    lyzed and certified as clean sand without  identifiable levels of PCP.

    The PCP will be purchased in drums,  analyzed, mixed with the sand, and stored in
    sealed  drums until the Kin-Buc trial burn.  The PCP and sand mixture  will  be
    metered into the ram feed hopper and fed to the incinerator.   During  the ram

-------
                                       III-6
    feed hopper  loading,  grab samples  will be taken,  composited,  and analyzed for
    PGP.
C.  SOLIDS HANDLING AND  FEED

1.  PCB Contaminated  Soil
    The PCB  contaminated soil  will  be  loaded from drums to the ram feed hopper
    either by a  vehicle  with drum handling capability or by a drum unloading mecha'
    nism which will be part of the  mobile  incinerator solids handling system.
    Fugitive dust will be  controlled by  a  cover/seal on the hopper and negative
    pressure in  the hopper being  vented  into the  RK.

2.  PCP/Sand Mixture
    The PCP  and  sand  mixture will also be  loaded  from drums to the ram feed hopper
    either by a  vehicle  with drum handling capability or by a drum unloading mecha-
    nism.  Fugitive dust will  be  handled in the same  way as discussion for  the PCB
    contaminated soil.

D.  SAMPLING ANALYSIS AND  MONITORING PROCEDURES

1.  Sampling Locations

a.  Stack Sampling Location  — During the  trial burn  the gaseous  and  particulate
    emissions produced by  the  combustion process  (flue  gas  and stack  gas) will
    be monitored at three  locations.  Two  of  these  locations  are  primary
    sampling locations to  measure incinerator emissions.  The  remaining location
    is to be used to provide a backup oxygen  monitoring station for gaseous
    emissions.   The primary  locations are  located on  the quench elbow duct,
    before gas  cooling,   and  on the mobile  incinerator stack  (see  Fig.  6).   The
    quench elbow location will be used to  continuously  monitor the  combustion
    gases leaving the SCC.    The actual sampling point will  be  positioned in  the
    center of the exhaust  duct that leaves  the SCC  immediately upstream of  the
    spray nozzles.   The concentrations of CO, C02,  and  O2 are  monitored at  this
    location as it allows for their determination from  a point that is unaf-

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                                    III-7
 4" Pore for
Combustion Gas
    1/4" Pore cor
  Concinuous Oxygen
       Sensor
                                              Discharge
                                            30 fc. Above
                                            Ground Level
                                     REFLO DUCT
                                                           \
  5-3" Pores for
Modified Method 5
    Samp ling
                                                                        4" Pore for
                                                                      Concinuous Stack
                                                                         Monitor
    Silencer
                                                                     DIESEL
                                                                    I.D.  FAN
                                                                     DRIVE
                                          Fig.  6

                                STACK GAS SAMPLING LOCATIOfS

-------
                                      III-8

    fected by air infiltration  or  interactions  with alkaline scrubbing solu-
    tions.  Therefore,  the  results  obtained  for these three gases at this point
    are expected to be  more representative of  the actual gas composition that
    exists within the SCC.   The SCC combustion  gases are withdrawn from the
    center of the quench  elbow  duct immediately prior to gas quenching through a
    1/2 in. ceramic probe.

    The second primary  gaseous  and  particulate  specie sampling location is
    located on the upper  section of the  stack  ducting.   There are sample ports
    for contnuous monitoring of emissions  (NO  ,  S00, and total hydrocarbon) and
                                             X     £•
    for specialized stack sampling  for particulate,  HC1, and POHCs.   One four-
    in. port will be provided for  the continuous monitoring of combustion gases
    such as NO . SO.,, and total hydrocarbon.   This port is located 24-in.  down-
              X    ^£
    stream from the stack silencer  section.  The design of the sample port and
    sampling unit is identical  to  the combustion gas samples located on the
    quench elbow duct.  The samplers are described in detail in Section II-I.
    The other sampling  location on  the stack consists of five 3-in.  connections
    mounted on a single face stack  duct.  The  connections are spaced to allow
    sampling for particulate matter in accordance with EPA Methods 1 and 1-5
    protocols.  The MM5 equipment will be used  to measure particulate and orga-
    nic emission rate using the methods  described in Section III.D.3.  The cen-
    terline of these sample ports  is 72-in.  downstream of the stack  silencer.

    There are two additional gas sampling locations  on the mobile incinerator.
    The first of these  points is located on  the exit duct from the SCC.   This is
    a  1/4-in. connection  for withdrawing a continuous gas sample which is chan-
    neled to the backup oxygen  monitor.

b.  Waste Feed Sample Location  — Both the PCB  contaminated soil and the
    PGP/sand waste mixtures will be fed  to the  ram feed hopper out of steel
    drums.  Before emptying a drum  of PCB/soil  or PCP/sand to the hopper, a
    sample will be taken  from each  drum  fed  during a run and composited.  The
    run composites will be  analyzed using the procedures discussed in
    Section III.D.3.

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                                       III-9

c*   Scrubber Water Sample Location — Combined scrubber,  CHEAP, and quench
     effluents will be grab sampled on an hourly basis during each run.  A com-
     posite  will be made from each 12 hour run and andlyzed according to the pro-
     cedures discussed in Section III.D.3.  The sample location will be located
     in the  wastewater purge stream line.

d.   Ash Sampling Location — Ash from the RK ash discharge will be collected in
     a  bulk  container located between trailer 1 and 2 (see Fig. 1) at the back
     end of  the RK.   When cool,  the ash will be sampled and analyzed according to
     the analysis procedures discussed in Section III.D.3.

e.   CHEAF Ash Sampling Location — Ash captured by the CHEAF fiberglass mat will
     be  collected in drums and sampled after each run.

2.   Sampling Procedures

a.   Waste Feeds  — Each drum of PCB contaminated soil fed to the  incinerator
     will be  sampled using acceptable techniques from SW-846 such  as a trier,  a
     thief,  or  an auger.  The actual sampling device will have to be determined at
     a  later  date when the type  of soil to be incinerated  has been identified.
     The sampling plan will also be determined at a later  date when it has  been
     determined whether artificially contaminated or actual PCB contaminated soil
     will be  incinerated.   The sampling plan  will be based on sampling strategies
     discussed  in Section 1  of the 2nd Edition of SW-846.

     Each drum  of PCP and sand fed to the  incinerator will be sampled  using a
     trier or  a thief as discussed in SW-846.   The sampling device  and sampling
     plan will  be determined at  a later date.

b.   scrubber Water  and Quench Water  — Grab  samples will  be  taken  every  60 min.
     during  each  test run from the purge line  to the  sewer.   One composite
     sample will  be  made for each test run.   Two grab samples  (blanks)  will be
     taken 30 min.  apart and composited before  the start of  each test  run.
     Samples °f t^ie  influeivt process  (makeup) water  will be  taken before  and

-------
                                       111-10

    after each test  run  and  composites.   The composites will be analyzed pri-
    marily for Arochlor  1260 or  PCP  concentrations.

c.  Stack Gas  — A sample will be  taken  during each  test run with an inert
    sample probe, using  the  proper EPA method for  each  parameter,  at a sample
    port in  the incinerator  stack.   Parameters to  be measured are CC>2, ®2 an^
    HC1.  Particulate  sampling and stack  flue gas  flow  measurements will also be
    performed.  A modified EPA Method  5  (MM5) sampling  train will be employed
    for the  collection of stack  gas  samples  to be  analyzed for Arochlor 1260 or
    PCP content.  Table  6 indicates  the  stack gas  sampling schedule for the
    various  parameters of interest.

    Sampling locations will  meet acceptable  standards for  distance from duct
    bends.   Steady state operating conditions will be maintained for the
    required duration  (approximately 3 hr) during  each  test run while the stack
    gas samples and  flow measurements  are taken.

d.  Ash Sampling —  After cooling, the ash from each run will be sampled with a
    thief or trier from  the  bulk ash collection container.   The sampling device
    and sampling plan  will be determined at  a later  date.

e.  CHEAP Sampling —  CHEAF  mat  samples will  be taken from the  used mats
    collected from each  run.  The  sampling plan will be determined at a later
    date.

3.  Analytical Procedures
    During the trial burn,  the following sampling  and analytical procedures
    which are summarized in  Table  7,  will be  used.

a.  Arochlor 1260 — During  test 1, the soil,  diesel fuel,  makeup  water,  kiln
    ash,  purge water,  alkaline scrubber solutions, CHEAF filter ash,  and stack
    samples  will be analyzed for Arochlor 1260.

    Because  of the low level  (40-49yg/g) of Arochlor 1260  in the soil that will
    be used  in the test and  the predicted destructive efficiency (>99.99%),  the

-------
                           Table 6.  Summary of Trial Burn Sampling

                             and Analytical Methods for Stack Gas
Parameter
°2
co2
HC1

Particulates
Arochlor 1260
Pentachlorophenol
Sample Method
EPA 3
EPA 3
Impinger with
0.1N NaOH
EPA 5a
EPA 5
EPA 5
Time
Per Sample
30 min
30 min
15 min

2 hours
12 hours
12 hours
Analytical
Method
ORSAT
ORSAT
Ion-specific
electrode
EPA 5
ITAS SOP
EPA 8250
Samples
Per Run
4
4
4

1
3
3
EPA Method 5 includes measurement of stack gas temperature,  flow rate,  and moisture content.
                                                                                                              H
                                                                                                              H
                                                                                                              i

-------
                                          Table  7.    Scope  of Work  - Details of  Proposed  Sampling
                                                            and  Analysis for  Tests  1  and  2
Sample
Spiked soil
feed and PCP


Diesel fuel
Make-up water

Kiln asli

Purge water





Alkaline
scrubber
sol ution
C1IEAF

Stack sample

Sampling Method
and Frequency
One composite sample
per run (2 grabs)


One grab sample per
delivery, composite
sample for one
analysis per lot
One sample per stage

One sample per DRE test
(if any)

One composite sample
per DRE run

Daily composite
(1 hr grabs)
Weekly grabs
Weekly grabs
Weekly composite
One grab sample per batch
Composite grab sample
One sample per DUE run

Modified Method 5
One sample per DRE run
Number of Samples
Analyzed for
Tests 1 and 2
6
6
6
2
2
1
1
3
3
3
3
15
2
2
2
2
3
3
3
3
Stack sample
                          (throe samples per  test)
                       U.S. EPA Method 5
                          (three samples per  test)
                       Gas bag, one per run
                                                                                              Analysis
Organic Cl,  density

Heat value,  ash,  moisture

Arochlor 1260 or  PCP

Organic Cl

Density, ash, moisture, heat value

Presence of Arochlor  1260, PCP

Presence of Arochlor  1260

Presence of PCP

Presence of  PCP

Presence of Arochlor  1260

Presence of  Arochlor  1260

Presence of  PCP

Total organic carbon, pH, temperature


Total suspended solids

Total dissolved solids

PCBs, PCP

PCBs, PCP



Presence of  Arochlor  12GO

Presence of  PCP

Arochlor 1260 emission rate

PCP emission rate


HC1 emission rate**

Particulate  emission  rate
                                                                                 o2 ,  co2
                                                       Analytical Method	
                                                                                                                               Standard method (where  appropriate)

                                                                                                                               Standard method (where  appropriate)

                                                                                                                               GC/EC or GC/MS

                                                                                                                               Standard method (where  appropriate)

                                                                                                                               Standard method (where  appropriate)

                                                                                                                               Extraction, concentrate,  GC/EC or GC/MS
                                                                                                                               Extraction, concentrate,  GC/EC*

                                                                                                                               Extraction, concentrate,  GC/MS*

                                                                                                                               Extraction, concentrate,  GC/EC*

                                                                                                                               Extraction, concentrate,  GC/MS

                                                                                                                               Extraction, concentrate,  GC/EC*

                                                                                                                               Extraction, concentrate,  GC/MS

                                                                                                                               Standard methods  (where appropriate)
Extraction,  concentrate, GC/EC*

Extraction,  concentrate, GC/EC*



Extraction,  concentrate, GC/EC*

Extraction,  concentrate, GC/MS

Extraction,  concentrate, GC/EC*

Extraction,  concentrate, GC/MS


Scrubbing,  Standard Method 325.3

EPA Partiuulate Method 5



ORSAT
                                         H
                                         H
                                         H
 *Positive  results confirmed by GC/MS -
**PCB runs  will not be analyzed for IIC1  since IICl emission rate
  will be  <4  Ib/hr

-------
                                       111-13

    only practical detection  device  for  the  quantitation of  Arochlor 1260 is the
    electron capture  detectors which are more  sensitive  than the GC/MS.

    Samples and extracts  representing discrete MM5  sampling  train components
    will be analyzed  by GC/EC followed by compositing  them together and  then
    further concentrating the extracts.  The  final extracts will  be re-analyzed
    by GC/EC.  If the resulting concentration  levels are adequate,  the con-
    centrated composite extracts will be analyzed by GC/MS using the selected
    ion monitoring made for some of  the  discrete Arochlor 1260 isomers.

    While aqueous samples will be extracted  with solvent in  a normal fashion,
    the soil, the MM5 sorbent traps  and  particulates will be extracted by an
    ultrasonic assisted desorption procedure using  hexane.

    Complete details  of the analysis  are  described  in  the ITAS Standard
    Operating Procedure for Analysis  of  PCBs (see Appendix 1 of  Appendix  A).

b.  Pentachlorophenol —  The  analysis  for pentachlorophenol  in the  test  2
    samples will be performed using Method 8250, "GC/MS  Method for  Semivolatile
    Organics:  Packed Column  Technique,"  Test  Methods  for Evaluating Solid
    Waste, July 1982,  SW-846, Second  Edition.

c.  Heat of Combustion — This parameter  will  be determined  on the  soil and
    diesel fuel by ASTM Methods D240,  D2015, or D3826.

d.  Ash Content — The ash content of  the soil and  diesel fuel will  be deter-
    mined by ASTM Methods D482 or D3174.

e.  Water Content —  The water content of the  soil  and diesel fuel will be
    determined by ASTM Methods D95,  D1796, or  D3173.

f.  Total Organic Carbon,  pH  Temperature  —  Total suspended  and  dissolved
    solids.

-------
                                       111-14

    These parameters will be  determined in the purge water according to the
    methods given in Table  7.

g.  02/C02 — These parameters will  be determined by EPA Method 3 on integrated
    bag samples of the stack  flue  gas  samples  taken from sampling train or
    exhaust of the EPA Method 5.

h.  HC1 — Using modified EPA Method 13,  HC1 will be determined on stack flue
    gas samples collected for each test run.   This procedure uses NaOH impinger
    solution and chloride selective  ion-specific  electrode for analyses.

i.  Particulate — The stack  flue  gas  samples  will be analyzed for particulates
    using EPA Method 5, as  described in Federal Register,  42 (160);  41776-41782,
    August 1977.

    The ASTM, Standard methods and EPA methods  cited above are referenced from:

      *  Annual ASTM Standards, Parts  23,  24,  25,  26,  29,  30,  and 31.   American
         Society for Testing  and Materials,  Philadelphia,  PA (1981).
      *  Standard Methods for the  Examination  of  Water and Wastewater  15th
         Edition, APHA-AWWA-^?PCF,  Washington,  DC'TfOSOj.     '
      •  Standards of Performance  for  New  Stationary Sources.  A Compilation as
         of October 1, 1977,  EPA-340/1-77-015,  NoVember 1977,"u.S.  Environmental
         Protection Agency.
      «  Test Methods for Evaluating Solid Wastes  Physical/Chemical  Methods,
         EPA-846, 2nd Edition, July  1 982",  USEPA Off ice" of  Water Imd" ~Was te~ ~
         Management.
4.  Monitoring
    During the incineration of the PCB/soil  waste  and the  PGP/sand waste,  the stack
    and SCC flue gases will be monitored for the  important gaseous components:   02,
    CO2,  CO,  NOX,  S02, and THC.  The analyzer  section of  the monitoring equipment
    operates  in conjunction with the microprocessor to direct  sample gases to
    (1) the thermal conductivity detector  GC for  analysis  of C02,  O2,  and SO2;
    (2) through a methanizer  to a  flame  ionization detector GC for analysis of CO;
    (3) the flame ionization  detector  GC for analysis  of  THC (compared to a methane

-------
                                      111-15
    standard);  and  (4)  a  chemiluminescent detector for analysis of NOX-   The
    microprocessor  generates  printouts  of all analytical results.,  A detailed
    description  of  the  gas  analysis  monitoring system can be found in Section II.I
    of the Trial Burn Plan.

    Summaries of the monitoring equipment used are given in Tables 8 through 13.

E.  DETAILED TEST BURN  PROTOCOL
    There will  be six runs  made during  the solids  trial burn on two different
    wastes.  Three  identical  runs  will  be made with the PCS contaminated soil,  and
    three identical runs  with the  PGP/sand mixture.   Table 14 presents the conditions
    for each of  the two tests and  six runs.

    The objectives  of the first test (Test 1)  is to show that the  mobile incinerator
    can effectively incinerate  organically contaminated soil.   The  second objective
    of the trial burn (Test 2)  is  to demonstrate that the  mobile incinerator can
    effectively  incinerate  a  solid hazardous  organic  chemical (PGP)  at a high rate
    and thereby  obtain  a  flexible  RCRA  permit for  the incineration  of  solid hazar-
    dous wastes.

1.  Trial Burn Operating  Condition
    As can be seen  from Table 14,  only  one set of  conditions  will  be used for each
    test.   A description  of the  two  tests  is  as follows.

a.  PCB/Soil —  The PCB/soil  mixture will  be  incinerated in the RK  at  about 1600°F.
    The combustion  gas  from the  RK will enter  the  SCG and  be  subjected to a tem-
    perature of  about 2200°F  and have a SCC combustion gas flowrate  of about
    14,500 acfm.  The temperatures and  combustion  gas flowrate will  be controlled  as
    closely as possible,  but  may vary somewhat from run to run because of normal
    operational  considerations.

    The actual feed rate  of contaminated  soil  used during  runs  1-1,  1-2,  and 1-3 may
    differ from  the 2000  lb/hr  given in Table  14 because of  the soil moisture con-
    tent.   The actual soil feed  rate will  be  determined during  the  Phase I testing

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                                    111-16
                                   Table 8


                         ANALYSIS METHOD FOR OXYGEN

     This method will be used for quantitative determination of oxygen in
the SCC flue gas for all nine trial burn tests. The Q£ results will be
used for calculation of combustion efficiency for the mobile incinerator.
Basic Method:                 Continuous Monitor System

Matrix                        Cool, dry, filtered stack gas (see  •
                              Section III C).

Apparatus:                    Bendix Model 9120 gas chromatograph/thermal
                              conductivity detector

Gas chromatographic           Column: 1/8" x 8' molecular sieve 5A
  Conditions:
                              Carrier Gas:  helium

                              Injector:  Hastelloy C sampling
                                         valve @ 11QOC, 40/jL
                                         sample loop

                              Oven:  110 °c isothermal

Calibration  Gas:              Zero gas:  Nitrogen
                              Span gas:  8% 02 in nitrogen

Analysis Range:               0-10% 02

Anticipated  Detection         0.10% 02
   Limit:

Anticipated  Accuracy:         ±0.10% 02  (or ± 1% of range)

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                                 111-17



                                 Table 9


                     ANALYSIS METHOD FOR  CARBON DIOXIDE
     This method will be usad for quantitative determination of carbon
dioxide in the stack gas for all nine trial burn tests. The C02 results
will be used for calculation of combustion efficiency for the mobile
incinerator.
Basic Method:                 Continuous Monitor System

Matrix:                       Cool, dry, filtered stack gas (see
                              Section III C)

Apparatus:                    Bendix Model 9120 gas chromatograph/
                              thermal conductivity detector

Gas Chromatographic           Column:  1/8" x 4' Poropak Q 50/80 and
Conditions:                            1/8" x 8' Poropak Q 50/80

                              Carrier Gas:  helium

                              Injector:  Haste Hoy C sampling
                                         valve @ 110 OC,
                                         40 juL sample loop

                              Oven:  110 OC isothermal

Calibration Gas:              Zero gas:,  nitrogen
                              Span gas:  10% C02 in nitrogen

Analysis Range:               0-10% C02

Anticipated Detection          0.1%
   Limit:

Anticipated Accuracy:         ± 0.1% C02 (or ± }% Of range)

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                                111-18


                               Table 10

                    ANALYSIS METHOD FOR CARBON MONOXIDE

    This method will be used for quantitative determination of carbon
monoxide in the SCC flue gas for all nine trial burn tests.  The CO
results will be used for calculation of combustion efficiency for the
mobile incinerator.


Basic Method:                    Continuous Monitor System
                                                             «
Matrix:                          Cool, dry, filtered SCC flue gas
                                 (see Section III C)

Aparatus:                        Bendix Model 9220 methanizer coupled to
                                 a gas chromatograph/flame ionization
                                 detector.

Gas Chromatographic              Column:  1/8" x 6' Poropak Q 50/80 and
                                          1/8" x 12" Poropak Q 50/80

Conditions:                      Carrier Gas:  Hydrogen

                                 Injector.-"'Hastelloy C sampling valve
                                            0 66°C,
                                            0.25 mL sample loop

                                 Oven:  66°C isothermal

Calibration Gas:                 Zero Gas:  nitrogen
                                 Span Gas: 100 ppm CO in nitrogen

Analysis Range:                  0 - 200 ppm CO

Anticipated Accuracy:            ± 2 ppm CO (or ± 1%  of range)

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                               111-19



                               Table 11

                  ANALYSES METHOD FOR OXIDES OF NITROGEN

    This method will be used for qualitative determination of oxides of
nitrogen in the stack gas for.all nine trial burn tests.


Basic Method:                    Continuous Monitor System

Matrix:                          Cool, dry, filtered stack gas..
                                 (see Section III C)

Apparatus:                       Bendix Model 8102 chemiluminescent
                                 NO - NOX analyzer

Calibration Gas:                 Zero Gas:  nitrogen
                                 Span Gas:  ISOppm NOX  in nitrogen

Anticipated Detection            1 ppm NOX
  Limit:

Analyses Range:                  1 - 500 ppm NOX

Anticipated Accuracy:            -± 5 ppm NOX (or ± 1% of range)

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                                   111-20


                                 Table  12

                     ANALYSIS METHOD FOR SULFUR DIOXIDE

     This method will be used for quantitative determination of sulfur
dioxide in the stack gas for all 9 trial burn tests.


Basic Method:                 Continious Monitor System

Matrix:                       Cool, dry, filtered stack gas (see
                              Section III C)

Apparatus:                    Bendix Model  9120 gas chromatograph/thermal
                              conductivity detector.

Gas Chromatographic           Column:  1/8" x 4' Poropak T/Poropak Q 50/80 and
 Conditions:                           1/8" x 2' Poropak T 50/80

                              Carrier Gas:   Helium

                              Injector:  Hastelloy C sampling
                                         Valve @ 110 °C
                                         2 mL sample loop

                              Oven:   110 QC Isothermal

Calibration Gas:              Zero gas:  Nitrogen
                              Span gas:   2000 ppm S0£ in nitrogen

Analysis Range:               0-2000 ppm S02

Anticipated Detection         20 ppm S02
    Limit:

Anticipated Accuracy:         ±20 ppm S02 (or ± 1% of range)

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                                 111-21



                                 Table 13

                   ANALYSIS METHOD FOR TOTAL HYDROCARBON

    This method will  be used for relative determination of total
hydrocarbons (THC) in the stack gas for all  nine trial  burn tests.   The
THC results will be used as an indirect indication of combustion
efficiency for the mobile incinerator.


Basic Method:                    Continuous  Monitor System

Matrix                           Cool, dry,  filtered stack gas
                                 (see Section III C)

Apparatus:                       Bendix Model 9220 gas  chromatograph/flame
                                 ionization  detector.

Gas-Chromatographic           '   Column:  1/8" x 4' Poropak Q 50/80
  Conditions:
                                 Carrier Gas:  Nitrogen

                                 Injector: ^-Hastelloy C sampling
                                            valve @ 66QC,
                                            40 ,uL sample loop

                                 Oven:  66°C isothermal

Calibration Gas:                 Zero Gas:  nitrogen
                                 Span Gas:  100 ppm CH4 in nitrogen

Analysis Range:                  0 - 200 ppm THC

Anticipated Accuracy:            ± 2 ppm THC (or ± 1% of Range)

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                                         Table 14. Trial Burn Operating Conditions
                                    Waste                                              SCC     SCC  Gas
                                    Peed      Phys.  Heat Value   chlorine   RK  Temp.   Temp.   Velocity  Aux.  Fuel   SCC
Test  Runs   Waste Feed    POHCs    (Ib/hr)    Form     (Btu/lb)   . .  {%).  ..	(°F)	(°F)    (ACFM)     Range RK  (MMBtuh)

 1   1,2,3   Soil with     PCBs     2000      Solid    ^0            ^0       1600      2200    14,500     4.5-5.0   4.5-5.0
               <50 ppm
               PCB

 2   1,2,3   PCP with      PCP       500      Solid    :1880          33.3     1600      2200    14,500     3.5-4.0   5.-5.5
               sand
                                                                                                                         H
                                                                                                                         H

-------
                                       111-23

    with clean soil which  is  discussed in Section I.   It is  expected that the active
    soil feed rate for  the  trial  burn  will be  somewhere  between 1500 and 2500 Ib/hr.

    Because of the low  heat value of the  soil,  auxiliary fuel will be used during
    the PCB/soil trial  burn.   It  is expected that about  5 MM Btuh will be needed in
    the RK and about  5  MM  Btuh in the  SCC.  The acutal values needed will depend on
    the soil moisture content and will be in the 4.5  to  5.5  MM Btuh range.

b.  PGP/Sand — The pentachlorophenol  and sand  mixture will  be incinerated in the RK
    at about 1600°F.  The  hot combustion  gas from the RK will enter the SCC and be
    subjected to a temperature of about 2200°F  and have  a SCC combustion gas flow
    rate of about 14,500 acfm.  The temperatures  and  combustion gas flow rate will
    be controlled as closely  as possible,  but may vary somewhat from run to run
    because of normal operational considerations.

2.  General Trial Burn  Considerations
    In preparation for  the  trial  burn,   auxiliary  fuel (diesel oil)  will be  used as
    necessary to raise  the  combustion  system to  the desired  test run temperatures,
    assuming the incineration  system has  been operated at reduced fire  conditions
    between test runs.  Recycle water  sumps will  be flushed  clean within practical
    limits.  The solid waste will be received,  and stored in a designated
    receiving/storage area  at  the Kin-Buc  site.

    Each test run will require approximately 12 hours  to  complete.   This  means  that
    approximately six days will be required for  the trial burn  program,  assuming
    smooth operation of all test  equipment and that all  6 runs  are  made.  A  typical
    test run will include the  following sequence  of events;

      •  Raise  temperature of RK  and SCC  to desired levels using auxiliary  fuel
         (approximately 2 hr)
      •  Check  sampling and analytical equipment;  standardize where  necessary
      «  Adjust gas  cleaning quench and scrubber water flows  to desired levels
         during this  time
      •  Start  appropriate scrubber water  feed pumps  through  appropriate  recycle
         loops

-------
                                       111-24

      •  After the system is up  to  temperature  and  lined  out,  conduct POHC blank
         sampling for scrubber water  and  flue gas  (approximately 1  hr)
      •  After blank sampling is  completed, start waste feed  to the ram hopper and
         start ram feed mechanism;  fine-tune waste  feed rates  and diesel oil
         atomization by observation of  the  flame characteristics;  monitor combustion
         air blower, quench, recycle  water  system,  and pH control;  set  system on
         automatic temperature control  and  allow for  steady-state conditions
         (approximately 1 hr)
      •  After achieving steady-state conditions, conduct sampling and  analytical
         tests over an appropriate  time period
      •  After completing the test  run, empty ram feed and hopper,  take final
         readings; allow combustion system  to cool  down to low fire conditions
         (approximately 2 hr)
      «  Clean up sampling and analytical equipment for next test run during this
         period
      «  Clean out recycle water  sumps  in preparation for next run;  prepare  samples
         for transport to laboratory; button down equipment for  overnight storage
      •  Maintain system on auxiliary fuel  at low fire overnight

F.  EMISSION CONTROL EQUIPMENT DESCRIPTION  AND  OPERATING  CONDITIONS

1.  Description
    As illustrated in Fig. 7, a skid-mounted quench surge  sump  and  recycle pump  is
    located on the ground between Trailers  2 and 3.   The  quench  system  is  the  ini-
    tial stage of the air pollution control (APC) system  in that the  cooling and
    saturation of the gases preconditions them  for  the rest of  the  APC  system.
    Through pH adjustment with an alkalne solution, the excess water  in  the  quench
    removes part of the acid gases  in the flue  gas.   If the quench water pH  drops
    below 7, alkaline solution is added to  the  quench sump from  auxiliary alkaline
    supply tanks.  Some particulate is also removed in the quench.

    Mounted on the third trailer are  the particulate  scrubber, mass  transfer
    scrubber,  induced-draft fan,  fan  drive engine,   flue gas stack,  instrument  air
    compressor and control panel.  The particulate  scrubber is a commercially
    available cleanable high efficiency air filter  (CHEAF) constructed of
    Inconel 625 for corrosion resistance.    It operates with a  25 to  30  in. w.c.

-------
                                             111-25
COMBUSTION CAS ANALYSIS
     (Oj CO. C02> -7     EMEflCENCY
                      /   VENT
                                         KEfl.0 OUCT
                               STACK GAS ANALYSIS
                               |TMC. NOj. SOj. Oj. CO. COjl
   QUENCH ELBOW SUMP:


   DUCT TO CHEAP:
   EMERGENCY VENT:

   CLEANA8LE HIGH EFFICIENCY AIR
    FILTER:

   MX SCRUBBER:
   REFLO OUCT:
   INDUCED DRAFT FAN:


   DIESEL ID FAN DRIVE:


   STACK:
Inconel 625, 35 in. (91.5 cm) width X 72 in. (183 cm) length X
30 in. (76 cm) height
Inconel 625, 20.4 in. (52cm) ID

Inconel 625, mechanical operated, includes butterfly shutoff valve
Anderson 2000, Inconel 625, Wetted glass fiber filter pad with auto-
matic controls to maintain 30 in. (76 cm) WC AP, pad is 100 ft (30.5
m) roll by 4 ft (1.2 m) width, moved by Inconel 625 chain mat
Ceilcote cross-flow irrigated scrubber filled with 2 in. (5 cm) plastic
packing, 7.8 ft (2.4 m) height X 6.5 ft (2 m) width X 29
ft (8.9 m) length,  FRP

304 SS, 12 in. (30.5 cm) dia.

347 SS housing, Inconel 625 shaft and impeller, 36 in. (91.5 cm) dia.
rotor

155 hp, (1 16 kW)  Allis-Chalmers 6-cylinder turbocharge diesel
engine, 6491 series, 300 in.'  (0.0005 m3) displacement

Two sections
   9 ft (2.7 m) noise attenuator, carbon steel
    10 ft (3.1 m) section, 304 SS
                   Fig.  7.   Air  Pollution  Control  Equipment

-------
                                       111-26

    pressure  differential across a wetted fiberglass filter mat to remove submicron
    particulates  from the flue gases.

    The  mass  transfer scrubber is a horizontal,  crossflow irrigated,  packed bed
    absorber  tower  appropriately designed and reinforced for this specific mobile
                                             2
    application.  The packed bed has a 25 ft  cross-section and is over 8 ft long,
    with the  last 9 in.  of packing acting as a demister.   The scrubbing media is
    kept alkaline by automatic pH adjustment from an off-trailer alkaline solution
    feed system.  Sumps  for the CHEAP and the scrubber are located in the bottom of
    the  packed  scrubber.   Recycle water pumps are utilized for both scrubber units.

    The  induced-draft fan is driven by a 155 hp diesel engine and operates at a
    nominal speed of 3,350 rpm in order to maintain a negative pressure of
    42 in. w.c.   The fan is a single stage,  heavy duty industrial unit with a
    347  stainless steel  housing and an Inconel 625 shaft and 36 in.  diameter rotor.

    The  exhaust stack is mounted on top of the fan and is hinged so that it will lay
    down in a horizontal position during transport.   Part of the stack is a sound
    attenuator  designed  to reduce the  fan discharge sound pressure levels to 85 db
    at 5 ft from  the stack outlet.   The overall  height of the stack  is 30 ft above
    ground level.   Also  mounted on the third trailer is the control panel used  to
    operate all the equipment on the trailer.   The air compressor on  the trailer
    provides instrument  air for all three trailers.   Figure 8 is a dimensional
    sketch of the APG system.

2.  Operating Conditions
    Table 15 summarizes  the expected operating condition  ranges for  the mobile
    incinerator-air pollution equipment.   Actual trial burn values will depend  on
    the waste being incinerated and will be  within these  ranges.

G.  PROCEDURES  DURING EQUIPMENT MALFUNCTION

1.  Waste Feed  Shutoff and Incinerator Shutdown
    In the event  of an equipment malfunction a system of  interlocks will trigger

-------
COMBUSTION GAS ANALYSIS
    (Oj. CO. COj)
                                                        STACK GAS ANALYSIS
                                                        (THC. NOX, SO2. Oj. CO, C02)
                        AIR POLLUTION CONTROL
                                                                                                    H
                                                                                                    H
                                                                                                    I
                                                                                                    NJ
                Fig. 8.   Dimensioned Sketch  of APC Equipment

-------
                                      111-28
     Table 15. Operating Condition  Ranges Air Pollution Control Equipment










	Water  Flow  (gpm)	AP  (in.  W.C.)	pH




Quench Elbow               80-90                        -                   7-8.5





CHEAF                      15-20                      25-30




MX Scrubber               120-130                      8-12                8-8.5

-------
                                      111-29

    rapid shutdown  of  the  waste  feed and/or the thermal oxidation system if abnormal
    values of key parameters  are measured.   High combustion flue gas  temperatures,
    caused by loss  of  water,  low scrubber water flows,  loss of power,  loss of ID
    fan, etc., result  in waste feed cut-off and the extinguishing of  all burner
    nozzle flames.   The details  of  waste feed cut-off system shutdown are discussed
    in Sections III-H  and  III-M.

    During the feeding of  solid  wastes,  a malfunction will cause the  ram solids feed
    mechanism to stop.  If possible,  however,  the diesel fuel burners  in the RK and
    SCC will stay on in order to assure  adequate destruction of the combustion gases
    generated by the solid wastes still  remaining in the RK.

2.  Emission Control
    During an equipment malfunction the  SCC combustion gases  will either be routed
    to the APC equipment or to the  emergency  vent (see Section III-N).   The actual
    combustion gas  routing will  depend on the type of malfunction.

H.  TRIAL BURN INSPECTIONS

1.  Spill Inspection Plan
    This general spill inspection plan for  the  USEPA mobile incinerator  system was
    developed to detect and respond in a systematic and timely manner  to potential
    equipment malfunctions, facility  deterioration,  operator  errors, and waste
    discharges that  might  release hazardous waste constituents to the  environment or
    threaten human health.  It was  specifically designed to meet the requirements
    set forth in Standards for Owners and Operators  of  Hazardous Waste Treatment,
    Storage,  and Disposal  Facilities, 40 CFR  Section 264.15,  and related sections;
    and the Oil Spill Prevention  Regulations,  40 CFR Part 112.

    This plan will be reviewed,   and amended annually or if  necessary,  for any  of the
    following reasons;   (1) if there  is  a significant facility revision,  (2)  if  a
    significant incident occurs  and the  condition causing the  incident was  not ade-
    quately detected and responded  to, or (3) to comply with  future requirements,
    changes,  or additions  to  the  regulations.

-------
                                      111-30

    As a part of the Spill  Inspection  Plan,  copies  of  the  construction  plans,
    prestartup inspection procedures,  housekeeping  procedures,  safety operations
    manual, and inspection  procedures  for  the facility are kept with the  incinera-
    tion system whenever it is  mobilized and operated  in the  field.  In addition,
    the standard operating  procedures  for  the facility require  that the process
    operators routinely walk  through their operating areas (versus operating only
    from the control panel)  to  visually observe/monitor and record the  condition of
    all equipment and the facility.  Further, the facility will have an active pre-
    ventive maintenance program in which schedules  will be established  for  the
    routine maintenance of  equipment requiring such attention.  A key part  of this
    program will be the record  keeping on  equipment items  and systems.  These
    records cover such information as  purchase date, manufacturer, specifications,
    test results, past maintenance and repair history,  and required maintenance
    schedule.  Although the  above programs  are not  incorporated into this inspection
    plan, they complement and supplement this plan  to  provide a comprehensive pro-
    tection program.

2.   Inspection Organization
    Routine inspections will be performed  under the direction of the Research and
    Development (R&D) Group Leader by  supervisory personnel who have operational or
    equipment responsibilities  in the  area  inspected.

    The mobile incineration system will typically be set up and operated for periods
    of less than 90 days.  All  equipment will be inspected before the system is set
    up and when the system is dismantled after each operation.  At the  time inspec-
    tions are made,  written inspection forms will be filled out.  A copy of the
    completed inspection report will be sent to the project engineer and a  copy
    retained in the inspection  area operating log.  It is  the responsibility of the
    project engineer to maintain complete  records for  this inspection plan.  These
    records will be maintained  for three years.

    It is the responsibility of  the R&D Group Leader to initiate and follow up any
    response actions required by conditions  discovered in  an  inspection.  The pro-
    ject engineer is responsible for reviewing the  inspection reports and responses

-------
                                      111-31


    and taking any additional corrective actions required.  The R&D Group Leader

    will prepare a monthly summary report to the EERU Project Manager, covering such
    i terns as:


           •  Inspections completed
           •  Problem conditions found
           •  Responses completed
           »  Responses pending
           «  Recommendations


3.   Inspections

    Once each day during operation, the shift supervisor will inspect all safety and
    emergency equipment to ensure that all are operating properly.  All information

    will be entered into the operations record.  The shift supervisor will remedy

    any deterioration or malfunction of equipment or structures quickly enough to

    avoid environmental or human health hazards.  Where a hazard is imminent or has

    already occurred, remedial action will be taken immediately.


    At the beginning of each shift the shift supervisor will inspect the following
    areas:
    a.   Tank overfilling prevention equipment  (for example, waste feed cut-off
         systems and by-pass systems) - to ensure that it is in good working order;
         continuous monitoring by an operator shall be mandatory during times when
         process tanks are being filled;

    b.   Data gathered from monitoring equipment  (for example, pressure and tem-
         perature gauges) where present, at least once each operating shift to
         ensure that the equipment is being operated according to its design;

    c.   Monitoring equipment (for example, pressure and temperature gauges) used
         continuously during uncovered operation;

    d.   Tank waste level at least once each day to ensure compliance with N.J.A.C.
         7:26-10.5(c)2ii (NJDEP Hazardous Waste Facility Permit Requirements);

    e.   Condition of above-ground tanks to detect corrosion or leaking of fixtures,
         pipes, and seams;

    f.   Area immediately surrounding the pre-existing on-site waste storage areas
         (containers, valves,  conveyors, piping) to visually check for malfunctions,
         leaks, spills, and fugitive emissions.  It should be noted that before the
         mobilization of the treatment system, regional, state, and local emergency

-------
                                      111-32

         response personnel will have secured the waste storage areas, thus
         affording a safe working environment.


    At the close of the incinerator operation and before incineration dismantling,

    the shift supervisor will ensure that the equipment and site decontamination
    procedures are initiated.


4.   Corrective Actions

    The operator shall immediately notify the shift supervisor of any condition

    requiring corrective action.  The shift supervisor shall determine the correc-

    tive action to be taken and see that the work is immediately initiated and pro-

    perly carried out until completed.  The shift supervisor will issue a written

    order to the operator; when the work is completed the operator will date and

    sign the work order and return it to the shift supervisor.


    This corrective action will be dependent on the problems, but if a hazard is

    imminent or has already occurred, remedial action will be taken immediately.

    Some examples of conditions and corrective actions are:
         Condition

         Monitoring equipment
         malfunction

         Leaky valve
         Eroded dike
         Used or missing safety
         or firefighting equipment
Corrective Action

Immediate maintenance by
instrument technicians

Immediate maintenance by
maintenance man; initiate
work order to repair or
replace if required

Make temporary repairs,
initiate work order for
permanent repair

Replace from stock,
follow up on reason for
equipment condition and
correct
    Any drips, leaks, or spilled waste material shall be  cleaned up  immediately
    after detection or after repair.  Drip pans under the waste feed pumps and

-------
                                      111-33

    piping shall be vacuumed out immediately after a rain shower to prevent unne-
    cessary contamination of the rain water if a leak should occur subsequent to the
    rain fall.  Discharge of rain water will be supervised to ensure compliance with
    applicable water quality standards and to prevent a  "harmful" discharge as
    defined in 40 CFR, Part 110.

I.  TRIAL BURN RECORD KEEPING
    An operating log  (see Pigs.  9 through 11) will be filled out once each hour for
    all operations.  These logs will be a record of operating conditions and provide
    evidence that the operator has  checked and is aware  of the actual operating sta-
    tus of the system.  The time at which entries are made will be shown, as will
    the actual instrument reading for each variable.  If automatic shutdown occurs,
    the log will state the nature of the shutdown, the time it occurred, and the
    suspected cause.  This will  be  noted in the  "remarks" column along with any unu-
    sual conditions or situations such as spills or leaks.  The log will be dated
    and signed by the operator.  In addition, once each  shift the shift supervisor
    will inspect the facility for malfunctions and deterioration, operator errors,
    and discharges which may be  causing, or may  lead to:

      •  Discharge of hazardous  waste constituents to the environment
      o  A threat to human health

    The completed log sheets will be kept in a three-ring binder under  the control
    of the shift supervisor.  Once  each day the  shift supervisor will submit all
    inspection reports, graphs,  etc. to the R&D  Group Leader.   If it is  determined
    that a spill potential exists it will be brought to  the R&D Group Leader's
    attention immediately.

J.  TRIAL BURN SCHEDULE
    The current schedule for the trial burn portion of the Kin-Buc demonstration
    test is shown in Table 16.   Each test run is expected to  last 8 to  12 hours.  The
    maximum amount of PCB contaminated soil incinerated  will be about 72,000 pounds.
    This soil will contain a maximum of 3.6 pounds of PCBs.  The maximum amount of
    pentachlorophenol and sand incinerated will be about 18,000 pounds, with about
    9, 000 pounds being pentachlorophenol.

-------
                                                         Fig.  9

                                             ROTARY KILN AND SCC OPERATING LOG SHEET
                             TRIAL BURN TEST DATA - Collect at 15 Minute Intervals During Waste Feed
DATE:
SHIFT:
                                                                                       OPERATOR:
ITEM
Kiln Temperature (KILN-OG )
Kiln Oxygen (PANEL KILN-02)
Kiln Comb Air Flow (PANEL)
Kiln Comb Air Flow (ANNUBAR)
Kiln Ambient Air Temperature
Kiln Water Flow (KILN-H20)
Kiln Waste Oil Flow(KILN-WO)
SCC Temperature (SCC-OG)
l
SCC Oxygen (THERMOX SCC-02)
SCC Comb Air Flow (ANNUBAR)
BuTv\€r H Fue\ "Flooo (.Ot-pp)
fWner 3>Fw.«A "Plov*j (.133, -pr)
turner / F~ad F7oco(Gi -r>Fj
' Gu
-------
                                                             Fig.  10
                                        AIR POLLUTION CONTROL EQUIPMENT  OPERATING  LOG  SHEET
                                                            HOURLY LOG
DATE i
SHIFT:
OPERATORz
ITEM
Quench Sump Level (QUE-LC)
Quench Water Temp (QUE-PW)
Quench £20 Press DNST(QUE-PW)
Quench H2O Press UPST (QUE-PW)
Quenched Gas Temp
CHEAF Exit Temp
Quench Water Flow (QUEP-PW)
CHEAF Water Flow (CHFP-PW)
Filter Roll
CHEAF Water Temp (CHF-PW)
CHEAF Filter Differ (CHFD-OG)
CHEAF Outlet Press (CHFO-OG)
CHEAF Inlet Press (CHFI-OG)
CHEAF H20 Press DNST (CHF-PW)
CHEAF H20 Press UPST (CHF-PW)
Scrubber Water Temp (MX-PW)
CHEAF Sump Level (CHF-PW)
Scrubber Sump Level (MX-WL)
Scrubber Water Press (MXP-PW)
Scrubber Water Flow (MX-PW)
ID Fan Inlet Press (FAN-OG)
Quench Water pH (QUE-PH)
CHEAF Water pH (CHF-PH)
Scrubber Water pH (MX-PH)
ID Fan Water Spray (FANH20)
ID Fan Vibration (FANVIB)
Stack Temperature
ID Fan Drive Speed (QUE-H20)
Makeup Water Press (QUE-H20)
Makeup Water Flow (MU-H20)


UNITS
%
OF
PSI
PSI
OF
oF
GPM
GPM

oF
inH20
inH20
inH20
PSI
PSI
OF
in
in
PSI
GPM
inH20



GPM
mil
OF
RPM
PSI
.GPM


TIME












































































































































































































































































































































































































H
H
H
1
U)
Ul

-------
                                                               Fig,  11

                                                    UTILITY  OPERATING LOG SHEET
                                                              HOUR LOG
DATE:
                                            SHIFT:
OPERATOR:
ITEM
Quench Sump Inst Air (QUE-IA)
Quench Pump Seal H20(QUEP-SW)
CHEAT Pump Seal H20 (CHFP-SW)
Scrubber Pump SealH20(MXP-SW)
Diesel Tank Level #1(DT1L-DF)
Diesel Pump Press (DFP-DF)
Fan Drive Temperature (FAN)
Fan Drive Oil Press (FAN -MO)
Scrubber Sump Inst Air(MX-IA)
CHEAF Sump Inst Air (MX-IA)
Alkaline Tank #1 (SATL-SA)
Alkaline Tank #2 (SATL-SA)
Alkaline Pump Press (SAP-SA)
Waste Water Tank Level (WWTL)
Steam Generator Temp (STG-SO)
Steam Generator Press (STG-SO)
Steam Gen Water Level( STG-SO)
Feed Water Press DNST(STG-FW)
Feed Water Press UPST(STG-FW)
Feed Water Tank Level ( STG-FW)
Dynactor Tank Level (DYNA-DF)
Dynactor Oil Temp (DYNA-MO)
Dyn Gen Engine Press { DYNA-MO)
Dyn Gen Engine Temp( DYNA-H20)

UNITS
SCFM
GPM
GPM
GPM

PSI
o
PSI
SCFH
SCFH
in
in
PSI
in
°F
PSI
inH20
PSI
PSI
inH20
in
°F
PSI
°F

TIME
,

























,







































































































,


















































































































































































-------
                                     111-37
       Table 16. Solids Trial Burn Schedule/Kin-Buc Demonstration  (1983)











	Date	Scheduled Activity	




August 13            Start-up incinerator on fuel oil




August 15            Start Kin-Buc oily leachate




August 29            Start Phase I testing; clean soil and oily leachate




September 5          Start Phase II testing; PCB's in soil with diesel oil




September 8          Start Phase III testing; PCP in sand with diesel oil




September 10         Finish last run  (Test 2, Run 3)

-------
                                      111-38

K.  SITE CLEANUP
    Following completion of  the  trial burn program,  all residual solid wastes that
    remain will be destroyed.  Assuming  that  incineration operations  went smoothly
    based on on-site observations, and that preliminary analytical results are posi-
    tive  (e.g., as indicated by  low CO values),  EERU will destroy any trial burn
    residual wastes in  the mobile  incineration  system.   During residual waste
    destruction the unit will be operated under the  trial burn conditions (see
    Table 14).  If the  quantities  of remaining  solid wastes  are too large to inci-
    nerate, environmentally  acceptable treatment/disposal procedures  will be iden-
    tified and utilized for  the  left-over wastes.  The  rotary  kiln ash will be
    either delisted according to 40 CFR  260 requirements or  disposed  of as hazardous
    waste in a permitted secure  landfill.

L.  QUALITY ASSURANCE PROJECT PLAN
    The Quality Assurance Project  Plan which  includes a QA operations plan
    (Part A) and  a QA Sampling and Analytical Plan  (Part B)  is given  in
    Appendix A.

-------
          APPENDIX A
QUALITY ASSURANCE PROJECT PLAN

-------
                                                       Section No:
                                                       Revision No:
                                                       Date:   Draft
                                                       Page 1  of 1
    1.0  QUALITY ASSURANCE PROJECT  PLAN
         PROJECT TITLE:

         DOCUMENT CONTROL NUMBER:
         EPA PROJECT OFFICER:
         EERU PROGRAM DIRECTOR:
         PERFORMING ORGANIZATION:

         DURATION:
         TYPE OF PROJECT:
         SUPPORTING ORGANIZATION:
             The U.S. Environmental Protection Agency
             Mobile Incinerator System Solids Trial Burn
             EERU/QA-3
             Ira Wilder
             K. E. Honeycutt
             IT Corporation - EERU, GSA Raritan Depot,
             Edison, New Jersey  08837
             February 1983 to December 1983
             Work Order under EPA Contract 68-03-3069
             U.S. Environmental Protection Agency
             Municipal Environmental Research
             Laboratory, Solids and Hazardous Waste
             Research Division, Oil and Hazardous
             Materials Spills Branch
APPROVALS:
IT CORPORATION
                  EPA
NAME:  Victor KaIcevie
TITLE:  QA Officer
SIGNATURE:
Date
NAME:  Ira Wilder
TITLE:  Project Officer
SIGNATURE:              Date
NAME:  K. E. Honeycutt
TITLE:  Program Director
SIGNATURE:                Date
                  NAME:  Lawrence J. Kamphake
                  TITLE:  QA Officer MERL
                  SIGNATURE:              Date
NAME:  R. A. Miller
TITLE:  Demonstration Test Task Manager
SIGNATURE:                 Date
NAME:
TITLE:  Sampling and Analytical Program Manager
SIGNATURE:                Date

-------
                                       CONTENTS
                                                                 Section No:   2
                                                                 Revision No:  0
                                                                 Date:  Draft
                                                                 Page 1 of  3
SECTION NO.
 1.0       Title  Page
 2.0       Table  of  Contents  and Distribution
 3.0       Project Description
 4.0       Project Organization and Responsibilities

          Part A -  Operations
 5.0A      Quality Assurance  Objectives
 6.OA      Sampling  and  Data  Collection  Procedures
 7.0A      Sample Custody
8.OA      Calibration Procedures  and  Frequency
9.0A      Analytical Procedures
 10.OA     Data Analysis, Validation,  and Reporting
 11.OA     Internal  Quality Control Checks
 12.OA     System and Performance  Audits
13.0A     Preventive Maintenance
14.OA     Specific  Procedures  to  be Used to
          Routinely Assess Data Precision,
          Accuracy, and Completeness
15.0A     Corrective Action
16.OA     Quality Assurance Reports to Management

          Part B  - Source Sampling and Analytical
5.OB      Quality Assurance Objectives
6.OB     Sampling and Data Collection Procedures
7.OB     Sample Custody
8.OB     Calibration Procedures and Frequency
9.OB     Analytical Procedures
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                                CONTENTS (Continued)
                                                           Section No.:  2
                                                           Revision No..  0
                                                           Date:  Draft
                                                           Page 2 of 3
10.B     Data Analysis, Validation, and Reporting
11.OB    Internal Quality Control Checks
12.OB    System and Performance Audits
13.OB    Preventive Maintenance
14.OB    Specific Procedures to be Used to
         Routinely Assess Data Precision,
         Accuracy, and Completeness
15. OB    Corrective Action
16.OB    Quality Assurance Reports to Management
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                                     APPENDICES

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                                  TABLES
Table
 No.                                                                Page

Part A
  1       Quality Assurance Objects for Precision, Accuracy, and
          Completeness for Combustion and Operating Parameters      5A-2

Part B
  2       Quality Assurance Objectives for Precision, Accuracy,
          and Completeness                                          5B-2

  3       Summary of Trial Burn Analytical Procedures               6B-2

  4       Activity Matrix for Calibration of Equipment              8B-2

  5       Activity Matrix for Calibration of Apparatus              8B-4

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                                  FIGURES


Figure
  No.                                                              Page

Part A
   1      Overall Project Organization                             4A-2

   2      Sampling and Analysis Project Organization               4A-5

   3      Data Flow and Reporting Scheme                          10A-4


Part B
   4      Organic Sampling Train                                   6B-3

   5      Sample Bottle Label                                      7B-2

   6      Chain of Custody Form                                    7B-3
                                                                   "7 ID	 A
   1      Sample Analysis Request

   8      Sample Distribution Sheet                                7B~6
   9      GC/MS Directed Analysis Report Form                     10B-6

  10      GC/MS Survey Report Form                                10B-7

  11      LRMS Analysis Report                                    10B-8

  12      Certificate of Analysis                                 10B-9

  13      Proximate Analysis Reporting Form                       10B-10

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                                                            Section No;   2
                                                            Revision No:   0
                                                            Date:   Draft
                                                            Page 3 of 3
                   DISTRIBUTION OF TRIAL  BURN  QA  PROJECT PLAN
IT CORPORATION:
    W. D. King, IT Corporation President
    K. E. Honeycutt, EERU Project Director
    C. Pfrommer, EERU R&D Group Manager
    R. A. Miller, EERU R&D Trial Burn Task Manager
    J. H.. Exner, EERU Project Technical Coordinator
    V. Kalcevic, EERU Project QA Officer
    T. Geisler, Trial Burn QA Coordinator
    R. Lovell, EERU R&D Senior Project Manager
    	, Sampling and Analytical Program Manager
          	, Sampling Coordinator
    	   , Analysis Coordinator

EPA MERL:
    I. Wilder, EERU Project Officer
    L. J. Kamphake, MERL QA Officer
    J. J. Yezzi, Jr., EERU Deputy Project Officer

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                             PART A OPERATIONS
D90STB

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                                                       Section  No:   3A
                                                       Revision No:   0
                                                       Date:  Draft
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3.0 A     PROJECT DESCRIPTION
         This project covers the RCRA solids feeds demonstration  test burn
         operation of the Environmental Protection Agency's Office  of Research
         and Development's Mobile Incinerator System by the Environmental
         Emergency Response Unit (EERU) at the Kin-Buc landfill site in  Edison,
         New Jersey.  The operation system and planned tests are  described  in a
         separate document "Mobile Incinerator System Solids Trial  Burn  Plan",
         February 24, 1983.  The system consists of a rotary kiln,  a secondary
         combustion chamber,  and an air pollution control train,  each  mounted on
         .a heavy duty over-the-road semitrailer.  The system is designed for
         field use to destroy/detoxify hazardous and toxic organic  substances
         that have contaminated soil or water at spill sites or at  "orphaned"
         dump sites.  Liquids,  sludges,  and contaminated debris that have been
         shredded or otherwise prepared for processing can be introduced into
         the system.

         The incinerator system has undergone a previous trial burn  incinerating
         chlorinated liquids.   The  purpose of these demonstration tests is  to
         evaluate and demonstrate the mobile incinerator's ability  to safely
         destroy hazardous and toxic solids materials in accordance with the
         requirements of the  Resource Conservation and Recovery Act  (RCRA).
         This objective  will  be met by:   (1)  measuring the destruction and remo-
         val efficiencies (ORE) for the  specified test materials,  (2) deter-
         mining particulate and acid gas removal efficiencies for the air
         pollution control equipment,  and (3) continuously monitoring the
         system's operating conditions and emissions.   In addition to defining
         the performance capability of the system,  the data generated will fur-
         nish background information for subsequent permitting associated with
         the on-going use of  the  mobile  incineration system for cleaning up
         spill  and dump  sites.   As  such,  the  data quality level objective for
         this project is Level  2, requiring a high degree of quality assurance
         coverage.

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                                              Section No:  3A
                                              Revision No:  0
                                              Date:  Draft
                                              Page 2 of 2

 The  solids  feed demonstration test burn is planned for the last 7 days
 of the  30-day Kin-Buc demonstration operation.   The test burn will be
 done in three phases:

 Phase I
 Clean soil  will be fed to the incinerator while burning Kin-Buc oily
 leachate.   The purpose of this phase would be to determine practical
 operational ranges for the solids  handling system, the incinerator ram
 feed system,  the rotary kiln  (inclination and RPM),  and the  rotary kiln
 ash  handling system.   Phase I will not be either a RCRA or TSCA solids
 trial burn  since the  soil used will be certified as  nonhazardous.

 Phase II
 Will consist of  three  test runs  feeding 2000 Ib/hr of  a soil  con-
 taminated with less than 50 ppm of PGBs.   During this  phase  diesel fuel
 will be used as  auxiliary fuel rather than the  Kin-Buc oily  leachate.
 The  PCB contaminated  soil which  will be either  a clean,  artificially
 contaminated soil,  or  an actual  PCB contaminated soil  from an existing
 site.   Phase II  will  be an RCRA trial burn,  but not  a  TSCA trial burn
 because the  PCB  soil  concentration will be <50  ppm.  The purpose of
 this  phase  is  to demonstrate  the mobile incinerator's  capabilities for
 detoxifying  contaminated soil.

 Phase III
Will  consist of  three  test runs  feeding 500 Ib/hr of a 50:50  mixture of
pentachlorophenol  (PCP)  and sand.   During this  phase diesel fuel will
be used as auxiliary fuel  rather than the Kin-Buc oily leachate.
Phase III will be  a RCRA solids  trial burn.   The purpose of this phase
is to obtain a flexible  solids RCRA permit for  the mobile incinerator.

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                                                       Section No:   4A
                                                       Revision No:   0
                                                       Date:   Draft
                                                       Page  1  of 7

4.0A     PROJECT ORGANIZATION AND RESPONSIBILITIES
         The overall project organization and reporting  relationships are  shown
         in Fig. 1.  IT Corporation, the EERU operations  contractor,  has overall
         responsibility for the demonstration test burn.  This  responsibility
         includes the  operation, sampling and analysis,  accumulation of data,
         and reporting  the results.  This Quality Assurance  Project  Plan  covers
         these activities.  The following sections of  this plan  are divided  into
         two parts.  Part A covers operation, data accumulation, and  reporting
         results while Part B covers source sampling and  analytical.   This trial
         burn is a major  task and therefore will have an assigned QA coor-
         dinator.  Descriptions  of the responsibilities  of key  individuals  are
         given below:

         The quality assurance officer,  V.  Kalcevic,  has  the primary  respon-
         sibility for reviewing and approving the QA Project Plan and  for over-
         seeing the project to assure that the QA objectives are met.  He
         reports directly to the IT Corporation president, W. D. King, who has
         overall responsiblity for the organization's activities, including  QA.

         The quality assurance coordinator,  T. J. Geisler, is responsible for
         reviewing and advising on all aspects of QA/QC.   He reports  to the ESRU
         project director,  K.  E. Honeycutt.   Some responsibilities of  the QA
         coordinator are:

           •  Assisting the task manager,  R.  A.  Miller, in specifying  QA/QC pro-
              cedures  to be used for this  project.

           •  Reviewing and commenting on  the QA Project  Plan for sampling and
              analysis  to ensure that the  methodologies and QA/QC procedures
              proposed will meet the overall  quality objectives set forth in
              this  plan.

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QUALITY ASSURANCE
   QA OFFICER

   V. KALCEVIC
  TRIAL DURN QA
   COORDINATOR

  T. J. GEISLER
         I	
                                       IT CORPORATION
                                          PRESIDENT
                                         W.  D.  KING
                                       EERU  PROGRAM
                                     PROJECT DIRECTOR

                                      K.  E.  HONEYCUTT
                          EERU R&D
                        GROUP MANAGER

                         C.  PFROMMER
                                                       t
                     MOBILE INCINERATOR
                         TRIAL DURN
                        TASK MANAGER

                        R.  A. MILLER
                                                        USEPA/MERL

                                                        01IMS BRANCH
                                     ITAS
                             JAMPLING & ANALYTICAL
                                PROGRAM MANAGER
                                                                     HJ O JO W
                                                                     (U PI (D (t>
                                                                                           O D
                                                                                               W  H-
                                                                                               H- O
                                                                                               O  3
Fig.
                               Overall Project  Organization
-J H> 0
  rf ••

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                                              Section No:  4A
                                              Revision No:  0
                                              Date:  Draft
                                              Page 3 of  7
  •   Conducting any required performance and systems audits.

  •   Reviewing data generated during the trial burn, including ex-
      amining chromatograms,  calculations,  and data books.

  «   Submitting brief  reports on field inspections and audits con-
      ducted.

  •   Reporting,  as  a section in the final  test burn report to the EPA,
      the  results  of the  Quality Assurance  Program.

The task  manager, R.   A.  Miller,  has overall responsibility for the
mobile incinerator  operations and for the  coordination with the
sampling  and  analysis  program manager during the  test burn program.
For this  purpose  he reports  to the EERU R&D group manager,  C.  Pfrommer,
who in turn  reports to the ERRU project director,  K. E.  Honeycutt,  who
has the overall responsibility for the EERU project to the EPA.    Some
of the task manager's  responsibilities are:

  »  Preparing, obtaining approval of,  and distributing the QA Project
     Plan for  the mobile  incinerator test  burn.

  •  Managing  the field operations of the  mobile  incinerator.

  «  Deciding when  test run  sampling shall be conducted.

  •  Calling to the attention of  the quality assurance officers  and
     others, as appropriate,  any  problems  arising during  the test burn
     that affect  this  QA  Project  Plan so that the  problems  can be
     resolved in a  timely manner.   Responsible  for properly documenting
     any modifications to this  plan.

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                                              Section No:   4A
                                              Revision No:   0
                                              Date:   Draft
                                              Page 4 of 7
  •   Issuing  a  final  test  burn  report to the  EPA.

The sampling  and  analysis  program manager,	,  has  overall tech-
nical and management  responsibility  for  the sampling and analysis
operations and  for  coordination with the mobile incinerator operations
task manager.   For  this  purpose  he  reports to the EERU project direc-
tor, K. E. Honeycutt, who  has  overall responsibility  for  the  EERU pro-
ject to the EPA.

The sampling  and  analytical project  organization and reporting rela-
tionships are shown in Fig. 2.

Descriptions  of the responsibilities  of  the individuals  who will  spe-
cify the elements of  a QA/QC program are  given below.

The Quality Control and Data Manager  is  responsible  for  QA/QC  activi-
ties such as  reviewing and advising  on all  aspects of  QA/QC.   This
includes:

  •  Assisting  the  Program Manager in specifying QA/QC procedures  to be
     used during  the program.

  •  Making in-house  QC evaluations  and  submitting audit samples  to
     assist in  reviewing QA/QC  procedures,  and

  •  If problems are detected,  making recommendations  to the Program
     Manager,  Sampling Coordinator and Analysis  Coordinator, concerning
     repeat samples and analyses  and/or procedure changes.

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                                         ITAS
                                SAMPLING & ANALYTICAL
                                   PROGRAM MANAGER
 ANALYSIS
COORDINATOR
 SAMPLING
COORDINATOR
QUALITY CONTROL
fi DATA MANAGER
                                 YORK SUBCONTRACTOR
                                        SUPPORT
                   Fig.  2.   Sampling and Analysis Project Organization
                                                                                          pi p> (D Q>
                                                                                          Ul
                                                                                          o
                                                         W H-
                                                         H- O
                                                         O 3
                                                                                               25 O
                                                                                               0 "
                                                                                               O >

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                                              Section No:   4A
                                              Revision No:   0
                                              Date;   Draft
                                              Page 6 of 7
  «  Receiving  samples  from the  field and verifying that incoming
     samples  correspond to  the packing list or chain-of-custody sheet;

  •  Maintaining records  of all  incoming samples,  tracking those
     samples  through  subsequent  processing,  analysis,  and ultimately
     appropriate disposal of those  samples  at the  conclusion  of the
     program;

  »  Preparing  quality  control samples for  analysis before and  during
     the program;

  •  Preparing  QC and sample data for review by the Analysis  Coor-
     dinator  and the  Program Manager;

  •  Preparing  QC and sample data for transmission and entry  into the
     computer data base.

The Analysis Coordinator  is  responsible  for  laboratory activities.
These include:

  «  Training and qualifying personnel in specified laboratory  GC and
     analytical procedures,   before  receiving samples;

  «  Verifying  that laboratory QC and  analytical procedures are  being
     followed as specified in the plant-specific S/A plan  and reviewing
     sample and  QC data at  least weekly.  This  weekly  review will
     include examination  of  raw data  such as  chromatograms  and  checking
     of arithmetic calculations for a  minimum of 5% of  the  samples ana-
     lyzed, as well as inspection of  reduced  data,  calibration  curves,
     and bound laboratory notebooks.

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                                              Section No:   4A
                                              Revision No:   0
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The Sampling Coordinator  is  responsible  for  field  activities.   These
include:

 •    Interacting with  YSC to ensure  that the stack  sampling is  being
      conducted  in  a  manner consistent with this  project plan.

  •   Determining,  with the Analysis  Coordinator, appropriate sampling
      equipment  and sample containers to  minimize contamination;

  •   Ensuring that samples are  collected, preserved,  and  transported  as
      specified  in  the  plant-specific detailed S/A plan.

  •   Checking that all sample documentation  (labels,  field  notebooks,
      chain-of-custody  records,  packing lists)  is correct  and trans-
      mitting that  information with the samples to  the  analytical
      laboratory.

The YSC Stack Sampling Manager  is responsible  for all  stack  sampling
activities.  For this  purpose he reports  to  the  ITAS Sampling
Coordinator.

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                                                       Section No:   5A
                                                       Revision No:   0
                                                       Date:   Draft
                                                       Page 1  of 3
5.0A     QUALITY ASSURANCE  OBJECTIVES
         As part of  the  overall measurement objective of the  test burn,  the
         mobile incineration  system must be shown capable of  operating at the
         conditions  set  forth in RCRA  regulations.

         The test burn overall quality objective  is  Level 2 coverage,  which
         means that  the  test  burn will provide  extensive scientific data,
         requiring regular  QA audits and rigorous QC procedures.

5. 1       PRECISION,  ACCURACY,  COMPLETENESS
5.1.1    Combustion  Parameters  — The  regulations require continuous  monitoring
         of contaminant  mass  flow rate and  combustion temperature as  well  as
         flue gas concentrations  of CO,  C02, O2,  and NOX.  In addition to  these
         parameters, the RCRA interim  regulations require monitoring  of  the air
         feed rate.  Although not required  by the regulations,  the  S02 con-
         centration  in the  flue  gas will be monitored to verify the low  sulfur
         content of  the  auxiliary fuel oil  used.   The data for these parameters,
         as well as  others  measured by the  source sampling contractor, must be
         precise,  accurate,  and  complete.   The  objectives  for precision,
         accuracy,  and completeness of  data for the  parameters  indentified above
         are given in Table 1.   Definitions  of  these terms are  as follows.

         Accuracy—The degree of  agreement  of a measurement (or an  average of
         measurements of the  same thing), X, with an accepted reference  or true
         value,  T,  usually  expressed as  the  difference between  the  two values,
         X - T,  or the difference as a percentage of the  reference  or  true
         value,  100  (X - T)/T.  Accuracy  is  a measure of  the  bias inherent in
         the system.

         Precision—A measure of  mutual  agreement (or variability)  among indivi-
         dual measurements of the same property,  usually  under  prescribed  simi-

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                                                                          Section No:
                                                                          Revision No:
                                                                          Date:   Draft
                                                                          Page 2 of 3
                                                                 5A
                                                                  0
                                Table 1,  Quality Assurance  Objectives  for
                                 Precision,  Acuracy,  and  Completeness for
                                   Combustion and Operating Parameters
   Parameter
Method of Measurement
SCC temperature

Waste oil flow rate

CO



C02 d
Air feed rate

Total hydrocarbons^
Thermocouple

Electronic flow meter

Methanizer coupled to
gas chromatograph/
flame ionization det.

Gas chromatograph/
thermal conductivity
detector

Gas chromatograph/ •
thermal conductivity
detector

Chemilurainescent
analyzer

Annubar

Gas chromatograph/
flame ionization
detector
Precision3 (%)  Accuracyb(%)  Completenessc ("%T

     5              5              90

     5              5              90

     5e             5e             90
                                   90
                                                                                 90
     10*


     5

     5e
                                                                  10*
80


90

90
aExpressed in terms of the relative standard deviation as defined in Section 14.1.
^Expressed as the percentage difference from tire true (standard)  value.
cExpressed as the amount of valid data obtained compared to the total amount expected,
^Based on experience during the incinerator shakedown test.
eBased on results of the liquid trial  burn,      the levels of CO and THC in the
 combustion gases were very low.  Precision and accuracy will need to be within +5%
 or 5 ppra., which ever is greater.
^Based on results of the  liquid trial burn,     the level of NOX in the combustion
 gases were very low.  Precision and accuracy will need to be within _+10% or 10 ppm,
 whichever is greater.

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                                                       Section No:   5A
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          lar  conditions  and usually expressed in terms of the standard
          deviation.   Various measures of precision exist, depending on the
          "prescribed  similar conditions."

          Co_mpleteness_—A measure of the amount of valid data obtained from a
          measurement  system compared to the amount that was  expected to be
          required  to  fully  evaluate and understand the system under optimum con-
          ditions,  usually expressed as a percentage.

5.2       REPRESENTATIVENESS
5.2.1     Definition — This term refers to the degree  to which data accurately
          and  precisely represent a characteristic or a population,  parameter
          variations at a sampling point,  or an environmental condition.

5.2.2     Combustion Parameters  — The combustion parameters  for which represen-
          tativeness could be a  problem are combustion  temperature and the  flue
          gas  component concentrations.   The thermocouple for temperature
          measurement will be shielded from flame radiation and will have com-
          bustion gases circulated around it.   The sampling points for flue  gas
          compounds will  be  located in the centers of the ducts.  At test con-
          ditions the gas  flow at the  sample points will be turbulent,  ensuring
          complete  mixing.

5.3      COMPARABILITY
5.3.1    Comparability is defined as  the  measure of confidence with which  one
         data set  can be  compared with  another.

5.3.2    Triplicate sampling runs  will  be conducted for each test.   The com-
         parability of the  triplicate  data sets  will be addressed in the final
          QA report.  All  data will be  reported in consistent SI units.

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                                                       Section No:   6A
                                                       Revision No:   0
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                                                       Page  1  of 4

6'°A     SAMPLING AND DATA COLLECTION  PROCEDURES

6.1       COMBUSTION PARAMETERS
         The sampling and data  collection  procedures  for waste flow rate,  fuel
         flow rate, water flow  rate, temperature,  CO,  C02,  02, NOX,  air flow
         rate, and total hydrocarbons  are  described below.   Other  parameters
         required by regulations  are covered in the source  sampling and analysis
         section.

         The waste solids feed  to the  rotary kiln is  controlled by a mechanical
         timer/sequencer that cycles a hydraulic  feed ram.   The desired feed
         rate is obtained by adjustment  of the  cycle  time and pull back position
         of the ram feeder  (volume).

         The incinerator operator will manually record the  waste feed rate every
         15 minutes.  The solids  feed  for  each  test before  being fed will  be in
         weighed drums and the  amount  used will be measured to confirm that the
         instantaneous flow rates are  consistent.

         The flue gas composition will be  continuously monitored at two loca-
         tions.  The first location is in  the quench  elbow  immediately upstream
         of the water spray; the  second  is at the  stack.  One advantage of moni-
         toring at these two points is that the amount of air in-leakage from
         the air pollution control equipment can be calculated.

         A gaseous sample is withdrawn from the center of the duct  through a
         1/2-in. ceramic probe.  The extracted sample  passes through a ceramic
         inertial filter, located inside the probe, to remove particulate
         material (greater than 100 micron)  from the  gas  sample.  There is
         another filter at the Perma Pure  dryer.   Filtration  is  required for

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                                              Section No:   6A
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instrument protection.   Next,  the filtered gas is partially cooled in
an air-air heat exchanger to lower the temperature to 10 to 20°C (50 to
68°F).   Entrained liquids are  collected in a liquid trap at the bottom
of the exchanger.   The  gas sample then passes through a vaporizer
(120°C)  to ensure that  any entrained liquids from the process are
vaporized  before entering the  gas drying unit.  Gas drying will be
accomplished  in a Perma Pure dryer that removes water vapor from the
gas sample without using a condenstion process, since condensation
often removes key gaseous components from the sample.  The cooled and
dried gas  sample is then transported to the gas chromatographs and
chemiluminescent analyzer through Teflon® tubing.   The sampling and
sample transport functions are all controlled by a microprocessor.   The
sampling function of the gas monitoring system is continuously
operating  to  provide fresh,  up-to-date gas samples to the analyzers for
stack and  flue  gas analysis.

The temperature of the  SCC will be monitored with a thermocouple,  ANSI,
type S (Pt/Pt-Rh),  in direct contact with the flue gases.   The ther-
mocouple is located at  the exit of the SCC and is  shielded from the SCC
burner flames to eliminate temperature measurement error  associated
with flame radiation.   The millivolt thermocouple  signal  is  converted
to a (4-20 ma)  signal and is recorded on a strip chart recorder which
is in the  control  panel on the kiln trailer.   System specifications  and
calibration points  are  listed  below:

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                                                       Section No:   5A
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                                                       Page 3 of 4

               Temperature range:      0 - 2500°F
               Linearity:              ±1.3°F
               Calibration accuracy:   ±1%
               Calibration points:     0% of full scale = 0°F = -0.092 mV
                                      50% of full scale = 1250°F =  6.029 mV
                                      100% of full scale = 2500°F = 14.018 mV

         Several  operating parameters not required in the TSCA and RCRA regula-
         tions for  monitoring incinerator performance will also be measured.
         These include  the auxiliary fuel feed rates to the kiln and the SCC;
         the water  injection rate  to the kiln;  the skin temperatures of the
         kiln,  SCC,  and ducts;  the quantity of wastewater blowdown collected;
         and the  alkaline water feed rate and concentration.   These data will  be
         employed in heat and material balances calculations.

         The fuel and water feed rates and air flow rates will be  read from
         rotameters  and recorded hourly in the log sheets.   These  instruments
         will  be  calibrated before the trial burn program according to manufac-
         turer's  recommendations.  Skin temperature of the kiln, SCC,  and
         ducting  will be  measured  at least once during each test using a digital
         surface  thermocouple.  Wastewater collected during a test will be
         measured at the  end of each test by the change in liquid  level in the
         wastewater  tank.   An ORSAT  analyzer will be used to obtain backup data
         on Oo  and COo  concentrations.   One  ORSAT sample  will be taken during
         each  test.  The  ORSAT  analysis  is described in EPA Method  3
         (40 CFR  60).

6.2      SAMPLING PERIODS
         Sampling using the  MM5 apparatus  must  be conducted when the incinera-
         tion  system is at  steady-state.   The project task manager  will  deter-

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         mine when sampling may  begin, based on a review of data from the
         continuous monitoring equipment.  The sampling time will be sufficient
         to process 5 dry standard cubic meters of stack gas through the MM5
         apparatus.  During sampling  the task manager will periodically verify
         that steady-state conditions exist.  Steady-state operation is defined
         as consistent operation with less than 5% drift during 1 hr on the
         following parameters:   SCC temperature, waste feed, and flue gas O2
         concentrations.  These  parameters will be checked at least every
         30 minutes.  If a transient  condition develops during sampling, the
         task manager and QA coordinator will decide whether to temporarily
         interrupt or terminate  sampling.

6. 3      SAMPLING OF CONTAMINATED SOIL FEED
         PCB contaminated soils, <50 ppm, for the Phase II  tests will either be
         on actual contaminated  soil, if one can be located, or a prepared mix-
         ture.  The method of preparing a synthtic mixture  is discussed in the
         test burn program.  Arochlor 1260 would be used as the PCB  source
         material.

         The petachlorophenol (PCP): sand 50:50 mixture will be prepared by
         mixing commerical grade PCP  (mp.~180°C) manufactured by either Vulcan
         Chemicals or Reichold Chemical Company with certified clean sand.

         The prepared feed materials will be placed in sealed drums for storage
         and handling.   While being placed in drums several soil samples per
         drum will be obtained and composited.

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7.0A     SAMPLE CUSTODY


7.1       COMBUSTION  SYSTEM PARAMETERS

         Samples  for CO,  CO2,  £>2'  N<-*x' an(^ TH("' are 'fca^cen  an<^ analyzed on-site
         automatically.   Sample custody procedures are  not required because
         samples  are transferred to the analyzers in  a  sealed system.

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8.0A     CALIBRATION  PROCEDURES  AND  FREQUENCY

8.1      COMBUSTION PARAMETERS

8.1.1    Temperature  Monitoring  System
         The thermocouple  converter  and  recorder are calibrated by  inputting a
         millivolt signal  which  corresponds  to  a given temperature  signal
         according to ANSI Standard  Thermocouple Tables.   The output signal is
         then adjusted  to  proper temperature reading.   The temperature moni-
         toring system  cannot be calibrated  during  operation  of the mobile
         incinerator, so calibration of  the  instrument will be done before  the
         start of the trial burn, during the shutdown  periods,  between tests 3
         and 4, between tests 6  and  7, and after test  9.   If  the calibrations
         show a significant drift (>2%)  in the  accuracy of the temperature  moni-
         tor, the deviation will be  recorded and the instrument recalibrated.
         The thermocouple  will be calibrated before  the trial burn  program  with
         ASTM thermometers traceable to  the  National Bureau of Standards.

8.1.2    Waste Feed Rate
         The hydraulic feed ram  volume,  stroke  adjustment, and cycle  timing will
         be calibrated just before the test  burns are  conducted and will  be
         checked before the start of each test  period.

8.1.3    CO, C02,  02,  NOX,  THC (Continuous Monitors)
         The gas chromatographs  and chemiluminescient  analyzers  used with the
         continuous off-gas monitoring equipment will  be calibrated by selec-
         tively opening valves on certified  gas  standards  that direct  calibrated
         gas mixtures  into the sampling probe assemblies on the  incinerator.
         The calibration gas passes through  the  same sample conditioning  and
         transfer  systems  to the analyzers as the actual incinerator samples.

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         This technique not only calibrates  the  analyzers  but corrects for
         losses that can occur during sample  conditioning.   The calibration of
         the analyzers generates a four-point calibration  curve for each gas
         component using a zero gas, pure nitrogen,  and  three standard gases
         with different concentrations.  The  gas  mixtures  used for calibration
         will be certified gas standards traceable  to  the  National Bureau of
         Standards where possible.  The concentrations of  the calibration stan-
         dard gases used will be close to and will  span  the  expected values in
         the gas stream.

          A four-point calibration will be conducted daily before  the start of
          any testing operations.  A single-  point  calibration check,  using a
          Standard gas near the measured  concentration  of each gas,  will be
          conducted between each test run.

8.2      SECONDARY PARAMETERS
         Some operating parameters not requiring  monitoring  according to TSCA
         and RCRA standards include:   auxiliary fuel feed  rates  to  the kiln and
         SCC, the water injection rate to the  kiln,  the  skin temperature of the
         combustion chambers and ducts, the wastewater purge  rate,  and the  alka-
         line water feed rate.  The instruments used to  measure  these parameters
         will be calibrated before the trial  burn according  to the
         manufacturer's specifications.

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                                                       Section No:   9A
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9. OA     ANALYTICAL PROCEDURES

9.1       COMBUSTION PARAMETERS
9.1.1    No analyses are required for the following:   combustion temperature,
         fuel oil rates to kiln and SCC, waste oil flow  rates,  water  flow rate
         to kiln and wastewater collected in each test.   These are  all  direct
         readings from the instruments.

9.1.2    The stack and SCC flue gases will be analyzed for  the important gaseous
         components:  02, CO2, CO, NOX, S02, and THC.  The  analyzer section  of
         the monitoring equipment operates in conjunction with the  microproc-
         essor to direct sample gases to (1) the thermal  conductivity detector
         GC for analysis of C02/ 02, and S02; (2) though a methanizer  to a
         flame ionization detector GC for analysis of CO; (3)  the flame  ioniza-
         tion detector GC for analysis of THC (compared to a  methane standard);
         and (4) a chemiluminescent detector for analysis of  NOX.   The
         microprocessor generates printouts of all analytical results.   A
         detailed description of gas analysis procedures can  be found in
         Section VI of the Trial Burn Plan, Appendix 17.1.

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10.OA    DATA ANALYSIS, VALIDATION,  AND REPORTING

10.1     DATA REDUCTION
10.1.1   Combustion Parameters
         The CO and CO2 data will  be used  to  calculate combustion efficiencies
         by the following equation:

                                           [C02]
           Combustion efficiency  (%)  =   Trv-n	IT71T  X 100%
              Where:
                   [CO] = concentration of CO, percent by  volume
                   [CO2J = concentration of C02,  percent by volume
         The [CO] values recorded  in ppm will be  converted to percent  for  use  in
         the above equation.

         The average mass flow rate  of  waste oil  will  be determined  by dividing
         the total mass flow for a sampling period by  the  sample  time.

         If the internal calibration  checks described  in Section  11.0  indicate
         that instruments are operating within the accepted accuracy tolerances,
         any drift in calibration will  be taken to be  linear  with time  and the
         data will be corrected accordingly.

1 0. 1. 2   The combustion parameter and source sampling  data will be reported to
         the project task manager, who will calculate  destruction and  removal
         efficiencies (DREs) for the specific POHCs fed  to the incinerator.  The
         ORE for any material is defined as the efficiency of  the system in
         destroying or removing that material from the gaseous effluent of the
         incinerator.   It is mathematically defined as follows:

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                                                       Section No:  1 OA
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                                                       Page 2 of 4
                  DRE  (%)  .              .  x 100

              Where:
                   W in  =  mass  feed  rate  of a POHC in the waste stream feeding
                           the incinerator,  based on mass  feed of waste oil and
                           composition

                   W out = mass  emission  rate of the same POHC present in
                           exhaust emissions  before release  to the atmosphere,
                           based on  stack gas flow rate and  concentration

10.2     VALIDATION
10.2.1   Combustion Parameters
         Backup measurements will help validate  the primary  data.   The total
         contaminated solids used during each test will be measured by the
         weight and volume used  from prepared feed drums.  An ORSAT analyses  of
         the stack gas will be run and compared  to the gas component con-
         centrations determined  by the continuous  monitors.   The backup measure-
         ment for contaminated soil  quantity  used  must agree  within ±5% of that
         measurement to be valid.  The ORSAT  and continuous  monitor analyes must
         agree within ±10%.

10.3     DATA REPORTING
10.3.1   Combustion Parameters
         The incinerator operators'  log sheets and  the continuous  monitoring
         system operators'  logs  will be used  for reporting data  to the  task
         manager.   These log sheets are shown  in the Appendix.   Calibration
         check results  will be recorded in the "Remarks"  sections  of  the  log
         sheets.   The  results of calibration  checks for all instruments will be
         reported  along with the data in the  final  report.

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10.3.2   Data varying more than two relative standard deviations from the mean
         values will be called outliers.  The outliers will be investigated by
         examination of of log sheets and by comparing the results  from dupli-
         cate samples and backup analyses to determine the cause of  the
         deviation.  If these efforts are unsuccessful, the outlying data will
         not be used in performance assessment of the incinerator system/-
         however, outliers will be reported and discussed in the final report.

10.3.3   Figure 3 shows the sampling, analysis, and reporting responsibilities
         for the test burn.

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                                         REPORTS TO  MANAGEMENT AND EPA
          EMISSION RESUl.TS
              ANALYSIS
           FIELD SAMPLING
 SOURCE SAMPLING AND ANALYSIS


  M.m k G.isns  ( Incl ud i n'j Flow)
-  Wu:;l(! l'ci-d:i Coiri|K).si tion
-  S<•> nli!>r r l.i <|ii ids
-  K I I ii Ash
-  Clir:AF Ash
•  I'irM and l,  Audit
                                                        1
                                                   TRIAL DURN
                                                  TASK MANAGER

                                                  R.  A.  Miller
                                                    I      t,
                                                  -*J      W-
                                                             £
                                                    INCINERATOR
                                                    OPERATIONS
PROJECT .RESULTS ANpJIEPORl-J NG
- Destruction and Removal  Efficiencies
- Heat and  Material Balancer*
- Operating Summarien
- Reports
                                                                     OPERATIONS IjOGS

                                                                        OPERATORS
          :ONTINUOUS MONITOR
                 LOGS
             OPERATORS
  OPERATIONS AND MONITORING
        IT CORPORATION
  System Conditions
  Waste Feed  l-'Jow
  Socondary Combust ion
  Temperature
  Comluiutlon Gau Com[>os J lion,
  (Continuous  Monilorlnq)
  Field Audit  Sampler,
V
0)
«
                                    Fig.  3.   Data 71ow and Reporting Scheme
                               O D
                               Ml ^
                                 Qj
                               J^>. l""h
                                 rt
V cn
(D (D
5 °
03 H-
M- O
O S
3

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                                                      Section No:   11A
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11.OA    INTERNAL QUALITY CONTROL CHECKS

11.1      COMBUSTION PARAMETERS
         Calibration checks will be performed as described in Section  8.0.  The
         operators will perform these checks with standards .of known con-
         centration.

         Internal operating check samples for the continuous monitors  for  flue
         gas CO, C02/ C>2' N0x' and THC wil1 be submitted by the  QA  coordinator.
         The concentrations of the standards supplied by the QA  coordinator will
         not be known by the incinerator operating personnel.  These calibration
         checks will be conducted approximately once per eight-hour shift.

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                                                      Section No:   12A
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12.0A    SYSTEM PERFORMANCE AUDITS

12.1      COMBUSTION SYSTEM PARAMETERS
         A system audit will be made by T. J. Geisler, IT Corporation  trial  burn
         quality assurance coordinator, before the trial burn program  starts.

12.2     SOURCE SAMPLING AND ANALYSIS
         The following samples will be prepared and submitted by  T.  J.  Geisler,
         for analysis before the start of the trial burn program  on  contaminated
         soils as a performance audit of analytical procedures for PCBs and  PCPs
         on solids.  These samples will also be submitted to another laboratory,
         approved by the EPA, for analysis.

         (Note:  These audit samples have not yet been determined.)

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13.OA    PREVENTIVE MAINTENANCE

13.1      COMBUSTION SYSTEM PARAMETERS
         The mobile incinerator operating logs and the monitoring equipment
         operating logs will be used for early identification of potential
         problems that may require correction during an operating period.
         Normal equipment inspection and maintenance will be performed between
         test operating periods according to the equipment manufacturer's recom-
         mendations.

         A spare secondary combustion chamber thermocouple assembly will be kept
         on hand.  An adequate inventory of the recommended supplies and spare
         parts for the monitoring equipment will be maintained.

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14.OA    SPECIFIC PROCEDURES USED TO ROUTINELY ASSESS DATA  PRECISION,  ACCURACY,
         AND COMPLETENESS

14.1      COMBUSTION PARAMETERS
         At the conclusion of each trial burn test period the  data collected
         from the monitoring systems will be assessed in terms of precision,
         accuracy,  and completeness.  This is to ensure that the instrumentation
         is operating properly and to initiate corrective actions if equipment
         performance drifts beyond specified tolerance values.  Precision of the
         data will be expressed in terms of the relative standard deviation
         under similar conditions.  It will be calculated by the following for-
         mulas .
                         1     r
              Mean = x = -   J   x..
                                    where n = number of replicate measurements
                                          x = series of replicate measurements
                                                      -x)2
         Relative  standard deviation =	X 100%

         Accuracy  of  the data will be expressed as the percentage of the
         measured  value compared to the true or accepted value.  The equation
         for  this  calculation is shown below:

             Accuracy  = -~-  X 100%
                                  where x = measured value
                                        T = true value from calibration standard

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                                              Section  No:   14A
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Completeness of the data will be expressed  as  the  amount of  valid data
                                         V
obtained compared to the amount expected.

The importance of maintaining the performance  of the  incinerator  moni-
tors cannot be overstressed.  This equipment provides the primary
measurements for ensuring proper incinerator performance and regulatory
compliance.  The equipment will be maintained  in accordance  with  manu-
facturers specification and an ample supply of critical  spare parts
will be maintained to minimize disruptions  to  the  operation  of  the
incinerator.  If any modifications to the identified  procedures become
necessary to improve operational performance or safety the project task
manager (see Section XII) will approve all  corrective actions and docu-
ment them to the EERU QA Officer.

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                                                       Section  No:   15A
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15.0A    CORRECTIVE ACTION

15.1      OPERATIONAL AND MONITORING PROBLEMS
15.1.1    Combustion Parameters
         Calibration checks will be performed on the waste feed ram and  the SCC
         thermocouple at the end of each test period.  If accuracy is  outside
         the limits specified in Section 5.0, the instrument will be  reca-
         librated and put back into service-  If a second calibration  check
         shows that accuracy is once again outside the acceptable range, the
         instrument will be replaced.   The drift noted in each  of the  calibra-
         tion checks will be taken as  linear with time and readings will be
         corrected accordingly.

         As  defined in Section 11.1,  internal calibration checks will  be per-
         formed on the continuous gas  monitors.   If the accuracy of each gas
         measurement is within limits,  source sampling will continue.   If
         the calibration check shows  that the accuracy of any instrument is out-
         side the acceptable range,  source sampling will be interrupted.  The
         flue gas will then be analyzed again for the concentration of the com-
         ponent in question after which another  calibration check of the instru-
         ment will be  performed.   Two  courses of action are possible depending
         on  the results of  the sample  analysis and second calibration check.

         If  the sample analysis and second calibration check agree  with the pre-
         ceding values,  then the instrument has  apparently stabilized.  A four
         point calibration  of the instrument will be conducted  and  the
         instrument will be put back in service.   Source  sampling will be
         resumed and the data will be  treated as follows:

          •   All data from source sampling and  unaffected combustion parameter
              instruments will be valid.

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           •  Data from the affected instrument will  be  invalid for  the  time
              period during which calibration drifted.

           •  The invalid data will be replaced with  the  first data point
              obtained from the flue gas after the recalibration.  This  single
              value will be applied to the parameter  for  the entire time period
              in question.

         If the sample analysis and second calibration check disagree  with  the
         previous values, there is continuing deterioration  in the integrity  of
         the sampling or analysis trains.  No further source sampling  can be
         conducted until the problem has been discovered  and corrected and  the
         equipment has been recalibrated.  The data taken prior  to discovery  of
         the problem will be invalid,  and the entire test will have to be
         redone.

15.2     NONCONFORMANCE AND OTHER QA PROBLEMS
         A specific corrective action program for each problem will be defined
         as the need may arise.   In general, this program would  be a step-by-
         step analysis to determine where the problem originates, what actions
         are required to correct the problem, or,  if it cannot be controlled,
         what would be the impact on the program results.

         The project QA officer,  V.  Kalcevic, has the responsibility to  promptly
         communicate to the IT Corporation president,  W.  D.  King, and  the EERU
         project  director,  K.  E.  Honeycutt,  these nonconformance or non-
         compliance type problems.   He  is also responsible for ensuring  that the
         corrective actions taken produce the desired results.  As appropriate,
         the IT Corporation president;  the EERU project director; the EERU R&D
         group manager,  C.  Pfrommer;  the task manager, R. A. Miller;  or  the

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source sampling and analysis program manager,	, will be
assigned the  responsibility to implement the appropriate corrective
action program.

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16. OA    QUALITY ASSURANCE REPORTS TO MANAGEMENT
         The project QA officer, V. Kalcevic, will meet with the task manager,
         R. A. Miller,  and the trial burn QA coordinator, T. J. Geisler,  after
         the test burn operating period to review all aspects of the projects
         quality assurance performance.  The project QA officer will assess  and
         summarize the results of this meeting in a memorandum that will  be
         distributed to the IT Corporation president, W. D. King; the EERU proj-
         ect director,  K. E. Honeycutt; the EERU R&D group  manager, C.  Pfrommer;
         the trial burn QA coordinator, T. J. Geisler; and  the task manager,
         R. A. Miller.

         The trial burn QA coordinator will be responsible  for a separate sec-
         tion of the trial burn program report, which will  cover:

           •  Assessment of measurement data precision, accuracy, and complete-
              ness
           «  Performance audit results
           •  System audit results
           •  Significant QA problems and solutions

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                  PART B SOURCE SAMPLING AND ANALYTICAL
D90SSA

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                                                            Section  No. :   5B
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5.OB  QA Objectives
    The overall measurement objective is to determine,  for  each  of  the  feed
    materials selected for testing/ the effectiveness  of  the mobile incineration
    facility in achieving thermal destruction of Arochlor 1260 in soil  and penta-
    chlorophenol  (PCP).

    At the present time, the Agency has not established quantitative guidelines  as
    to the precision, accuracy, completeness, representativeness and/or com-
                                                                       A
    parability criteria that must be met by data generated  in a  trial burn of  hazar-
    dous waste.  However, some specific numerical  QA objectives  for accuracy and
    precision of the sample preparation and analysis procedures  used in the analyti-
    cal laboratory have been developed for this project.  These  guidelines are based
    on ITAS's previous experience in applying comparable  procedures to  a variety of
    complex sample matrices.  In the event that the QA objectives given in this  sec-
    tion are not achievable  due to the fact that  sample  matrices are highly
    variable as well as complex, revised objectives will  be formulated  in con-
    sultation with the EPA.

a.  Accuracy
    Accuracy is defined in QAMS-005/80 as the degree of agreement of a  measurement
    or average of measurements with an accepted reference or true value.   In
    general, our accurach goals for this project are to use reference materials  of
    highest, inown purity for calibrations and spiking so that determinate errors
    due to instrument response and incomplete preparation recoveries can be
    corrected for, so that the primary uncertainties in the analytical  data are  due
    to random errors not exceeding those in Table  2.   For this project,  the QA
    objectives for accurach are expressed in terms of  the following parameters:

    (1)  Reference materials;  All reference materials used as calibration standards
         will be the highest purity commercially available, usually >98%.   Mass
         spectra of Arochlor 1260 and PCP used as  reference materials will be
         obtained to confirm qualitative identification.

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                Table 2.  Quality Assurance Objectives  for Precision,  Accuracy, and Completeness
Analysis
PCP
PCBs
Arochlor 1260
HCl
Particulate
emissions
Measurement •<
Type Matrix Reference
GC/MS 1,4,5,6
GC/EC 1,4,5,6,7 ITAS-SOP
GC/MS 1,4,5,6,7 ITAS-SOP
Titrimetric 1 EPA 325.3

Gra vime tri c 2,6
Precision
Relative Accuracy As
STD/Dev. % Recovery
<30 >50
<30 >50
<30 b
<10

<10
Completeness
95
95
b
95

95
b
Matrix code
1 - MM5 train,  discrete  components except impingers
2 - EPA Method  5  train
3 - Ambersorb/Tenax traps
4 - Scrubber water
5 - Kiln ash
6 - CHEAP ash
7 - Arochlor spiked soil

GC/MS, operated in  the select ion monitoring mode, will be used  as  a verification tool on select samples,
                                                                                                                ^d o ?d en
                                                                                                                u> p> OP a>
                                                                                                                tQ rt  2! 0
                                                                                                                ^ t-h O •
                                                                                                                  ft •  ••
                                                                                                                      Ul
                                                                                                                    o dd

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                                                           Section  No.:   5B
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    (2)   Instrument Performance:  Each instrument used in  this project  will be
         checked on each day that samples are analyzed to  demonstrate performance.
         One of the QA objectives is that the absolute instrument response  (e.g.,
         area counts/ng injected for the internal standard(s) and/or surrogates  in  a
         GC/MS analysis) can be within 50% of the value of comparable measurements
         made subsequent to the most recent calibration of the instrument.

    (3)   Recovery of Arochlor 1260 and PCP;  The recovery  of Arochlor  1260  and  PCP
         will be defined as follows:

         _             (ug P found in spiked sample  - |ag P in native sample)  v  . nn
         Recovery, % = -U—?	*•	^	r^—;—*.— -'*	;	—	 X  100
                *                        ng P added  to sample
b.  Precision
    Precision is defined in QAMS-005-80 as a measure of mutual agreement among  indi-
    vidual measurements of the sample property.  For this  project,  the  QA objectives
    for precision are expressed in terms of the following  parameters:

    (1)   Analysis of Standards:  One of the QA objectives  for this  project  is that
         the correlation coefficient for each calibration  curve, including  all  data
         points for standards analyzed subsequent to the most recent recalibration
         of the instrument, should be >0.90.

    (2)   Analysis of Surrogates:  Another QA objective for this project is  that  the
         standard deviation for analysis of surrogate compounds in  replicate  samples
         from a given waste stream be within the limits specified in Table  2.

    (3)   Analysis of Replicate Samples:   A final QA objective is that the results of
         directed analysis of laboratory replicate samples (i.e., replicate samples
         drawn from the same field composite sample) be within the  limits specified
         in Table 2,  when at least three replicate samples are analyzed.  At  least
         10% of all analyses performed will be duplicate QA checks.

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c.   Completeness
    The QA objective for this program is to obtain  analytical  results  for  at least
    95 percent of the samples collected during this program.

d.   Representativeness
    The following factors are addressed elsewhere in  this  trial  burn plan
    (Sections III and IV) in order to ensure as much  as possible a  representative
    sample:  sampling sites, process cycles, catch  flow rates  (sampling frequency),
    sample preservation, and sampling procedures and  equipment.

e.   Comparabili ty
    All data will be reported in mg, ug or ng of analyte per kilogram,  liter,  or
    cubic meter of original sample.  When precise recovery values for  a given com-
    ponent are known, the recovery information and  the corrected concentration data
    will also be provided.

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                                                            Section No. ;   6B
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6. OB Sampling Procedures
a.  Sample Collection
    Sample locations and numbers of samples  for  soil  (spiked with Arochlor 1260 and
    PCP feed), diesel fuel, makeup water, kiln ash, purge water,  alkaline scrubber
    solutions, and CHEAP filter ash are detailed in Table  3.

b.  Modified Method.5 (MM5) Sampling
    ITAS recognizes the value of conducting  modified  method  5 (MM5)  sampling with
    the same train configuration which has been  employed for  previous  performance
    tests' on this mobile inicnerator.  The MM5 train  illustrated  in  Fig.  4 will be
    utilized for the collection of stack gas samples.

c.  Sorbent Trap Composition
    The front sorbent trap in the MM5 Train  (Fig. 4) will contain Florisil;  the
    backup sorbent trap will contain XAD-2 resin.

d.  Particulate Sampling
    Particulate sampling procedure will be in accordance with  the U.S. EPA par-
    ticulate method.

e.  HC1 Sampling
    HC1 samples will be collected by use of  a sodium hydroxide solution in the
    caustic scrubber traps of the MM5 Train  (Fig. 4).

-------
                                       Table  3.    Summary  of  Trial  Burn  Analytical Procedures
   Sample
       soil
  feed and PCP
Diesel fuel
Make-up water
Kiln ash
Purge water
Alkaline
  scrubber
  soluti on

CHEAP'
Stdck sample
Stack sample
  Sampling Method
   and Frequency
                                                      Number of Samples
                                                        Analyzed for
                                                        Tests 3 arid 2
                                                                                               Analysis
One composite sample
  per run (2 grabs)
                        One grab sample per
                          delivery/  composite
                          sample for one
                          analysis per lot

                        One sample per stage
                        One sample  per  DRE  test
                          (if any)
                        One composite  sample
                          per  DRE  run
Daily composite
   (1 hr grabs)

Weekly grabs

Weekly grabs

Weekly composite

One grab sample per batch
  Composite grab sample


One sample per DRE run



Modified Method 5

One sample per DRE run
   (three samples per test)
                        U.S.  EPA Method  5
                          (three samples per  test)
                        Gas bag,  one  per  run
 6

 6

 6

 2

 2


 1

 1

 3

 3

 3

 3

15


 2

 2

 2

 2



 3

 3

 3

 3


 3

 6
Organic Cl, density

Heat value, ash, moisture

Arochlor 1260 or PCP

Organic Cl

Density, ash, moisture,  heat value

Presence of Arochlor 1260, PCP
Presence of Arochlor 1260

Presence of PCP

Presence of PCP

Presence of Arochlor 1260

Presence of Arochlor 1260

Presence of PCP

Total organic carbon,  pH,  temperature


Total suspended solids

Total dissolved solids

PCBs, PCP

PCBs, PCP



Presence of Aroohlor 1260

Presence of PCP

Arochlor 1260 emission rate

PCP emission rate


I1C1 emission rate**

Particulate emission rate
                                                           02 ,  co2
                                                                                                                                           Analytical  Method
Standard method (where appropriate)

Standard method (where appropriate)

GC/EC or GC/MS

Standard method (where appropriate)

Standard method (where appropriate)

Extraction, concentrate, GC/EC or GC/MS
Extraction, concentrate, GC/EC*

Extraction, concentrate, GC/MS*

Extraction, concentrate, GC/EC*

Extraction, concentrate, GC/MS

Extraction, concentrate, GC/EC*

Extraction, concentrate, GC/MS

Standard methods (where  appropriate)
Extraction, concentrate,  GC/EC*

Extraction, concentrate,  GC/EC*



Extraction, concentrate,  GC/EC*

Extraction, concentrate,  GC/MS

Extraction, concentrate,  GC/EC*

Extraction, concentrate,  GC/MS


Scrubbing, Standard Method  325.3

EPA Particulate Method 5
 'Positive results  confirmed by GC/MS.
*«PCB runs will not be analyzed for  I1C1 since HC1 emission rate
  will be <4 Ib/hr
 [D  fU  CD  (D
uq  ft  <  O
 CD  (D  H-  rt-
    ••  ra  H-
 KJ     I-1-  O
       O  0
 OOP
 H)  H     2;
    P>  2!  O
 LO  Hi  O  •
    rt  •   ••
                                                                                                                                                                            O

-------
                                  FIGURE /|
                          ORGANIC SAMPLING TRAIN
   SENSOR
 ft
. LJw
                     HEATED AREA
 \  I  FAC*
___^y LJWALL
THERMOMETER

    FILTER HOLDER

                         HERMOCOUPLE WELL
          CONDENSER   '
        /          /80RBENT TRAPS
REVERSE TYf E
 mOTTUBC
         X
              -r
         ^1
                 3
           f ITOT MANOMETER



                 nECIHCULATION PUMP
                                                                        CHfCK
                                                                        VALVE
                  /
                                                                                        VACUUM LINE
                                KNOCK-OUT TRAPS
                                       THERMOMETERS
                           £_J (^ J av-fAss VALVE


                                       rt&i—^Q.
                                                v>«3-
                                                MAIN
                                               VALVE
                                                                                                  ~O O ZQ CO
                                                                                                  (D Q) CD CD
                                                                                                  iQ n- < o
                                                                                                  CD CD H- rt-
                                                                                                    -• 0) H-
                                                                                                      H- O
                                                                                                  u>

                                                                                                    O J _„
                                                                                                  O hi   2
                                                                                                  l-h pj 2 O
                                                                                                    Hi ° •
                                                                                                  co rt •
                                                                                                        en
                                                                                                      -  W
                                                                                                      o
                                      DRYGASM£TE«  AIR-TIGHT

-------
                                                            Section No.:   7B
                                                            Revision No.:   0
                                                            Date:   Draft
                                                            Page  1  of 6
7.OB Sample Custody
    The sample custody procedures to be used  for  this program conform to  the  guide-
    lines of SW-846, Section  2.0.  The Sampling Coordinator will be responsible  for
    sample custody in the field.

    The Quality Control and Data Manager will be  responsible  for acting as  the
    sample custodian at the ITAS laboratories.

a.  Field Chain-of-Custody
    Before collecting samples in the field, the sampling  coordinator will issue  num-
    bered sample tags to field  samplers  (Fig. 5).   Field  samplers  will  label  each
    sample collected, filling the appropriate information in  waterproof ink.  The
    cap of each container will  be sealed with a paper tape bearing the  sample
    number.  The field sampler  will be responsible  for  collecting  the samples and
    for logging the samples into assigned  field notebooks until they are  transferred
    to the sampling coordinator.  The sampling coordinator will acknowledge receipt
    of the samples from the field sampler  in  writing and  verify that chain-of-
    custody procedures have been followed.  He will then  transcribe the field sample
    information to the Chain-of-Custody record  (Fig. 6) and assign an ITAS  Labora-
    tory Number.  The original  of the Chain-of-Custody  record will remain with the
    sample at all times.  In addition, a sample analysis  request sheet  (Fig.  7)  will
    accompany sample.

b.  Transfer of Custody
    The sampling coordinator will transfer custody  of all samples  to the  analysis
    coordinator who will acknowledge receipt  on the Chain-of-Custody record.
    Samples which are to be shipped will be accompanied by the Chain-of-Custody
    records,  with appropriate signatures.

c.  Laboratory Custody Procedures
    The QC and Data Manager will immediately  acknowledge  receipt of sample  in

-------
                                     Section  No.   7B
                                     Revision No.  0
                                     Date:   Draft
                                     Page 2 of 6
         YORK RESEARCH CORP.
(  SAMPLE
    1.0.
      Figure 5. Sample Bottle Label
                                        IT ANALYTICAL SERVICES, IN(

-------
Date Sample Taken:

Time Sample Taken:
Person Taking Sample:

Sample Location:  	
Reason For Sampling:
                                    CHAIN OF CUSTODY FORM

                                IT Analytical Services, Inc.
                                Stewart Laboratories Division
                                                                Section No.  7B
                                                                Revision No.  0
                                                                Date:   Draft
                                                                Page  3 of  6
                             Sample Number:

                             IT Lab Number:
Other Related Samples (Taken by IT or other organization):
Type of Sample:

Container Size:
Liquid
Gas
 Sludge       Other  (specify):

	 Container  Type: 	
Quantity of Sample Taken:
Person whom results, original of this form and remaining sample should be returned  to:
SAMPLE TRANSFER
1
2
3
Relinquished by:
Received by:
Relinquished by:
Received by:
Relinquished by:
Received by:

(Name)
(Name)

(Name)
(Name)

(Name)
(Name)

(Organization)
(Organization)

(Organization)
(Organization)

(Organization)
(Organization)

(Date/Time)
(Date/ Time)

(Date/Time)
(Date/Time)

(Date/Time)
(Date/Time)
                     ORIGINAL MUST  BE  RETAINED  WITH  SAMPLE  AT  ALL  TIMES
                                           FIGURE 6

-------
                                                                Section No. 7B
                                                                Revision No.  0
                                                                Date:  Draft
                                                                Page  _4 of 6
                                   SAMPLE ANALYSIS REQUEST
Collector (s)
Company Affiliation:
IT Analytical Services, Inc.
Stewart Laboratories Division
5815 Middlebrook Pike
Knoxville, TN  37921
(615) 588-6401
Case Number
Location of Sampling:
Date 4 Time of Collection:
Collector's   Laboratory    Type of     Analysis
Sample No.    Sample No.    Sample      Requested
                                              -Field
                                              Information
Samples Received By

Comments
                           Title
                                                                          Date
                                           FIGURE  7
                                                                  IT  ANALYTICAL SERVICES, INC

-------
                                                       Section No. :   7B
                                                       Revision No.:   0
                                                       Date:  Draft
                                                       Page  5 of 6
writing.  She will verify  that  the  information  on  the  sample  tags  matches  the
information in the Chain-of-Custody records.  She  will then  log in all  samples
by previously assigned  laboratory identification numbers,  every sample  having a
unique, non-recurring laboratory number.   The log  notebook will include the
field number, date of receipt,  condition  of  sample when received,  a qualitative
description, the assigned  laboratory number, sample  preparation (spiking,  etc.),
sample distribution, and any  other  information  deemed  appropriate.   The QC and
Data Manager will be responsible for preparing  and introducing control  samples,
blanks, and check standards.

Samples will be kept in refrigerated storage when  not  being  analyzed.   Sample
distribution sheets  (Fig.  8), will  also accompany  the  samples.   The analysis
coordinator will be responsible for preparing the  sheets.

The analyst will be responsible for samples  during analysis  and for logging
laboratory analysis information.

-------
SAMPLE CATEGORY:


FROM:
       Name



SAMPLE PREPARATION:


TO:
       Name
SAMPLE NO.:
                                                         Section No.  7B
                                                         Revision No. 0
                                                         Date:   Draft
                                                         Page  6 of 6
                                                    Project Code
                           'SAMPLE DISTRIBUTION SHEET
Emp.No.       Signature
Emp.No.
Signature
                            Date
Name
ANALYSIS:
TO:
Name
STORAGE:
TO:
Emp.No. Signature , Date
i
Emp.No. Signature • Date
Cl
Date
                                    FIGURE  8
                                                            IT  ANALYTICAL SERVICES, INC

-------
                                                           Section No. :   8B
                                                           Revision No.:   0
                                                           Date:  Draft
                                                           Page  1 of  5
8.OB  Calibration Procedures and Frequency
a.  Sampling
    Calibration of stack sampling equipment will be performed within  two weeks pre-
    vious to initiation of field sampling.  The procedures will conform to  the spe-
    cifications of the EPA document, Quality Assurance Handbook for Air Pollution
    Measurement Systems, Volume III, Stationary Source Specific Methods  (von Lehmden
    £t ai., EPA-600/4-77-027b, January  1980).  Dry gas meters, nozzles, orifices,
    and pitot tubes will be covered in  the calibration.  Tables 4 and 5 summarize
    the methods to be used.

    The dipper (waste feds and scrubber water) and scoop (ash samples) require no
    calibration.

b.  Analytes

    (1)  Instrument Performance and Tune

         i.   At the outset of the analytical activity for this program, a  perfor-
              mance check on each instrument will be made to demonstrate compliance
              with manufacturer's specifications.

         ii.  Before analysis of each set of samples and on a daily basis during the
              analysis,  the instrument will be tuned to meet an operating perfor-
              mance standard.  The tuning criteria for the organic analyses are:

                   GC/MS               Federal Register, 12/3/79
                                       Method 625

                   GC/EC               ITAS-SOP

-------
                                                           Section No. SB
                                                           Revision No. 0
                                                           Date:  Draft
                                                           Page  2 of  5
Table  4
 ACTIVITY MATRIX FOR CALIBRATION OF EQUIPMENT
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Wet Test Meter
Capacity >_3.4 nr/h
(120 ft 3/h); accuracy
within ±1.0?i
Calibrate initially,
and then yearly
by liquid dis-
placement
Adjust until
specifications
are met, or
return to manu-
facturer
Dry gas meter
   = Y ±0.02 Y
Calibrate vs wet
test meter initially,
and when posttest
check exceeds
Y ±0.05 Y
Repair, or re-
place and then
recalibrate
Thermometers
Impinger thermometer
±1°C (2°F); dry gas
meter thermometer
±3°C (5.4°F)'. gver
range; stack tempera-
ture sensor ±1,5% of
absolute temperature
Calibrate each ini-
tially as a separate
component against a
mercury-in-glass
thermometer; then
before each field
trip compare each as
part of the train
with the mercury-in-
glass thermometer
Adjust; de-
termine a con-
stant correc-
tion factor;
or reject
Probe heating
  system
Capable of maintaining
120° ±14°C (248° ±  >
25°F) at a flow rate of
20£/min (0.71 ft3/min)
Calibrate component
initially by
APTD-0576; if con-
structed by APTD-
0581, or use
published calibra-
tion curves
Repair, or re-
place and then
reverify the
calibration
Barometer
±2.5mm (Q.I in.) Hg of
mercury-in-glass barom-
eter
Calibrate initially
vs mercury-in-glass
barometer; check
before and after
field test
Adjust to
agree with a
certified
barometer
Probe nozzle
Average of three ID
measurements of nozzle;
difference between high
and low _<0.1 mm
(0.004 in".)
Use a micrometer to
measure to near-
est 0.025 mm  (0.001
in.)
Recalibrate,
reshape, and
sharpen when
nozzle becomes
nicked, dented,
or corroded
(continued)
                                           IT  ANALYTICAL  SERVICES,  INC.

-------
                                                           Section No. SB
                                                           Revision No. 0
                                                           Date:    Draft
                                                           Page 3 of 5
Table 4  (continued)
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Analytical
  balance
± mg of Class-S
weights
Check with Class-S     Adjust or
weights upon receipt   repair
Source:   EPA-600/4-77-027b
                                                           IT ANALYTICAL SERVICES,  INC

-------
                                                           Section No.   8B
                                                           Revision No.  0
                                                           Date:   Draft
                                                           Page  4 of 5
Table  5
ACTIVITY MATRIX FOR CALIBRATION OF APPARATUS


Apparatus
Type S pitot
tube and/or
probe
assembly






Stack gas tem-
perature
measurement
system





Barometer



Differential
pressure
gauge (does
not include
inclined
manometers)





Acceptance limits
All dimension speci-
fications met, or
calibrate according
to Sec 3.1.2, and
mount in an interfer-
ence free manner




Capable of measuring
within 1.5% of minimum
stack temperfture
(absolute)





Agrees within 2.5 mm
(0.1 in.) Hg of
mercury-in-glass
barometer
Agree within ±5% of
inclined manometers








Frequency and method
of measurement
When purchased, use
method in Sees 3.1.1
and 3.1.2; visually
inspect after each
field test





When purchased and
after each field
test, calibrate
against ASTM 3C or





Initially and after
every field use,
compare to a liquid-
in-glass barometer
Initially and after
each field use







Action if
requirements
are not met
Do not use
pitot tubes
that do not
meet face
opening
specifica-
tions; re-
pair or re-
place as re-
quired
Adjust to
agree with Hg
bulb thermom-
eter, or con-
struct a cal-
ibration
curve 'to cor-
rect the
readings
Adjust, re-
pair, or
discard

Reject test
results, or
consult
administra-
tor if post-
test calibra-
tion is out
of specifi-
cation
                                                            IT  ANALYTICAL  SERVICE'S,  INC.

-------
                                                       Section No. :   8B
                                                       Revision No. :   0
                                                       Date:  Draft
                                                       Page  5 of 5
     iii.  For directed analysis of Arochlor 1260 and PCP the daily performance
          check will iclude analysis of at least one blank and one standard
          prior to analysis of samples.

     iv.   The absolute instrument response to the internal standard  (if any)
          will be noted at the completion of each sample analysis.  A variation
          of >±50% will be a signal for recalibration/retune.

(2)   Calibration Curve
     .For  directed analyses of Arochlor 1260, PCP, and HCE,  the GC/EC and GC/MS
     analysis procedures will be calibrated before the anaysis of each batch of
     samples by analyzing known mixtures of the group of test compounds under
     study at at least three concentration levels.  Any tendency for the
     calibration curve to drift will be monitored by reanalyzing at least one of
     the  standards daily.   A new calibration curve will be established if the
     response observed in the reanalysis of the standard varies by ±20% from
     that predicted from the previous calibration curve.

-------
                                                           Section No. :   9B
                                                           Revision No. :   0
                                                           Date:  Draft
                                                           Page  1 of  2

9.OB  Analytical Procedures
    The analytical procedures to be used in this program are given in Section VI of
    this trial burn plan.

    A general description of the analytical methodology is listed below:

a.   Quantitation of Arochlor 1260 by Gas Chromatography/Electron Capture  (GC/EC)
    Because of the low level (40 to 49 ug/g) of Arochlor 1260 in the  soil  to be used
    in this test and the predicted destruction efficiency  (>99.99%),  the  only prac-
    tical detection device for the quantitation of the Arochlor  1260 pattern is the
    electron capture detector which is more sensitive that the GC/MS.  Samples and
    extracts representing discrete MM5 sampling train components will be  analyzed by
    GC/EC followed by compositing them together and further extract concentration
    and re-analysis by GC/EC.  If the resulting concentration level is adequate, the
    concentrated composit extract will be analyzed by GC/MS using the selected ion
    monitoring mode for some of the discrete Arochlor 1260 isomers.

b.   Quantitation of Pentachlorophenol by GC/MS
    The analysis of pentachlorophenol will be performed using Method  8250, "GC/MS
    Method for Semivolatile Organics: Packed Column Technique," Test Methods for
    Evaluating Solid Waste, July 1982, SW-846, Second Edition.

c.   Sorbent Extraction Procedure
    ITAS will employ an ultrasonic assisted desorption procedure for  all  sorbent
    samples.

d.   Analysis of Particulate for Arochlor 1260 and PCP
    The filter will be extracted by an ultrasonic assisted desorption procedure
    using hexane.   This extract will be analyzed for Arochlor 1260 or PCP.

-------
                                                            Section No.:   9B
                                                            Revision No.:   0
                                                            Date:   Draft
                                                            Page  2 of 2


e.  Chloride Analysis

    Impingers from the Modified Method 5 train, water  rinse of these impingers,  and

    scrubber water samples will be analyzed for chloride by EPA  Method 325.3.

    Chloride results will be confirmed by use of ion chromatography.

-------
                                                            Section No.:   1 OB
                                                            Revision No.:   0
                                                            Date:   Draft
                                                            Page  1  of 10

10.OB  Data Reduction, Validation, and Reportings

a.  Data Reduction
    Raw data for the directed quantitative analysis procedure  to be used  in this
    project (GC/MS) will consist of peak areas  of  characteristic ions  for the  analy-
    tes of concern.  Raw data will be converted to concentrations  by use  of a
    calibration curve that related peak area to the quantity of analyte introduced
    into the instrument.  A calibration curve for  each  analyte/analytical method
    will be constructed by fitting the results  of  the analyses of  calibration  stan-
    dard solutions containing the analyte at three different concentration  levels.

    The raw data will usually be converted to concentration of analyte  in the  sample
    by software in our Finnigan Incos Laboratory Data System or by the  analyst.
    Peak areas for the series of known calibration standards are first  entered and a
    regression line is computed.  A plot of the calibration curve  with  the  actual
    calibration data superimposed on it is immediately  generated on a high  speed
    printer/plotter for examination.  Peak areas from the  analyses of unknowns are
    then entered, corresponding quantities of analyte are  computed from the
    regression line, and a summary of the raw and  converted data is printed.   The
    original copy of the data summary will be included  in  the  project work  file and
    be received by the Program Manager.

    Raw data for the GC/EC quantitative analysis procedure to  be used  in  this  pro-
    ject will consist of peak heights.  Raw data will be converted to  concentrations
    by use of response factors that relate peak height  to  the  ten  quantity  of
    analyte introduced into the instrument after the response  of standards  have been
    shown to be linear by developing three-point calibration curves.  A minimum of
    two standard checks will be run during each shift  (at  beginning and end of
    shift) to assure that response is within  10% of  calibration  curve.  See
    Section 13 of the appended ITAS-Stewart Labs Div. SOP  for  details.

-------
                                                            Section No.:   1 OB
                                                            Revision  No.:   0
                                                            Date:  Draft
                                                            Page  2 of 10

    As the possibility exists that incineration and sample  collection  and recovery
    techniques could cause alteration of Arochlor patterns, the  major  peaks in  the
    Arochlor 1260 pattern will be quantitated; and both  the average  value and
    highest value will be reported.

b.  GC/MS Analyses
    An internal standard  (such as d-\ g-anthracene) will be added  to each standard
    solution or concentrated sample extract immediately  before analysis.   The quan-
    tity added will be sufficient to give the same concentration (pg/mL)  of internal
    standard in all solutions/extracts analyzed.

    The calibration curve will be based on the response  factor  (RF)  where:

                   RF = (AsCis)/(AisCg)

    Where:

         A_  = Response for the parameter to be measured
          s

         AJ _ = Response for the internal standards
          J. o

         Cj_ = Concentration of the internal standard in Mg/1

         GS  = Concentration of the compound to be measured in pg/l

    If the RF value over the working range is constant  (less than 20%  relative  stan-
    dard deviation), the RF can be assumed to be invariant  and the average RF can be
    used for calculations.  Alternatively, the results can  be used to  plot a
    calibration curve of response ratios, Ag/Aj_s, against RF.

-------
                                                        Section  No. :   1 OB
                                                        Revision No.:   0
                                                        Date:  Draft
                                                        Page  3 of 10
The concentration of analyte or surrogate in  an unknown  sample  will  be  calcu-
lated as follows:


     Concentration in Extract, C*  (ng/uL)
               C*  (ng/pL) = As'Cis
                            Ais.RF
Where:
     As  = Response for the parameter to be measured


         = Response for the internal standards
      J0
      J.O
      J_ = Concentration of the internal standard  in  ng/yl
      .L5
     RF  = Response factor for the parameter  to be measured.


     Concentration in Sample, C  (mg/L or mg/kg)


     C is calculated from C*; the volume of the concentrated  sample  extract,  Vx;
     and the initial quantity of sample extracted.


     For awueous liquids, organics liquids, slurries:


               C (mg/L) = C*-VX * 100Q


     For solids, sludges:
                            W
                             s

-------
                                                           Section  No.:   1 OB
                                                           Revision No.:   0
                                                           Date:  Draft
                                                           Page  4 of 10
         Where:
              C* = Concentration in extract, ng/jjL =  ug/mL

              Vv = Volume of concentrated extract, mL
               A

              Vg = Volume of sample taken for extraction, L

              Ws = Weight of sample taken for extraction, kg

c.  Data Validation
    The principal criteria that will be used to validate the data  integrity  during
    collection and reporting of data are:

    (1)  Verification on a weekly basis by the QC and Data Manager that  all  raw  data
         generated in the preceding week have been stored on magnetic  tape and/or in
         hard copy and that storage locations have been documented in  the laboratory
         chain-of-custody records.

    (2)  Examination of at least 5% of the raw data  (e.g. chromatograms, AAS
         recorder outputs) on a weekly basis by the analysis coordinator to  verify
         adequacy of documentation, confirm peak shape and resolution  assure  that
         automatic integrator was sensing peaks appropriately, etc.

    (3)  Confirmation that raw areas for internal standards and calibration  stan-
         dards are within 50% of expected values  (see Section  5B).

    (4)  Reporting of all associated blank, standard, and QC data  along  with  results
         for analyses of each batch of samples.

-------
                                                           Section  No.:   1 OB
                                                           Revision No. :   0
                                                           Date:  Draft
                                                           Page  5 of 10

    (5)   Reporting of all analytical data for samples with no  values rejected  as
         outliers, because of the small number of replicate samples for analysis.

d.  Reporting
    Results of directed analysis, survey analysis and proximate  analysis  will  be
    reported in the formats illustrated by Figs. 9 through 13.

    Reports shall include documentation as outlined  in Appendix  2.   Protocol for
    Sample Analysis Reports.

-------
                                                       Section  No.  10B
                                                       Revision Mo.   0
                                                       Date:  Draft
                                                       Page  6 of 10
                  GC/MS DIRECTED ANALYSIS  REPORT  FORM
Contractor
Analyst Responsible

Instrument
             Date
Analysis Method

Column
Column Temo.
Preparation Method
                       Sample ID No.
Compound Identified

Surrogate
Concentration, yg/L(kg)
Corrected
Data

Recovery
Factor

Uncorrected
Data

Percent Recovery
                                Fig.  9

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                                                       Section No.  ]_QB
                                                       Revision No.  0
                                                       Date:   Draft
                                                       Page  7  of  10
                            MAJOR COMPONENTS

                        GC/MS SURVEY REPORT FORM
Contractor
Sample ID Number
Sample Description
Analyst Responsible

Instrument	

Column
  Date Analyzed_
 Time
GC Temperature Program_

Observations
Results:
     Compound
    Identified
         Peak   Rel.
             Intensity
RRT.
Goodness of
Fit Criterion
                  Fig. 10.  GC/MS Survey Report  Form

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                                                        Section No.  10B
                                                        Revision No.  0
                                                        Date:   Draft
                                                        Pacre  8 of 10
                MASS SPECTROMETRIC SURVEY ANALYSIS REPORT
Contractor
Sample ID Number
Sample Description
Analyst Responsible_

Instrument
Date Analyzed_
Time
Observations
Results

Major Categories, Subcategories, Specific Compounds:
Intensity





Category





MV Range





                        Fig. 11.  LRMS Analysis  Report

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                                                                  Section  No.  10B
                                                                  Revision No.  0
                                                                  Date:  Draft
                                                                  Page 9 of 10
         IT CORPORATION
                                         STEWART LABORATORIES DIVISION
                                      CERTIFICATE OF ANALYSIS
TO:
                            DATE REPORTED:

                            CODE:
                                                 ORDER  No.:
SAMPLE  DESCRIPTION:
CONCENTRATION UNITS ARE
ITAS  Samole No.
Identification
  Aroclor
    1242
and/or 1016
Aroclor
  1254
Aroclor
  1260
 Total
Aroclors
Sworn  to and subscribed before  me this

day  of 	
                                   IT ANALYTICAL SERVICES,  INC.
               NOTARY PUBLIC

My  commission expires 	
                                   By
                                       Subsidiary of IT Corporation
                IT Analytical Services • 5815 Middlebrooic Pike • Knoxviile. Tennessee 37921 • 615-583-6401
                  .  12.
                                               RGB Report Form

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Sample
                                                      Analyst or
Moisture,  Solids,  Ash  Content            %           Laboratory                     Date
      Moisture
      Solids
      Ash


Elemental  Composition

      Carbon
      Nitrogen
      Sulfur
      Phosphorus
      Fluorine
      Chlorine
      Bromine
      Iodine

Total Organic Carbon

Total Organic Halogens
                                                                                                         Tl O IX) CO
                                                                                                         (U (U (D  (D
                                                                                                         CIQ rr <  O
                                                                                                         (D fU H- rr
                                                                                                           •• W  H-
                                                                                                         (-<   H- O
                                                                                                         O   00
                                                                                                           a 3
                                                                                                         O ht    25
                                                                                                         Hi P) & O

                               Fig.  13.   Proximate Analysis  Reporting Form                              (-. ^ °
                                                                                                         O      M
                                                                                                                O
                                                                                                             O M

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                                                            Section  No.:   11B
                                                            Revision No.:   0
                                                            Date:  Draft
                                                            Page  1 of 2
11.OB  Internal Quality Control Checks
    Section 5B specifies the guidelines for number and frequency  of  replicate  and
    spiked QC samples and calibration standards to be used  in  the project,  including
    identity and concentration of surrogate spike compounds  to be added  to  each
    designated sample.

    Quality control samples will be analyzed in the same way as field  samples  and
    interspersed with the field samples.  The results of analyzing these samples
    will be used to document the validity of data and to control  the quality of data
    within predetermined tolerance limits  (see Section 5B).  QC samples  are as
    follows.

a.  Blank Samples
    These samples are analyzed in order to assess possible  contamination from  the
    field and/or laboratory, so that corrective measures may be taken, if necessary.
    Blank samples include:

      •  Field Blanks - These blank samples are exposed to  field  and sampling  con-
         ditions, and analyzed in order to assess possible  contamination from  the
         field (one for each type of sample preparation).
      *  Method Blanks - These blank samples are prepared in the  laboratory and are
         analyzed in order to assess possible laboratory contamination (one for each
         lot of samples analyzed).
      •  Reagent and Solvent Blanks - These blanks are prepared in the laboratory
         and analyzed in order to determine the backgound of each of the reagents or
         solvents used in an analysis  (one for each new lot number of  solvent  or
         reagent used).
b.  Analytical Replicates
    Replicate analyses of specific samples may be undertaken by the  analyst to check
    on the validity of certain analogous samples.  For example, if the internal
    standard response for a specific sample changes drastically from its prior

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                                                        Section No.:   11B
                                                        Revision No.:   0
                                                        Date:   Draft
                                                        Page  2 of 2
value, a problem could be present in the  instrument  or  in the  sample workup.
Repeat analyses of the sample in question and  a previous  "normal"  sample will
serve to indicate which of the possible problems  is,  in fact,  present.

Spiked Samples
All samples will be spiked with one or more selected surrogate compounds before
extraction and analysis.  The data on surrogate concentration  will be used to
calculate the recovery of the surrogate compounds  as one  measure of the  accuracy
of the sample preparation and analysis procedures.

For direct analysis of Arochlor 1260 or PGP, one  sample from each  set of three
replicates will be spiked with the analyte interest  at  a  concentration of 100 to
1000 ppm.  Depending on the concentration of analyte in the unspiked sample,
these data may provide an estimate of the recovery of the species  of interest
from the sample matrix.  A spiked blank sample for each method will also be ana-
lyzed in order to assess the inherent accuracy of  an analytical method.

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                                                           Section No.:   1 2B
                                                           Revision  No. :   0
                                                           Date:  Draft
                                                           Page  1 of 1

12.OB  Performance and System Audits

    A system audit by the Program Manager and the Quality Control and  Data  Manager
    will be made before the implementation of any new experimental procedures  in our
    labortories.

    System audits in this program will largely consist of a weekly review of all
    recent data to ensure that all required QC checks are being  made and  evaluation
    criteria followed.  The Quality Control and Data Manager will participate  in
    these reviews on at least a monthly basis.  Because of the anticipated  dif-
    ficulty in obtaining reference samples with matrices similar to  the waste
    samples we will be analyzing, performance audits will rely heavily on the  repli-
    cate analyses of real samples, spiked and unspiked.  However, we will be alert
    to opportunities to use standard reference materials as a means  of auditing
    performance.

    During the course of systems audits, the Quality Control and Data  Manager  will
    remain sensitive to the possible need for additional peer review of one or
    another aspect of the program, and she will suggest the inclusion  of  other
    appropriate ITAS staff in the audit process whenever necessary.

    In addition, ITAS will participate in the analysis of audit  samples supplied by
    the Trial Burn QA Coordinator and control agencies or their  representatives.

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                                                           Section No.:   13B
                                                           Revision  No.:   0
                                                           Date:  Draft
                                                           Page  1 of 1

13.OB  Preventive Maintenance

    The hardware associated with the GC/MS/DS and GC/EC systems  used for  analyses
    require very little in the way of regularly scheduled preventive maintenance.
    Chromatographic carrier gas purification traps and injector  septa are replaced
    on a regular basis.  The pump seals need to be replaced more or  less  frequently
    depending on the types of solvents employed.

    Most maintenance, however, such as column replacement, detector  cleaning,  source
    cleaning, filament replacement, etc. , must be performed on an as-needed basis
    when performance begins to degrade as evidence by degradation of peak resolu-
    tion, decreased ion sensitivity, shift in calibration curves, or failure to meet
    one or another of the QC check criteria.

    Adequate supplies of spares including GC columns, septa,  syringes, and  MS  fila-
    ments and separators are maintained so that they are available when needed.

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                                                            Section No. :   1 4B
                                                            Revision No. :   0
                                                            Date:   Draft
                                                            Page  1  of 2

14. OB  Specific Routine Procedures Used to Assess Data  Precision,
       Accuracy and Completeness

a.   Calculation of mean values and estimates of precision
    The mean, C of a series of replicate measurements of concentration,  Cj_,  for a
    given surrogate compound or analyte will be calculated  as:
                                 n
                        C =  J_   Z
                             n   i
    where n = number of replicate measurements; C, Cj_  are  both  in mg/L or mg/kg.

    The estimate of precision of a series of replicate measurements  will usually  be
    expressed as the relative standard deviation, RSD:
                        RSD     SD    X  100%
    where SD = Standard deviation
                                       n
                        SD =           E     (Cj_  - C)
                                     i =  1
                                            (n  =  1)
    Alternatively,' for the data sets with a small  number  of  points  (e.g.  concentra-
    tion of pesticide in duplicate samples of  one  waste stream),  the estimate of
    precision may be expressed as a range per  cent,  R:

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                                                           Section No.:   1 4B
                                                           Revision No. :   0
                                                           Date:  Draft
                                                           Page  2 of   2
                        R =   C1 - C2            X  100%
    where C-j = highest concentration value measured in data set
          C2 = lowest concentration value measured in data set


    The standard deviations calculated will be compared on a weekly basis with  the

    respective goals identified in Section 5B.
b.  Assessment of Accuracy
    Accuracy will be evaluated by comparing the mean recovery of surrogate  compounds
    on a weekly basis against the goals identified in Section 5B.  The recovery of a
    surrogate compound will be defined as:
                            C  . V   (or W  )   X 100
              Recovery, % =  s    s	s_
                               ~tr
    where C  = measured concentration of surrogate compound in sample, mg/L  (or
              V  (W ) = Total volume  (or weight) of sample to which surrogate was
               S   S
                        added, L  (or kg)
              Q  = Quantity of surrogate compound added to  sample, mg.
               5

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                                                           Section No.:   15B
                                                           Revision No.:   0
                                                           Date:  Draft
                                                           Page  1 of  2

15.OB  Corrective Action

    For each analytical method employed in this program we will  regularly  track  pre-
    cision and accuracy by computing the standard deviation or range  of  the results
    of replicate analyses.  We will make periodic determinations of recovery  of  the
    surrogates.  The mean recovery and the standard deviation of the  replicate set
    will be computed.  These data will be accumulated for each kind of sample matrix
    analyzed, e.g., solid, stack gas sample, aqueous liquid, ash.  These statistics
    will be updated from lot to lot as additional analyses are geing  performed and
    more experience is gained.  When either the relative standard deviation of
    replicate results, the average recovery, or the relative standard deviation  of
    replicate recoveries exceeds twice the most recently updated acutal  values for
    those statistics or the performance goals, whichever is more stringent, correc-
    tive action will be taken to improve performance before analyses  of  the next
    lot.

    If during system or performance audits, weaknesses or problems are uncovered,
    corrective action will obviously be initiated immediately.

    Corrective action will include, but not necessarily be limited to:   recalibra-
    tion of instruments using freshly prepared calibration standards;  replacement of
    lots of solvent or other reagents that give unacceptable blank values;  addi-
    tional training of laboratory personnel in correct implementation of sample  pre-
    paration and analysis methods; and reassignment of personnel, if  necessary,  to
    improve the overlap between operator skills and method requirements.

    Whenever a long-term corrective action* is necessary to eliminate the  cause  of
    nonconformance, the following closed-loop corrective action  system* will  be
    used.   As appropriate the sample coordinator, analysis coordinator,  or the
    program manager will ensure that each of these steps are followed:

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                                                       Section No.:   15B
                                                       Revision No.:   0
                                                       Date:  Draft
                                                       Page 2 of 2
     The problem will be defined
     Responsibility for investigating the problem will be assigned
     The cause of the problem will be investigated and determined
     A corrective action to eliminate the problem will be determined
     Responsibility for implementing the corrective action will be assigned
     and accepted
     The effectiveness of the corrective action will be established and the
     correction implemented
     The fact that the corrective action has eliminated the problem will be
     verified
*"Quality Assurance Handbook for Air Pollution Measurement Systems - Volume
 Principles," EPA-600/4-76-005,  January 1976.

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                                                           Section No.:   16B
                                                           Revision No.:   0
                                                           Date:  Draft
                                                           Page  1 of  1

1 6B.   Quality Assurance Reports

    a.   Quality Assurance Reports to Management
         The Program Manager, the Quality Control and Data Manager, and the Sampling
         Coordinator and the laboratory task leaders, meet on a  regular basis  to
         assure that all QA/QC practices are being carried out and to  review
         possible or potential problem areas.  It is important that all data anoma-
         lies be investigated to assure that they are not a result of  operator  or
         instrument deviation but are a true reflection of the methodology or  task
         function.

         The Quality Control and Data Manager documents the results of  blind spikes
         and performance standards in a. central logbook which is also  reviewed
         periodically with the program manager.

    b.   Quality Assurance Reports to the EPA
         The final report will contain a separate section or statement  that covers
         the data quality and validity.  At a minimum, the following information
         will be covered:

           •  Assessment of measurement data precision, accuracy, and  completeness
           •  Performance audit results
           •  System audit results
           •  Significant OA problems and recommended solutions

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         APPENDIX 1

STANDARD OPERATING PROCEDURE
    FOR ANALYSIS OF PCBs

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I.   Scope  and Application

l.L  This  method covers  the determination of polychlorinaced biphenyls

     (PCB's)  and certain organochlorine.  pesticides,  including  some  deg-

     radation products  and related  compounds in  all  vater  matrices  —

     i.e., drinking water, raw source water, wastewater  and  industrial

     effluents.  The following PCB's may be determined by  this method:
                    Aroclor
                           (R)
                       1016
                       1221
                       1232
                       1242
                       1243
                       1254
                       1260
                       1262
              EPA Storet No.

                  34671
                  39438
                  39492
                  39496
                  39500
                  39504
                  39503
      Additional  specific compounds which may be determined by  this method

      include:
      Parameter

      Aldrin
      a-3HC
      b-BHC
      d-BHC
      g-BHC
      Captan
      Carbophcnothion
      Chlordane
      4,4'-ODO
Storet No.
Parameter
Storet N'o
39330
39337
39338
39259
39340
39640


39350
39310
Endosulfan II
Endosulfan Sulfate
Endrin
Endrin Aldehyde
Heptachlor
Heptachlor Epoxide
T ff f\f^ r"^ *"i
LSOC L .. n
Methoxychlor
Mirex
34356
34351
39390
34366
39410
39420
39430

39430
39755
                               (continued)
                                   41
                          revised  1/30

                      Stewart Laboratories,  lac.
                      Knoxvllle, Tennessee  37921

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    Parameter           Storat Mo.     Parameter              Scorec !'o.

    4,4'-DDE              39320        PCS 3                     39029
    4,4'-DDT              39300        Perchane                 39034
    Dichloran             	        Strobane                 	
    Dicofol               39730        Toxaphene                39400
    Dieldrin              39330        Trifluralin              39030
    Endosulfan I          34361

1.2  This tnechod is. applicable  to  Che detaminacion of .chose compounds

    specified above  in municipal  and industrial discharges.   It is  de-

    signed  co be  used co  meeC  Che monicoring requiremencs of  the" National

    Pollutant Discharge Elimination System  (NPDES).  As  such,'it pre-

     supposes  a high  expectation of finding  the  specific  compounds  of

     interest.  When  screening  samples  for any or  all of  the compounds

     above,  independent  protocols for verifying  the identity of  che com-

     pounds must  be applied.

 1.3  The limit of detection for this method is usually  dependent upon

     Che level of interferences rather  than instrumental  limitations.

     Under favorable circumstances, the method- sensitivity is  0.05  yg/1

     (for Aroclors ^  1016, 1221, 1232, 1242 and 1248) and 0.10 ug/1

     (for Aroclors ^  1254, 1260 and 1262) when analyzing a 1 liter

     sample with  Che electron  capture detector.   The limits of detection

     listed in Table 1 represent  the limits for organochlorine pescicides

     Chat can be  achieved in wascewaters  in che absence of interferences.

 1.4  When PC3's and/or organochlorine pesticides exist as complex mixtures,

     the  individual  compounds  are frequently difficult to distinguish.

     High,  low, or otherwise unreliable results may be obtained chrough

     misidencificacion and/or  one compound  obscuring another  of lesser

     concentration.  Provisions  incorporated in  this mechod are intended

      Co minimize  che occurrence of such incerferences.   Nevertheless,

      chis sechod  is  recocsended for use only by  experienced residue ana-

      lyses  or under, che  close  supervision of  such persons.

                                  42           Sceuart Laboratories, Inc.
                                               Knbxville, Tennessee 37921

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2.   Applicable Docunents

2.L  US EPA Method 617  — "Organochlorine Pesticides and PCE's", Interim

     Pending Issuance of  Methods for Organic Analysis of Water and Wastes,

     EMSL, Cincinnati,  OH 45268.

2.2  National Pollutant Discharge Elimination System (NPDES) References:

     Federal Register, -38., No. 125, Pt. II, (1973).  "Method for Organo-
     chlorine Pesticides in Industrial Effluents  (11/28/73)".

     Federal Register, M.., No. 232, Pt. II, (1976_) .

     Federal  Register, 44_, No. 233, Pt. Ill,  (1979).

     Federal  Register, 44_, No.  244, Pt. IV,  (1979).

 3.  Sucnarv of  Method  (1)

 3.1 A L-liter saaple  of wastewater  is  extracted  with  15%  methylene

      chloride in hexane  using separatory  funnel techniques.   The extract

      is dried and concp^-frated to a volume of 10  nl or less.   Gas chroaatro-

      graphic  conditions  are  described which allow for  the accurate measure-

      ment of  the coapounds in the extract.  An electron capture detector

      or a halogen specific detector (tnicrocoulometric  or conductivity) is

      used for quantification.

 3.2  The method  incorporates selected general purpose cleanup  procedures

       to aid  the  analyst in the elimination of interferences.

 4.  Interferences

 4.1   Solvents,  reagents, glassware, and  other  saaple  processing hardware

       may  yield  discrete artifacts and/or elevated  baselines causing mis-

       interpretation of  gas chrooacograms.  All of  these materials must

       be demonstrated  to be  free  frca  interferences under  the  conditions

       of the  test by analyzing method  blanks.  Specific selection of  re-

       agents  ar.d purification of  solvents by  distillation in all-glass

       systems cay be required.

                                   43           Stewart Laboratories,  Inc.
                                                Knoxville, Tennessee 37921

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4.2  Interferences  coextracted  from  the  samples will vary considerably

     froa source to source,  depending upon  the diversity of*the  indus-

     trial complex  or municipality being sampled.  While general cleanup

     techniques are incorporated inco  this  method, unique samples may

     require additional cleanup approaches  to  achieve  the detection linits

     listed in Table 1."

4.3  Glassware must be scrupulously clean.   Clean all  glassware as soon

     as  possible after use by rinsing with the last  solvent used.  This

     should be  followed by detergent washing (7-X-O-Matic)  in hot water.

     Rinse with tap water, distilled-water, acetone, and finally, pesti-

     cide quality  hexane.  Heavily contaminated glassware may require

     treatment  in  a muffle  furnace at 400 C for 15 to 30 minutes.  Some

     high boiling  materials, such as PCB's, may not be eliminated by

     this treatment.   Volumetric  ware should not be heated in a  muffle

      furnace.   Glassware  should be  stored  immediately after drying or

     cooling  to prevent any accumulation or dust or other contaminants.

      Store  inverted  or capped  with  aluminum foil.

 4.4  Interferences by phthalate esters  can pose  a major problem in PCS

      and pesticide analysis.   These materials elute in all fractions

      of the florisil cleanup.   They usually can  be minimized  by avoiding

      contact with  any plastic  materials.   The contamination  from phthal-

      ata esters can be completely eliminated  with the use  of  a microcoulo-

      aetric or electrolytic conductivity detector.

 4.5  Elemental sulfur nay interfere with the  determination of PC3's  and

      orsanochLorine pesticides when the electron capture detector is used.

                                   44           Stewart Laboratories, Inc.
                                               Knoxville,  Tennessee  37921

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5.   Apparatus  and  >taterials

5.1  Sampling  equipment,  for discrete or composite sampling.

5.1.1  Discrete samples — Amber glass bottles,  (1-liter or 1-quart volume)

       fitted  with caps lined  with Teflon.  Foil may be substituted tor

       Teflon if the sample is not corros'ive.  French or Boston Round de-

       sign is recommended.  The container must be washed and solvent-

       rinsed before use to minimize interferences.

5.1.2  Compositing equipment — Automatic or manual compositing system.

       Must incorporate glass  sample containers for the collection of a

       minimum  increment of  250 ml.  Sample  containers must be kept  re-

       frigerated during sampling.  No  Tygon or rubber tubing may be used

       in the system.

 5.2  Separatory funnels  —  2000-ml,  1000-ml, 125-ml,  with  Teflon stopcocks.
                       j
 5.3  Drying column  —  20-mm ID Pyrex  chromatogv  . .:. -  column with coarse

      frit.

 5.4  Kudema-Danish (K-D)  apparatus

 5.4.1  Concentrator tube — 10-ml,  graduated (Kontes  K-570050-1025 or

        equivalent) .

 5.4.2  Evaporative flask — 500-ml (Kontes K-57001-0500 or equivalent).

        Attach to  concentrator tube with springs.   (Kontes K-662750-0012).

 5.4.3  Snyder column — three-ball macro (Kontes K-503000-0121 or equivalent)

 5.4.4  Boiling chips — solvent extracted, approximately  10/40 mesh.

 5.5  Volumetric flasks — NBS Class A, 1-ml and 10-ml.

 5.6  Water bach— capable of ternerature control (+ 2°C).  Bath should

      be  used in a hood.

                                  45           Stewart  Laboratories, Inc.
                                               Knoxville,  Tennessee  37921

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5.7  Gas chromatograph —  analytical system complete with gas chronaco-


     graph suitable for on-column injection and all required accessories


     including electron, capture or halogen-specific detector, column


     supplies, recorder, gases, and syringes.   A data system for measur-


     ing peak, areas or peak heights may be used.


5.7.1  Columns and analytical conditions.


       Primary Analysis Column (Column 1):  Supelcoport  (100/120 mesh)


        coated with 1.57. SP-2250/1.95% SP-2401  packed in  a  180-cm long


        x  4-cm ID  Pyrex glass column with Argon (95%)/methane (5%)  car-


        rier  gas at a  flow rate of  60-ml/min.   Column temperature,  iso-


        thermal at 200°C.


        Confirmation Column  (Column 2):   Supelcoport (100 x 120  mesh)


        coated with 3% OV-1  in  a  ISO-cm  long x  4-mm ID  Pyrax glass  column
                       5

        with Argone (95/0/Methane (5%)  carrier  gas at a *^J rate  of 60-ml/


        tain.   Column temperature, isothermal at 200 C.


 5.8  Chromatcgraphic  column — Pyrex,  400-mm.  x 25-mm. OD, with coarse


      fritted plate and Teflon stopcock (Kontes K-42054-213 or equivalent).


 6.  Reagents


 6.1  Sodium chloride — (ACS)  saturated solution in water  (pre-rinse


      crystals with hexane).


 6.2  Sodium hydroxide — (ACS)  10 N in distilled water.


 6.3  Sodium  sulfate — (ACS) granular, anhydrous  (purified  by  heating



      at  400°C for 4 hrs. in a shallow Cray).


 6.4  Sulfuric acid (1+1) — (ACS) concentrated  (Sp. Cr. 1.34)  mix equal



      volumes with distilled water.


  6.5  Mercury —  triple-distilled.


  6.6   Boiling chips'— Her.gar  granules  (Hengar Co.; Fisher Co.) or equivalent-,


  6.7   Acetone —  pesticide  residue analysis grade.


                                   46            Stewart Laboratories, Inc.
                                                rLnoxviile,  Tennessee 37921

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6.3  Acetonitrile  — pesticide residue analysis grade.

6.9  Diethyl ether — Nanograde,  redistilled in glass if nec.essary.

6.9.1  Muse be free of peroxides  as indicated by EM Quant test strips

       (Test strips are avilable from EM Laboratories,  Inc., 500 Execu-

       tive Blvd., Elasford, New York, 10523).

6.9.2  If test indicates positive, remove peroxides by eluting over "basic

       or neutral grade aluminum oxide as recommended in instructions

       provided with  the test kit.  Re-test before using.)*

 6.9-3  Distill de-peroxidized ether in glass.  Preserve with  2%  (V:V)

       nethanol.

 6.10 Hexane — pesticide residue  analysis grade.

 6.11 Isooctane  (2,2,4-trimethyl  pentane) — pesticide residue analysis

      grade.

 6.12 Methylene  chloride — pesticide  quality or equivalent.

 6.13 Aluminum oxide — basic or  neutral,  active.

 6.14 Florisil —  PR grade  (60/100 mesh);  purchase activated at 1250 F

     • and store  in glass containers with glass stoppers  or foil-lined

      screw caps.   Store at 130 G or activate each batch at least 16 hours

      at 130 C in a foil-covered glass container before use.

 6.15 Standard stock solutions.

 6.15.1 Prepare stock standards by dissolving a carefully weighed amount

        of  a pure standard Aroclor in pesticide grade isooctane and di-

        lute to volume  in  a ground glass stoppered volumetric  flask.

 6.15.2 Transfer  concentrated standard to a  septum vi«l,  seal  and store

         in  a refrigerator.  Check  frequently  for  signs  of degradation or

         evaporation,  especially  just  prior  to preparing working standards

         froa them.
                                  47            Stewart  Laboratories,  Inc.
                                                Knoxville, Tennessee 37921

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6.16 Calibration standards.

6.16.L Prepare calibration standards by serial dilution of-,the  stock

       standards.

6.16.2 Transfer solutions Co septum vials and seal.   Re-seal vials im-

       mediately after removing an aliquot for analysis.

7.  Calibration

7.1  Prepare calibration standards  (6.16) that contain  the compounds of

      interest, either singly or mixed,  together.  The standards should

      be prepared at concentrations  covering  two or more orders of mag-

      nitude  that will bracket  the working range of the  chroma tographic'

      system.

 7.2  Establish operating  parameters equivalent to those indicated in.

      Section 5.7.1.   By  injecting  calibration standards, establish  the

      detection limit  of  the detector and the linear  range of the  analyti

      cal  system for  each compound.   Typical  gas  chromatograms  of  select

      organochlorine  pesticides and PCB's are shown  in  Figures  1  to  11.

 7.3  The  cleanup procedure in Section 11.3  utilizes  Florisil chromatog-

      raphy-   Florisil from different batches or  sources may vary in ab-

      sorptive capacity.   To standardize the amount  of  Florisil which is

      used, the use of a lauric acid value (Mills,  1968) is  suggested.

      The referenced procedure (2)  determines the adsorption from hexane

      solution of lauric acid  (mg)   per grain Florisil.  The amount of

      Florisil to be used for  each  column is calculated by dividing this

      factor into 110 and multiplying  by 20 grams.

  7.4  Scfore using any cleanup procedure, the analyst nust process  a

      series of  calibration standards  through  the procedure  to validate

      elution  patterns and  the absence of interferences from the  reagents.

                                   43           Stewart Laboratories, Inc.
                                                Knoxville,  Tennessee 37921

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8.   QuaI icy Control


3.1  Before processing any samples,  the analyse  should  demonstrate through


     the analysis of a distilled water method blank,  that  all  glassware


     and reagents are interference-free.  Each tine a sec  of samples is ex-


     tracted or there is a change in reagents, a method blank should be


     processed as a -safeguard" against chronic laboratory contamination.


 8.2  Standard quality assurance practices should be used with this method.


     Field replicates should be collected to validate the precisian of


     the sampling technique.  Laboratory replicates  (7 to 10/i) should be


     analyzed  to validate  the precision of the analysis.  Fortified


     samples  should be  analyzed  to validate  the accuracy of the analysis.


     Where doubt  exists over  the  identification of a peak on  the  chro-


     matogram,  confirmatory  techniques  such  as mass  spectroscopy  should


     be used.


 9.  Sample Collection,  Preservation  and Handling


 9.L Crab  samples must  be collected  in glass containers.  Conventional


      sampling practices (3,  4)  should be  followed,  except that  the bottle
                            \
      must  not be pre-washed with sample before  collection.   Composite


      samples should be collected in refrigerated glass containers in ac-


      cordance with  the requirements of the program.   Automatic  sampling


      equipment must be free of Tygon and other  potential  sources of con-


      tamination.

 9.2  The  saaples must  be  iced or refrigerated from the time of collection


      until extraction.  Chemical preservatives should not be used in the


       field unless  more than 24 hours will elapse before delivery  to  the


       laboratory.   If the  samples will  not be extracted within 48  hours  of


       collection, the sample should  be  adjusted  to a pH range of  6.0  to


       8.0  with sodium hydroxide  or sulfuric  acid.  Prior  to adding acid

                                  49          Stewart  Laboratories,  Inc.
                                               r-rTo/H i o.   7jnr-.es see 37921.

-------
     or base, sark Che water meniscus on the side of the sampling hoc tie

     for later determination of sample volume.

 9.3  All samples must be extracted within. 7 days and completely analyzed

     within  30 days of collection.

 10.  Sanple Extraction

10.1  Pour  the entire"sample  into a two-liter  separatory funnel.  Check

      the pH  of  the  sample with wide-range pH  paper  and adjust  to within

      the range of  pH  5  to  9  with  sodium hydroxide or sulfuric  acid.

 10.2  Add 60-al of  15% methylene chloride in hexane  to the  sample bottle,

      seal,  and shake 30 seconds  to rinse the  inner  walls.  Transfer  the

      solvent into  the separatory  funnel, and  extract the sample by shaking

      the funnel for two minutes with periodic venting to release vapor

      pressure.  Allow -,the organic layer to  separate from the water phase

      for a minimum of ten minutes.   If the emulsion interface  between

      layers  is more than one-third the size of the  solvent layer,  the

      analyst must employ mechanical  techniques to complete the phase

      separation.  The optimum technique depends upon the sample, but

      may include stirring,  filtration of the emulsion through glass wool,

      or centrifugation.

 10.3 Drain  the water layer  into a second two-liter separatory funnel.

      Collect the solvent extract in a  250-ml Erlenmeyer flask.

 10.4 Add a  second  60-ml volume of 15%  methylene chloride  in hexane  to

       the  sacple bottle and  complete  the extraction procedure  a second

       time,  combining  the  extracts in  the 250-ml  Erlenmeyer  flask.   Pour

       che  water  layer  back  into the  first  separatory funnel.

 10.5  Perform a  third extraction  in  the same  nanner.  Pour the combined

       extract through a drying column containing  3  to 4  inches of  anhy-

       drous sodium sulfate,  and  collect it in a 500-al  Kuderna-Danish

                                   50           Stewart  Laboratories, Inc.
                                                 Kr.oxville. Tennessee 37921

-------
     K-D)  flask  equipped with  a.  10-ml concencracor Cuba.  Rinse  che Er-

     lenmeyer  flask,  and column Cwice with  20-  Co 30-col hexane  co complece

     the  quanticacive cransfer.

10.6 Add  1 or  2  clean boiling  chips Co  Che flask and  attach  a  chree-ball

     Snyder column.   Pre-wet  the Snyder "column by adding_ abouc  L  tnl  mechyl-

     ene  chloride to the  top.   Place the K-D apparatus  on a.  hot  water

     bath (80  to S5°C) so  that Che concentrator tube  is partially  immer-

      sed  in the hot vater, and the entire lower rounded surfaca  of the

      flask is bathed in vapor.  Adjust the vertical  position of  the ap-

      paratus and the water  temperature as required co complece Che con-

      centration  in  15 Co  20 minuCes.  Ac  Che proper  race of  distillation

      the  balls of the column  will  actively chatter but the chambers will

      not  flood.  When Che apparenC volume of liquid reaches  1 nil,  remove

      the  v-^ '-apparatus aad  allow  it to  drain for at lease 10 minutes

      while  cooling.

 10.7  Remove the  Snyder column and rinse the flask and its lower joint

      into the concencracor  tube wich  1  Co 2 ml of hexane, and adjust  Che

      volume Co  10.0 ml.   A  5-ml syringe is  recommended for  chis operacion.

      Scopper  che concencrator>Cube and  store  refrigerated if  further  pro-

      cessing  will not be  performed immediately.   If  che  sample  extract

       requires no further  cleanup, proceed with gas chromatographic analy-

       sis.  If che sample  requires cleanup,  proceed  Co  Seccion 11.

 10.3  Determine  che original sample volume by re-filling  che sample bottle

       to  che mark and Cransferring che liquid co  a 1000-tal graduaced  cyl-

       inder.  Record che sample volume Co che nearesc 5 ml.

                                    51            Scewart Laboratories,  Lnc.
                                                 Knoxville, Tennessee  37921

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11.   Cleanup  and  Separation


11.1  Cleanup procedures are used  to  extend  the  sensitivity  of  a  method


      by minimizing  or  eliminating interferences that  mask the  gas chro-


      oatographic response to  the  pesticides and PCB's.   The hexane-


      acetonitrile partition procedure is useful for removing gross amounts


      of fatty acids and oils  from the extract.   The Florisil column'al-


      lows for a select fraorionation of the conpounds and will eliminate


      polar materials.   Elemental  sulfur, which interferes*with  the elec-


      tron capture gas chromatography-of certain pesticides, can be re-


      coved by treatment with mercury as described below.
/

 11.2 Hexane-acetonitrile partition.  (5) —  this procedure is applicable


      to all of  the pesticides and PCB's except mirex.


 11.2.1   Quantitatively  transfer the  previously-concentrated  extract to a


       125-ml separate., '. jmel with  enough  hexane- to  bring  the final  volume


       to 15  ml.   Extract  the  sample  four  times  by shaking vigorously  for


      one ninute with  30-ml portions of  hexane-saturated acetonitrile.


 11.2.2   Combine  and transfer  the  acetonitrile  phases  to  a one-liter sepa-


       ratory funnel.   Add 650 ml  of  distilled  water and  40  ml  of satur-


       ated sodium chloride  solution.  Mix thoroughly for 30 to 45 seconds.


       Extract with two 100-tal portions of hexane by vigorously shaking


       aboutlS seconds.


 11.2.3  Combine the hexane extracts in. a 1-liter separatory funnel and


       wash  twice with 100-ml portions of distilled water.. Discard the


       vater  layer and pour the hexane layer through  a 3  to 4  inch anhy-


       drous  sodium sulfate column into a 500-ml K-D  flask equipped with


       a 10-ml concentrator tube.   Rinse the separator-/  funnel and  column


       with  three 10-ml portions  of  hexane.


                                    52           Stewart  Laboratories, Inc.

                                                          ,  Tennessee  37921

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11.2.4   Concentrate the extracts  to  6  to  10 31!  by  standard K-D  techniques

        (10.6).   Analyze by gas chrqmatography.

11.3 Florisil Column Cleanup (6)

11.3.1  Add a weight of Florisil, (normally   21 g)  pre-determined by cali-

        bration (7.3, 7.4), to a chromatographic column'.   Settle the Flori-

        sil by tapping the column.  Add sodium sulfate to the top of-the

        Florisil to form a layer 1 to 2 eta deep.  Add 60 ml of hexane to

        wet and rinse  the sodium sulfate and Florisil.  Juat prior to ex-

        posure of  the  sodium sulfate to air,  stop the elution of the hex-

        ane by closing the  stopcock on the chromatography column.  Discard

        the  eluate.

 11.3.2 Place a  500-ml K-D  flask and clean concentrator  tube under the

        chromatography column.   Transfer  the 10 ml sample extract volume

         from the K-D concentra4.   ->ibe to the  Florisil column.   Drain

         the  solvent into the  K-D flask.   Then  rinse  the  tube  twice with

         1 to 2  ml of hexane,  and each time just  prior  to exposure of  the

         sodium  sulfate layer  to  the air,  rinse the column with this  solvent.

 11.3.3  Drain the column into the flask  until  the sodium sulfate layer  is

         nearly  exposed, then  elute the column  with 200 ml of  62 ethyl ether

         in hexane (Fraction 1) using a drip  rate of  about 5 ml/min.   Remove

         the K-D flask and set aside for  later  concentration.   Elute the

         column again, using 200 ml of 157. ethyl ether in hexane (Fraction

         2),   into a second K-D flask.  Perform the third elution using

         200 ml of 50% ethyl ether in hexane (Fraction 3).  The  elution

         patterns  for  the pesticides and PCB's are shown in Table 2.

  11.3.4  Concentrate  the eluates by standard K-0  techniques (10.6).  Ad-

          just final  volume  to  10 ml with hexane.  Analyze by gas chrcmaccgraphy

                                   53           Stewart  Laboratories,  Inc.
                                                Knoxville,  Tennessee  37921

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11.4   Removal  of  Sulfur

11.4.1  Elemental sulfur  will eluta in Fraction I  of  the Florisil  column

        cleanup procedure.   If a large amount of sulfur is present in the

        extract,  it may  eluta in all fractions.  If so, each fraction must

        be further traaCid to remova the sulfur.  To remove sulfur inter-

        ference from this fraction or the original extract, pipet I'.OO al

        of the concentrated extract into a clean concentrator tube or

        Teflon-sealed vial.  Add 1 to 3 drops of mercury and seal.  Agi-

        tate  the contents of  the vial for 15 to 30 sec'nds.  Place the

        vial  in  an upright position on a reciprocal laboratory shaker an.d

        shake for up to  2 hours.~  This treatment may need  to be repeated

        several  tines.   Analyze by gas chromatography-

 12.   Gas  Chromatography

 12.1  Section 5.7.1  summarizes  the recomp- • - *«.d gas chromatographic column

       materials  and operating conditions  for the  instrument.  Table  1  lists

       retention times and detection limits  that should be achieved by  this

       method.  Examples  of  the separations  achieved by these columns are

       shown in Figures  1 through 10.

 12.2  Analysis of Calibration Standards

 12.2.1  The chromatographic system is calibrated with a minimum of three

         standards of each required Aroclor or Aroclor mixture (see Sec-

         tion  13-Calculations).

 12.2.2  A standard calibration curve is plotted of response (peak height

         or peak area)  versus  ng  using an appropriate  peak  (or peaks)  from

         a pure  or mixed Aroclor standard.  The largest or most clearly

          separated  peak  is chosen  if  the standard  is a  single Aroclor.   If

          the  standard is  a mixed Aroclor, the  peak or  peaks  with  the least

          interference or mutual contribution are  chosen.

                                    54           Stewart Laboratories,  Inc.
                                                 Kr.oxville, Tennessee 3/921

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12.2.3  If Che calibration curve shows that response is  Linear,  a.

        response factor R may be calculated for the peaks chosen.



           „   ng of standard      ng of standard
                 ?k he (mm)    °r     Pk area

12.3 Analysis of Samples

12.3.1  Inject  2 to 5 jil of the-sample extract 'using the solvent-flush

        technique (7).  Smaller  (1.0 ul) volumes can be  injected if auto-

        matic devices are  employed.  Record  the volume injected to the

        nearest  0.05 ul, and the resulting peak size, in area units or

        peak height  in mm.

 12.3.2 If  the  peak  area  (height)  exceeds  the  linear range of the system,

        dilute  the  extract and re-analyze.

 12.3.3  If  interferences  prevent the quantitation  of the sample, cleanup

         procedures  must  be followed (Section 11).

 13.  Calculations

 13.1  Qualitative Analysis

       In order to identify the Aroclor or Aroclor  mixture present  in the

       sample, the peak height and retention time pattern exhibited  by the

       sample chromatogram is compared to the patterns  exhibited by  the

       single Aroclor standards and/or mixed Aroclor standards.   The con-

       taminant  is identified as the Aroclor or Aroclor mixture whose pat-

       tern  matches or mast-closely matches  the sample chromatogram.

  13.2  Quantitative Analysis —  Peak Height  Procedure

  13.2.1   Determination of appropriate  peak(s)  to use for quantitation.

          Any peak measured  for  quantitation  must be free of interference.

  Case  1:  When  the sample  chromatogram is  identified as  a single Aroclor,

          the largest  or most  cleanly  separated  peak of  the Aroclor  pat-

          tern  is used  for  analysis.

                                     55          Stewart Laboratories, Inc
                                                       lie, Tennessee 379Z

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Case 2:  When the sample is Identified as an Aroclor mixture, peaks  that

         are unique to the single Aroclors  in  the mixture are used  for

         quantitation.

Case ,3:  .»iieu c.:^ a-i-z^-ii j.j a  mi.-, ^u.'i  ci .-....'uo_wCc.  cue  -i-vis  ;xo z  i-:l".^.b.l;

         peaks  that can be attributed  uniquely to  each single Aroclor,

         appropriate  peaks are chosen;  and  peak height ratios are used

         Co  determine the  contribution of  each single  Aroclor  (se'e 13.2-.2).

 13.2.2  Calculation using  standard curves

         Calibration curves:   At least three standards  are used  to fora

         a  calibration curve.   Calibration curves are determined from single

         Aroclor standards or from mixed Aroclor standards which have peaks

         unique to the single Aroclors present in the mixture.

         The peak height of the largest or most cleanly separated peak(s)

         is measured.   Peak height is measured from common b-"   Line.  The

         calibration curve is  determined by plotting peak height versus

         nanograms.



         Calculation  of Aroclor concentration:

  Case  L:  The sample  chromatogram base line is drawn  to match the base

          line  of the standard Aroclor chromatogram.   The height  of the

          appropriate peak is  measured.  The  amount  (ng)  of PCB corres-

          ponding  to  the  peak height is read  off of  the calibration curve.

          The Aroclor concentration is then calculated as follows:
                     PC3 ppm _. (A) x (V) x (D)
                                  (V) x (V)
                                     56           Stewart Laboratories, Inc.
                                                  KnoxvLlle,  Tennessee 37921

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       Where   A » ng from curve

               V = voluae of final.extract (ml)

               D = dilution factor, if any

               V  = volume injected into chromatograph  (ul)

               W = weight of  soil  used for  analysis  (g)

Case 2:   The peak heights of  the peaks unique  to  the  individual  Aroclors

         present  in  the  mixture  are measured.   Quantitation is performed.

         as in Case  1.

Case 3:   When the sample is  a mixed "Aroclor  and no mutually exclusive

         peaks can be used,  quantitation  is  more difficult.  The contri-.

         bution of each Aroclor to the peak chosen for quantitation must

         be determined.   This is done by  using peak height ratios calcu-

         lated from single Aroclor standards and then mathematically

         determining the peak height to be attributed to the single A1*-*-

         clor.  After peak heights are calculated, quantitation  is as  in

         Case  1.

 13.2.3   Alternative Calculation Procedure

         Calculate usin% response factors:  When  the  response  of  the  stand-

         ards  have been  shown  to be linear over a  period  of time,  response

         factors may be  used  for quantitation  in  place of the  standard

         curve.  A response  factor  (R) is calculated  by  dividing  the  amount

         of standard  (in ng)  injected  by  the peak height of the  appropriate

         peak.   Peaks  for quantitation are  chosen and measured as above.

         Quantication is performed  exactly  as  when using standard curves,

         with che following  substitution.

                 A (ng)  is  replaced by M  x  R.
                                   57           Stewart Laboratories,  Inc.
                                                Knoxville, Tennessee  37V21

-------
               The equation becomes:
               ?C3
                               (V2) x  (W)
               M = peak height  (ran)

               R = response  factor  (n*/mm)

13.3  Quantitative Analysis — Peak Area  Procedure

13.3.1  Determine the  concentration  of  individual  compounds  according to

        the formula:
                              (A)  (B)  (V )
        Concentration, ug/1 =» 	
                               CV  (VS)

        Where A = calibration factor for chromatographic system,  in
                  nanograas material per area unit

              B = peak size in injection of sample extract,  in area units'

              V. = voluae of extract injected (ul)

              V  «» voluae of total extract (ul)

              V  = volume of water extracted  (ml)

 13.4  Report results in ug/g (ppm).  Round off data to  the nearest yg/g

      or  two significant figures.

 13.5  Calculate  the  limit of detection  (LOD)  for  each Aroclor not detected,

      assuming  a 2 ran  peak  height or an  equivalent  peak area.
                                    
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                              REFERENCES
1.  "Determination of  Organochlorine Pesticides  in  Industrial  Effluents,
    Federal Register,  Volume 38,' Number 125,  Part II,  Appendix II,  p.  L731,
    Friday, June 29,  1973."

2.  Mills, P-  A., "Variation of Florisil Activity:   Simple*Method for  Mea-
    suring Absorbent Capacity and Its Use in Standardizing Florisil Columns,"
    Journal of the Association of Official Analytical  Chemists,  51, 29 (196S).

3.  ASTM Annual Book, of Standards, Part 31, D3370,  "Standard Practice  for
'    Sampling Water," p. 68, 1979.

4.  ASTM Annual Book, of Standards, Part 31, D3694,  "Standard Practice  for
    Preparation of Sample Containers and for Preservation," p. 601, 1979.

5.  Pesticide Analytical Manual, Vol. I, Food and Drug Administration,
    Washington, D. C., Revised.1969, Section 1.11.14b.

6.  "Development  and Application of Test Procedures for Specific Organic
    Toxic  Substances  in Wastewaters.  Category 10-Pesticides and PCB's."
    Report for  EPA Contract 68-03-2606.

7.  Burke,  J. A., "Gas Chromatography  for  Pesticide Residue Analysis; Seme
    Practical Aspects," Journal of  the  Association of Official Analytical
    Chemists, 43,  1037  (1965).
                                    59          Steuart Laboratories, Inc.
                                                Knoxville, Tennessee 37921

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                                   TA31E  1
                  GAS  CHROMATCGRAPHY  GF  PESTICIDES AND ?C3's
Perimeter
                       Retention Time (nin)
                       Column 1    Column 2
                                                       Cetection Lirni t°
Aldn'n
4-3HC
b-oKC
d-oHC
g-3KC
Captan
Carbopner.othi on
Chlordane
4,4'-OCO
4,4'-OC£
4,4'-OOT
Oi en lor an
Oicofol
0 i e 1 dr i n
tndosulfan I
Endosulfin II
"Endosuifan sulfata
Endrin
Endrin aldehyde
HepticMor
Heptachlcr epoxide
Isodrin
Methoxychlcr
Mi rex
PCN3
Perthane
Strobane
Toxapher.e
Triflural in
PC3-1Q15
PC3-1221
PC3-1232
PC3-1242
PC3-12i3
PC3-1254
PC3-126G
2. 40
1.35
1.90
2.15
1.70
6.22
1Q.SO
c
7.33
5.13
9.40
1.35
2.35
5. ^5
4. SO
8.00
14. 22
6. 55
11.32
2. CO
3.50
3. CO
18.20
14.50
1.53
c
c
c
0.94
c
c
c
c
c
c
c
4.10
1.32
1.97
2.20
2.13
5.00
10.90
c
9.QS
7.15
11.75
2.01
4.59
7.23
6.20
8. 28
10.70
8.10
9.30
3.35
5.00
4.33
26.50
15.50
2.01
c
c
c
1.35
c
c
c
c
c
c
c
O.C03
O.CC2
O.GQ4
O.CC4
O.C02
NO
NO
O.'Qi
0.012
O.C06
0.015
NO
NO
o.ccs
O.CC5
0.01
0.03
O.CC3
O.GZ3
O.C02
O.G04
NO
NO
NO
NO
NO
NO
0.40
NO
0.04
0.10
0.10
0.05
O.G3
- 0.03
0.15
  ^Column pac'xing ar,d analytical conditions given in Section  5.7.1.

  ^Cetacticn limit  is calculated frcm t.u.e minimum detachable  GC  response
   volume ~r"
 being  equal  to  five  times  the  GC  background  noise,  assuming a 10-^1  rinal
         f  t.*.e 1-liter  sample extract,  and assuming  3 GC injection  of  5
    roli tars.
Sceuarc uaboracories,  Inc.
      lie,  Tennessee 3/92L
   ^Vultip'e  ?ei<  resccnse.   See  figures  3  to  11.
NO » Mot der.er-ii-sc.
                                      60

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                                   TA3LS 2

             QIST3I3LTION AND RECOVERY OF CHLORINATED PESTICIDES
              A.NO ?C3s USING FLCRISIL COLUMN CKRC^ATCGRAPHY  (5)


Parameter                             Percent Recovery  by Fraction3
	1(-«r       2(15X1     3(-5C^

Aldrln                                     100
a-3HC                                      ICO
b-3HC                                       97
d-BHC                                       93
g-8HC                                      100
Captan                                       >
Carbofenthicn                              TOO
Chlordar.e                                  100
4.V-CQO                                   99
4,4'-CO£                                   98
 4,4'-DOT                                  ICQ
 Qlcofol                                      •*•              •*•
 Oieldrin                                    0             100
 Endosulfan I                               37             64
 Endosulfan II                               0               7         91
 Endcsulfan sulfate                          0               0        1C6
 Endrin                                      4             96
 Er.drin  aldehyde                             0             63         25
 Heptachlcr                                 ICO
 Heatachlcr ejcxida                         ICO
 Isodrin                                    1GO
 Methoxycnlor                               ICO
 Mirex                                      ICO
 Perthane                                   ICO
 Toxaphene                                   96
 PC3-1016                                    97
 PC3-1221                                    97
 PC3-1232                                    95               4
 PC3-1242                                    97
 PC3-1243                                   103
 PC3-1234                                    90
 PC3-1250                                    95                    	
  a£lu*lng solvent ccrrposi ticn given  in Section  11.3.3.

            occurs in both 6i and  152 fractions.
                                    61            Scewarc Laboracories,  Inc.
                                                  Knox'/illa, Tennessee  37921

-------
 COLUMN: 1.53 SP-2250*

          1.353  SP-2401 ON SUPS.CGPORT
 TEMPSATURE: 2QO*C.

 DETECTOR:  ELECTRON  CAPTURE
       at
       a
                             LU
                 8       12

                 N TI.Mc-Ml.NUTcS
Figure 1.  Gas chromatograrn of pesticides
                62
Scevarc Laboracories, Inc.

Knoxville, Tennessee  37921

-------
COLUMN:  1.Sy. SP-2250-
         1.95X S7-2401
TEMPERATURE: *2QQ*C.
DETECTOR: ELSCTSCN CAPTURE
                          SUPELCCPORT
0   ^   4        3       12
        RETENTION TIME-MINUTES

Figure 2.  Gas chrcmatogram of chlcrdane
        63
                   Scewarc  Laboratories,  Inc.
                   Knoxville,  Tennessee 379ZL

-------
                    COLUMN: 1.5r, SP-22SQ
                             1.35:-i SP-2401 'ON SUPS-CQPQRT
                    TEMPERATURE:  200'C.
                    DETECTOR:  ELECTRON  CAPTURE
                  10
                 22
25
                 RETENTION  TIME-MINUTES

Figure 3.  Gas chromatogram of toxaphene
           64
Scevarc Laboracori.es,  Cnc.
Kno:cviLLa, Tennessee 37921

-------
COLUMN:- 1.5S SP-2250* 1.35K SP-24QT ON SUPELCCPOHT
TEV.PE3ATURH: TSQ'C.
DETECTOR: ELECTRON CAPTURE
TO
14
                                   13
22
                    :^ Tl.V.EiMI.NUTES
Figure 4.  Gas chromatogram of PC3-T016
                      65
       Scewarc LaboracorLas,  Inc.
       iCnoxville,  Tennessee 3792L

-------
 COLUMN:  I.Sr. S?-22SQ»1.S5ri SP-2401 ON SUFSLCOPGHT
 TEYiPSARJRS:  1SQ*C.
 QE7ICTOR: ELECTRON CAPTURE
           5_     10      14       13

             RETENTION T1.Y.E-,V,INUTSS
          -  22
Figura 5.  Gas chromatogram  of PC3-122T
                   66
Scevarc Laboracories,  Ir.c.
      lle, Tennessee J792L

-------
   COLUMN:  1.5K SP-222&* LSS^,  SP-2401 ON SUPELCOP03T
   TEMPERATURE:  ISO'C,
   DETECTOR:  ELECTRON  CAPTURE
    u
u
                     10       U      .18
                 RETENTION TIME-,V,1NUTES
                                     22
24
Figure 6.  Gas chromatogram of PC3-1232
               67
                   Scevarc  Laboracories,  Inc.
                   Knoxville,  Tennessee 3792L

-------
  COLUMN:  1.5?t SP-22SQ »1.95  SP-2401 ON SUPSLCOPORT
  TEMP S3 A TU RE:  IStfC.
  DETECTOR: ELECTRON CAPTURE
            S       10       14      13
               RETENTION TlME-MINUTcS
Figure 7.  Gaa chromatogram of PC3-1242
                 68
Sceuarc Laboratories, lac.
Kno,-c/iLle, Tennessee  37921

-------
  COLUMN: 1.5y, SP-22SQ* 1.35* SP-2401 ON 3UPELCOPCRT
  TB1PEHATURE: ISO'C.
  DETECTOR: ELECTRON CAPTURE
5       10      14      IS
      RETENTION TIME-aiNUTc
                                           22
                           25
Figure 8.  Gas chramaiogram of PC3-1243
           69
Scewarc Laoocacories, Inc.
KnoxviiLe, Tennessee 37921

-------
   COLUMN:  1.5% SP-2250* 1.35?', SP-2401 ON SUP51.CCFORT
   TEMPERATURE:  200'C.
   DETECTOR: ELECTRON CAPTURE
              8        10        14.

                RETENTION TIME-,V,INUTE5.
          13
FTgura 9. Gas chromatogram of PC3-1254
                  70
Scewarc.Laboracocles,  Inc
Knox*/ille. Tennessee

-------
   COLUMN: T.SX SP-22SO* 1.35?'. SP-2401 ON SUPELCQPQRT
   TEMPERATURE:  200* C.
   DETECTOR:  ELECTRON  CAPTURE
                   10      14      13      22
                  "RETENTION TIME-MINUTES
Figure 10. Gas chromatogram of PC3-12SO
                      71
Scewarc Laboracories, Inc.
Knoxville. Tennessee 3792L

-------
             APPENDIX 2

PROTOCOL FOR SAMPLE ANALYSIS REPORTS

The following section was taken from
   "Protocol for Sample Analysis",
     OHMS Branch Chemistry Staff

-------
                                                                           Page  10

                                     APPENDIX  0

                        PKOTOlOL  FOR  SAMPLE  ANALYSIS REPORTS
1.  INTKOLJUCI [ON:

   The following procedure must be used when preparing a sample analysis report.
   In order for all documentation and data to be understandable and easily
   reviewed, the report must be sectioned as outlined below:

   REPORT TITLE:  On front cover of report

   TABLE OF CONTENTS:  First page^ot Section I

   SECTION  I:   OHMS8 sample documentation

   SECTION  II:  Chain of custody records

   SECTION  111:  Evaluation of calibration range data sheets

   SECTION.IV:  Evaluation of calibration range chromatograms and/or spectra

   SECTION  V:   Recovery studies chromatograms and/or spectra, and data sheets

   SECTION  VI:  Quantitative analysis by chromatography and/or spectroscopy data sheets

   SECTION  Vil:  Sample chromatograms and/or spectra

   SECTION  VII4:  Service laboratory chromatograms and/or spectra

   ^cte 1:   If both chromatographic and spectroscopic analyses are performed on
            the samples, Sections 111 thru VIII are each to be subdivided into
            two sections, labeled A and 8.

   Note 2:   If the contents of any one or more of the sections was not generated
            for the project, delete that section in the report,  making note of
            this in the table of contents.

2.  DETAIL OF EACH REPORT SECTION, I THRU VIII  .

   Listed below are the specific contents of each section of a sample  analysis
   report.   Each report must have a title, recorded on the front cover,  and a
   table of contents must appear as the first page of Section I.  The  sections of
   the report  must be kept separate through the use of dividers.  These  should be
   labeled  with the title of the represented section, and should also  have  listed
   any further organizational  method used within that section.

   -:, *.  SECTION I:   OHMSB sample documentation

       :. Chemistry Staff Sample Analysis Form (see Attachment 1)

       2. Technical  Services Report  (see Attachment 2).  The final version  of
         this  report,  after being  reviewed by U. frank,  must be typed and  must
         reflect  the Chemistry Staff's updated overtime hours.

       3. Chemistry Staff Sample Report (see Attachment 3).

-------
                                                                         Paye 11

        <*.  A copy  of  final  memo  sent  to  Requestor (attachment  4)
        t>.  Method  of  analysis  used  by  service lab.   This  should  be  included  if"
           the  sample is  contracted out.
        o.  Chemistry  Staff  procedure.   This  should  be  included  if  the  sample
           analysis  is  concurrently done  by  R&O.
        /.  Service lab  report  of analysis.
        8.  Tabulation of  results.
        9.  QC program which is used by  the  service  lab.
       10.  A Quality  Assurance procedure  used by  the Chemistry  Staff to
           validate  the service  lab results  should  be  included.
2.2  SECTION II; Chain  of custody  records
     1.  Polaroid pictures of the samples  are taken  upon receipt.  These
        must be  included, and  each must  be  signed and  dated.
     2.  Chain of Custody  Receipts  listing  the source of the  sample, date
        collected,  and  by whom.
     3.  Federal  Express receipt(s)
     4.  Record of  Communication  with EERU  for sample to be contracted  out.
2.3  SECTION III:   Evaluation  of calibration range  data sheets
     1.  Al1  data sheets must be  signed by  the verifying R&D member.
     2.  Spot check the  data entries from  the chromatograms to the data sheets,
        and  from the  data sheets to the tapes to  make  sure that they are
        correct.                             ;
     3.  Make certain  the  Ei calibration errors are  within ±10%.  This will
        assure that, all of  the samples are within the  calibration range.
        Otherwise, discuss  with  Mike Gruenfeld or Uwe  Frank.
2.4  SECTION IV:   Evaluation of  calibration  range chromatograms and/or spectra
     1.  Since the  chromatograms  or spectra have been placed in a separate
        section, make sure  that  it Is easy to cross-reference them to the data
        sheets.
2.5  SECTION  V:   Recovery studies
     1.  Include any previously collected data which pertains to methods and/or
        relative error  obtained  for the sample which is being analyzed.
2.5 SECTION VI;   Quantitative analysis by chromatography and/or spectroscopy
    data sheets
    1„ Make certain that a  Chemistry  Staff  member  has checked the
       calculations,  and signed  the data sheets,
    '. . 9ata sheets must have the signature  or initials of the analyst who
       performed the work,  and must be dated.
    3. Check the Microprocessor  tape  values  against the reported values on  the
       tabulation  of results to  be sure that they  agree.

-------
                                                                         Page !2
'{. I SHCIluN VII:  Sample chrumdtoijrains  and/or-  spectr-d
    1. lo insure easy cros^-reference,  number  these  so  as  to  correspond  with
       the appropriate data sheets  contained  in  Section  VI.
2.U SfcCTlQNVIIi:  Service  laboratory  chromatograms  and/or  spectra
    1. Make certain that these  are  dated,  identified,  and  signed.

-------
                 APPENDIX  B

ROTARY KILN AND SECONDARY  COMBUSTION CHAMBER
             BURNER ASSEMBLIES

-------
                                                                                 oy<-' '»
                                    MULTIFIRE® II  and III  Gas or  Light  Oil Burners
                Cross  Section  of Typical  MULTIFIRE®  Burner
                                                 Pilot Air
Burner Block
                           Gas or
                          Atomizing
                           Air Inlet
     Pressure Test Connection
     Oil Tube Inlet Insert

     Strainer \
                                                ^'  y.v    N ~ . ^ I  \ » e  • ' r~. • , ^   •
                                                IA j?.:- • • X  \T* ^ ^ " ^ -v •  : ,"\ •7-«:'*i
                                                &£•'v-v'yx "•4s&'*'...'<~?''';-2£^i~~^
      Oil Tip/Tube.
      Subassembly
        Nozzle Body
                                     Burner Block Frame
             MULTIFIRE II Burner Nozzle                       MULTIFIRE III Burner Nozzle
                   (FRONT VIEW)                                   (FRONT VIEW)
There  are minor differences   in  appearance  between the various sizes  of MULTIFIRE
Burners.   However,  the cross section drawing shown here may  be  considered represen-
tative for understanding the  inter-relationship   of flow of  combustion air,  atomiz-
ing air,  light oil  and gas.

The centering guide used  on most MULTIFIRE Burners  provides  a twist  to atomizing
air for oil  firing  and to the gas  for gas firing.

The MULTIFIRE II Burner nozzle provides a twist  to the combustion air which  creates
a tightly wrapped  flame.  The MULTIFIRE II Burner  may not be overfired.

The MULTtlFIRE.I.I I-Burner'.nozzle does  not provide  a  combustion air twist.   It may be
                             pl ications making use  of.available  secondary,, .air in the
                             •• ••- • •         •• -., ~ * ••-•  ...    :   .           ..:.......-.«---•'<•••'.•
 laxor?'
                  WAXON MtACTKU A MXtCT Of CONTINUOUS IMttOVCMCNt IN ITS ftOOUCT D15ICNS AND CONSKUCTIOM.
                        If IfSHVfS THC IICHT TO Altfl SP«:*
-------
 MULTIFIRE®
 Gas  or  Oil  Burners
                           2",   3"  and   4"  MULTIFIRE  II
                           Capacities  and  Specifications
 Table 1:
2S" we (14 oti)
NATURAL
2"
680
60
	
—
25-
M5
—
—
10.0-
9"
2.5-
12:1
•8
•9
- 1 0
3"
1450
140
	
	
25"
250
...
—
12.7"
12-
3.5'
11:1
•15
•26
-10
GAS
4"
2825-
420
	
	
25"
471
—
—
30.4-
16"
V
7: 1
0
0
-10
#2 OIL
2"
725
98
5.3
.7
25"
113
25"
14
5.5»
9"
3'
7:1
• 14
• 10
-10
3"
14 5O
no
10.4
1.2
25"
250
25"
27
20.0*
12"
4'
9:1
0
•35
-10
4"
29J5
255
20.2
i.a
25"
471
25"
54
I6.0«
16"
6'
11:1
•14
•28
-10
AIR PRESSURE O
FUEL
BURNER SIZE
K8TU/HR

GPH '
02 OIL
COMS. AIR
@> MAX
ATOMIZING
AIR
MAX
MIN
MAX
MIN
APO
SCFM
APO
SCFM
FU£L PRESSURE
AP @ BURNER O


OIA
LOTH
TURNDOWN RATIO
7. CHANGE
MAXIMUY.
CAPACITr
O
CASE
SI
CASE
#2
CASE
«3
32" w< (18 oti)
NATURAL CAS
2"
735
60
	
	
32"
122
...
...
n.5"
9"
i.5'
12:1
•19
•It
-10
3"
1600
140
	
	
32"
267
	
	
15.0"
12"
»3.5'
u:l
•6
•20
-10
4"
5005
420
	
	
52"
501
...
	
34.0"
16"
51
7: 1
0
0
-1C
t»1 OIL
2"
740
125
5.5
.9
32"
122
32"
16
6.1*
9"
5-
6: 1
•4C
•46
-1C
3"
I6OO
200
1 1.4
1 .4
32"
267
J2"
51
24. 0«
12-
4 '
9:1
• 5
•"
-'0
4"
29 5O
295
21.0
2.1
32-
501
J2"
61
18.0"
16"
5'
10: i
.»
•i=
-•-
                                                                       Capacities  shown  in Table I
                                                                       are based on .65 spgr natural
                                                                       gas  (1075  BTU/M-5)   and  *2
                                                                       fuel  oil  (using  a  separate
                                                                       oil control   valve  for  each
                                                                       burner).  The oil supply must
                                                                       be regulated to provide indi-
                                                                       cated pressure at inlet to the
                                                                       burner Y-strainer.    Oil must
                                                                       be  maintained  at   40° F  or
                                                                       higher  (50 ssu
                                                                       cosi tyl .
                                                                                      mininxim vis-
                                                                       Other gaseous  or  distillate
                                                                       fuels such  as /» I ,   *2,  JP4,
                                                                       etc. may be used.   V4 oil  or
                                                                       heavier may not be used. Con-
                                                                       tact Max on for specific recom-
                                                                           t i ons .
O-iif -
OUif f«
O*a>"
 bat*
               n«r all terentiai
                                  ew with no teeondar / aif avai'lsclo, 0"-
 *on«t p<*fts
 «*iy require
feot i*I pressure: Burner 9*1
Body o* r«ot«? E>as*d on liri/i
pressure
            C*S£ f| - ririrtt) info still fresn a i r
            CASE *2 - firing «cross fre*h «ir stre-ira o* 1,000 fp«« or I-is
PIPING  ARRANGEMENTS:
iVULTIFIRE Burners can  be shipped  in
either of  the piping configurations
shown.   Unless  arrangement  "L"   is
specified,   "0"  will be  furnished,
and  requires use of a  flexible con-
nection or  street elbow in the atom-
izing air  line  to avoid scanner in-
terference.                            «
                                                                       To achieve minimum capacities
                                                                       shown:  for gas firing,  dif-
                                                                       ferential  sir pressure at Tin-
                                                                       iinuin nxist  not exr f-eo   .i" we •
                                                                       for  oil  firing,  air control
                                                                       valve must  be fully closed at
                                                                       minimum.
                                                             MAXIMUM  AIR  TEMPERATURES
                                                              for Seal & Support  Housings
                                                             Carbon Steel    Stainless St_eel
                                                             900°  F Supply
                                                             600°  F Return
                                                                           1500° F  Supply
                                                                           1000° F  Return
Table 2:
                 Assembly Numbers

Basic burner
Burner
with Seal
and Support
Burner with
Seal and
Support and
Dcwflflrlng
Support Ring


DESCRIPTION: •-
Burner
Appro*. Sh. wt. ILbs.l
Replacement Block 4 Frame Asse^oly
with Carbon Steel Seal and Support
with «3IO Stainless Steel Seal
and Support
Approx. Sh. Wt. ILbs.l
fteplaewent "' »« C.S. S t Support
Block/Frame Assy w|th 310 S.S. S * Spt
with Carbon Steel Seal and Support,
Stainless Steel OownHrln^ Ring
with Stainless Steel Seal and Support,
Stainleaa Steel Oownflrlng Rln^
Approx. Sh. Wt. (Lba.)
Seeled, Pressure Type Pilot
Scanner Cooling Tee Set
2"
31528
70
28334
31529
31530
120
28337
28463
32047
32046
I2S
3»
31531
130
28351
31532
31533
200
28460
28464
32049
32050
205
&
JI534
210
2835J
31535
3153(5
310
28461
26465
32051
32052
315
IIS84 •'.V*~
30854
                                                         IMPORTANT:
                                                         Use only UV flame sensor systems  for oil
                                                         or.. dual fuel   firing.'   UV flame  sensor
                                                         systems are subject to excitation  by di-
                                                         rect  or reflected radiation  from  spark
                                                         Ignltors  or other burners.   While every
                                                         effort has been made in our burner design
                                                         to minimize the possibility  of spark ex-
                                                         citation,  each application  must be  re-
                                                         viewed  by the user  to Insure that  the
                                                         flame detection  system  Is not energized
                                                         u.nsaf.ely ...by direct or reflected UV radi-
                                                        *'-"-"•'-----•-'- jgni tbr.s br.other burners.
                                                                        . —\-" -u-v; i j.-.si-. .v f urn [shed.;
                                                        B£K:;...

-------
                                                                      MULTIFIRE®
                                                             Gas  or Oil  Burners.
                    .-<*'' '•:.''« '•
                        /  3"dncT4"  MULTIFIRE II-
                                 Dimensions
                  CLEAR FOR Oil TU6f REMOVAL
     ® SCAl AND SUPPORT
        PlAIf THICKNESS
         '«" CAS/AIOM.
 • - COMB. * I* AIR TEST CONN.
 TES! CONN.
ATOM. AIR/CAS CONN.

S)
  OIA
                               (v) on CONN.
                              u; COMBUSTION
                                Alt CONN.
,| «  > 10
j J |—*	I  ^-- K  SCANNER
          CONNECTION
          D 4 HOIES
 AMD SUPPORT MOUSCMO OlfffNSICNS
BURNER
SIZE
2"
3"
4"

A
9.C

i'..;

B
4.5
5.75
C.7'..

c
14.5
50.
SO.
20.5
SO.

D
5.25
6.25
7.75

E
.69

.69

F
.69

.ec
Burner Dimensions in Inches
G
5.12

6.56
H
5.56
6.58
7.4i
J
4.50
'j.oa
•>.<:.
K
9. CO

i 1.50
L
8.81

i i.K
M°
11.56
DIA.
01".
1 7 . i r
N
7.50

! ' . ':>.
O
7.63


P
'•'*
. . s.

o
.'..44


S
I.CXJ


T
1
'

U
2
'

V
1 ft


w
5.25
t.CC

X
. 19
.19

Y
t.oe
..94

z
11.36
14.26
14.73
                           mi ng
PIPC THKAOS ON THIS FAOC CONfOlM TO ANSI STANOAIO t).l
                           -1.28'H
                 3/4" Scanner
                    Conn,
                                      4.00"-
                                               3/j" Purge Air Conn.
                                  — 1.69"-

                     Scanner Cooling Tee Set
             MAXOfl MIACIKtl A fOKT Of CONHNUOUi IMFIOVIMINI IN IIS MOOUCI OlSICNi AND CONSHUCIIGN
                  II IEUIVIS IH( IICHI TO Allll SMCWKAIIONS AT ANT 1IMI WltHOUl f«IOI NOIlCt
        MAXON  CORPORATION, Muncie, Indiana, U.S.A.

-------
North American |
Mfg. Co.
Cleveland. OH 44 IDS USA 1
OIL ATOMIZERS
Steam or Compressed Air
J
BULLETIN 56.22
5-80 56.23
 Series 5622 and 5623 Nozzle  Mixing Atomizers produce 30° spray
 angles and fairly long  flames such  as required for  steel  mill reheat fur-
 naces, rotary dryers, and other long combustion chambers. The stainless
 steel oil nozzle is concentric in the stainless steel nose,  and flush with
 it; so steam and oil  pressures do not affect each other.

 Combustion air must be supplied around the atomizer.  To accomplish
 this, the atomizers can be supplied  as part of Luminous  Rame  Burners,
 Refractory-Lined Burners, or Magna-Flame  Burners.  By specifying the
 proper "L" dimension, a user can adapt the atomizers to existing burners.
 For installations where  adequate  combustion air is provided.  North
 American  can  furnish  a complete assembly consisting of atomizer,
 mounting, mounting plate, and refractory tile as shown  below. Special
 nozzles to produce  wider, shorter flames have been designed — consult
 North  American.

 Cleaning.  Strainers are recommended in  both the steam and oil  lines.
 The oil nozzle of any of these atomizers is readily accessible for  cleaning
 (with steam or a wire) by removal of a pipe plug at the back which  opens
 a straight passage to the oil nozzle if the customer has piped the unit as
 shown dotted for 5622.  The quick clean-out feature of Series  5622
 permits cleaning of the steam or air passage even during operation, simply
 by pushing the oil tube forward against  an internal  stop,  then returning
 it to operating position. The outside diameter of  the oil  nozzle is  sized
 to efficiently clean the inside of the steam nozzle of  any carbon deposits
 resulting from shutdowns of steam before oil. The quick disconnect
 feature of Series 5623 permits removal of the oil tube, opening a straight
 passage to the steam or air nozzle.

 The suggested oil  valve is  a North American Sensitrol (brass,   rated
 250  psi, 275 F). The oil pressure at  the oil valve inlet should be at least
 5 to 10 psi (OK to use a Ratiotrol).  The steam or compressed air  valve
 is a  Series  1832 Globe Valve  (bronze, rated 200 psig).

 Although the mountings for these atomizers provide  a place for installing
 a 4021-14  Pilot Tip,  the ability of this pilot to light the oil flame cannot
 be guaranteed because of the uncontrolled amount of air induced  through
 the register.
                                                                         250
                                              -0-3
           25       50       75       100
          Stoam or Air Pr«ffur« at Alopiictr in pti
500
          25       50       75       100
            St«am Pr«s>ur* at Atomit«r in p»i
                                            125
When using compressed air as an atomizing medium, air consumption in scfm is one-third of Ib steam/hr for the same pressure.
Example: An O8 atomizer uses 285 Ib/hr steam with 75 psi steam pressure or 285/3 = 95 scfm air with 75 psi air.
                                                                                                             '„ Drtt-4 Holts
       MOUNTING for -02 and -01 ATOMIZERS                             MOUNTING for -0 and -1 ATOMIZERS

t Opening in furnace shell or outer wad must be 54 * larger than tile dimension to allow for mounting plate fillet and draft.

-------
T
  NOHTH  AMERICAN Mlg. Co.
  Cleveland, OH 44105 USA
  DIMENSIONS
                                                                                           Bulletin 56.22/23. 5-80
                                                                                                         Page 2
                                                                                                                 Sl.orn Notlle
         c 5622-02-A & -02-8
         ; 5622-01-A & -01-B
         | 5622-0-A  & -0-8
         ° 5622-1-A  & -1-8
                                          V  '/  •>*/    i V   ts/  11/    i7/   i1/   x'/    i1/
                                          /I  /,  Z/14   I/,4  5/,  1/i    J/,   14   4/i    I/a
                                             J/  -»/    . V   cs/  i ix    ^ */   i1/   c V    i V
                                             /.  2 /i*   1 /«  5 /,  r/J    4 /,   1 /,   5 7,4   1 /,»
                                             X  314   iV,   6s/,  l'/*   S'/,   I1/,   S'X    lV*
    i   x,   y,  3*4   i5/.
                 fpt - femal. pipe thread (Anwicart Standard)
                                                      mot
              6%  17,4  S'/?   17,  67,4
             md< pipe thread (American Standard!
                                                                                      1*4
                                                                               Metric Conversions
                                                                               275 F  s 135 C
                                                                               1 psi   = 0.0703 kg/cm1
                                                                               1 gph  = 0.0631 t/s
                                                                               1 Ib   = 0.4536 kg
                                                                               1 scfm = 0.000 471 sm'/s
                                                                               1'    = 25.40 mm
        3-lpl Pipe Sin
          CM Intel
                                                          Bock Plot*
                                                                                                                       St«am NoixU

                                 • A-fpt Pip. Siw
                                Steam or CompresMd
                                     Air Inlet
                                                                                                                   CMMonU
                                                                                                                   Spid«r Unit
                                                                                              Series 5623 Atomizers
                            •+•
                                                                        -l" Km. 8" Unl«l
       PARTS LIST (S.I screw is a coek.t h.od K-20 x 3/16", IR77S-2020)

         Part No.   ^   -02-A      -02.B       -01-A      -OI-B
       Oil Nozzle
       Steam Nozzl
-It
Din-
in
ix-jT-n
en f ions
inches
?.A A. .n?
1 A B

XV V
F
^'/.
G
l'/
J
l1/.
M
IV
                  1-3289-1
                   3283-1
3-3289-2
3-3288-2
3-3289-3
3-3233-2
3-3289-4
3-3288-2
Part No. N(^ -0-A
Oil Nozzle V3-3289-S
Steam Nozzle J 3-3287-1
.0-8
3-3239-6
3-3287-2
-1-A
3-3289-7
3-3287-2
.1-8
3-3289-8
3-3287-2
     ; 5623-01-A & -01-8
    f 5623-0-A 4 -0-B
    °* 5623-1-A & -I-B
                                                                                                    4'/,
                                                                                                    4J/,
                                                                                                                  i'/»
                       iy,
                       I1/!
                                                                          To order, specify: "5622(or 5623)-(code for pipe sizel-detter
                                                                          for capacity) Atomizer Only with L {specify "L" dimension)."
                                                                              Example: 5623-02-A V,* Atomizer w/L dimension of 10*
         Port No.
     5622-     5622.     5622-     5622-
     2-A&-B   Ol-A&.B   O-A&.B   1-A&-B
                                                                      Part No.
Bod/
Copper Tubing
Globe  Valve
Oil Tube
0. T. Packing
Packing Nut
Packing Spring
Packing Seat
Sensitrol	
Steam  Tube
Stop Collar
                       3-760-3
                       3-310-7
                       1832-02
              3-760-2
              3-310-7
              1832-01
        3-724-3
        3-310-8
        1832-0
      3-724-2
      3-310-8
      1832-1
                       3-766-2    3-766-2
                       3-1069-1   3-1069-1
                       3-767-2    3-767-2
                        3-773-2   3-773-2
                        3-1069-2  3-1069-2
                        3-774-2   3-774-2
                        *,
                       3-770-1    3-770-1
                        I'lll'l
                        3-770-2
                      1813-02-C 1813-02-D  1813-01
                      3-3298-1
                      3-761-3
              3-3298-1
              3-761-3
        3-772-1
        3-761-4
      3-769-1
      3-770-2
      1813-01
      3-772-1
      3-761-4
        Body
        Oil Connection
        Oil Connection
            Locknut
        Oil Tube
        Retaining Ring
        Tru-seal Locknut
                                                                                 -^
                                                                                 5623-
                                                                               02-A&.B
                                                                5623-
                                                               01-A&-B
                                                                 5623.
                                                                0-A&.B
                                                                  5623.
                                                                 I.A&-B
                  3-3307-2
                  3-3233-1
3-3307-1
3-3233-1
3-3232-1
3-3310-2
3-3308-1
3-3309-1
3-3310-1
3-3308-1
3-3309-1
                  3-3232-1
                  3-3306-1     3-3306-1    3-3301-1    3-3301-1
                IR740-6360 IR740-6360  IR740-5390  IR740-6390
                      IR790-OUS              IR790-0120
Dotted parts olh.r than pip. fittings are for mounting atomizer
inside a burner. To replace these, specify part name, atomizer
series, burner series and size.
Parts not listed for Series S623 Atomizers are the same as for
Series S622 Atomizers.

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                 APPENDIX C

LOCATION  OF  MOBILE INCINERATOR INDICATING
           AND CONTROL DEVICES

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rt|	»--—-©-	

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I'          I          I'          I          II         I         II

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-   II          I          "          I          H          I          11

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Waste Feed Tank
(Trial Burn Only)

-------