EPA/540/2-89/019
      SUPERFUNDTREATABILITY
            CLEARINGHOUSE
               Document Reference:
PEI Associates, Inc. "BOAT Incineration of CERCLA SARMS at the John Zink Company
 Test Facility (Final Project Report)." Technical report prepared for U.S. EPA, ORD,
          HWERL, Cincinnati, OH. 375 pp. November 1987.
              EPA LIBRARY NUMBER:

           Superfund Treatability Clearinghouse - EUZM

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                 SUPERFUND TREATABILITY CLEARINGHOUSE ABSTRACT


 Treatment Process:      Thermal Treatment - Rotary Kiln

 Media:                  Soil/Generic

 Document Reference:     PEI Associates, Inc.  "BOAT Incineration of CERCLA
                         SARMS at the John Zink Company Test Facility (Final
                         Project Report)."  Technical report prepared for
                         U.S. EPA, ORD,  HWERL,  Cincinnati, OH.   375 pp.
                         November 1987.

 Document Type:          EPA ORD Report

 Contact:                Robert Thurnau
                         U.S. EPA-ORD
                         HWERL-ORD
                         26 W.  St. Clair Street
                         Cincinnati,  OH   45268
                         513-569-7629

 Site Name:               BOAT SARM-Manufactured Waste (Non-NPL)

 Location of  Test:        ORD-Edison,  NJ

 BACKGROUND;   This  report presents the results  of a treatability study of
 rotary kiln  incineration of a  synthetic "Superfund soil"  bearing a wide
 range of chemical  contaminants typically occurring at  Superfund sites.
 This surrogate soil is referred to as a synthetic analytical reference
 matrix (SARM), and was composed of clay,  sand,  silt,  topsoil,  and gravel.
 Two concentrations of contaminants were added  to this  material to produce
 SARM I and SARM II;  volatile and semivolatile  organics  (3000  ppm in SARM
 II  and 30,000 ppm  in SARM  I),  and metals  (1000 ppm in  SARM I and II).
 OPERATIONAL  INFORMATION;   Three 4-hour  test  burns were conducted on each
 SARM at the  John Zink pilot plant facility  in  Tulsa, Oklahoma  using a
 rotary kiln  incineration system capable of  handling 1000  Ib/hr of low BTU
 solids.   The runs  were conducted on  September  16-18, 1987.   The temperature
 and feed rates were  reasonably close to the  goals of 1800 F in the kiln,
 2000  F in the secondary chamber, and nominal  feed rates  of 1000 Ib/hr.
 Excess air was maintained at about 3% in  the kiln and  about 5% in the
 secondary. Emissions of  0,  CO^,  and CO were steady throughout the tests.
 PERFORMANCE;   The  contaminant  concentrations in  the ash,  scrubber water,
 and flue gas  were  measured  to  evaluate  the  performance of the  treatment.
 Little or no  volatiles were measured in  the  ash,  except for acetone and
 phthalate, and these appear to  be due to  sample  contamination.   Metal
 concentrations in  the ash were  unexpectedly  low  (50 to 80% lower than in
 the  feed).  As expected, cadmium  was at least  99.9% lower in the ash, due
 to  volatilization.   Only arsenic  concentrations  increased in the ash (more
 than double  the  concentrations  in the feed).  The scrubber  water was
essentially free of  all organics,  and  contained  only  low ppm  concen-
 trations  of metals.   Critical emission  parameters (oxygen,  HC1,  and CO)
were within RCRA allowable  limits.   The DRE  performance standard of 99.99%
3/89-41                                              Document Number:   EUZM
   NOTE:  Quality assurance of data may not be appropriate for all uses.

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 was achieved for the designed critical principal volatile organic
 contaminants for each SARM type.  The ORE for the principal semi-volatile
 organic contaminants show that anthracene was effectively destroyed.  ORE
 data for bis(2-ethylhexyl)phthalate showed three runs meeting the 99.99%
 criteria.
     The document discusses QA/QC procedures in detail.

 CONTAMINANTS;

 Analytical data is provided in the treatability study report.   The
 breakdown of the contaminants by treatability group is:
 Treatability Group

 WOl-Halogenated Aromatic
      Compounds

 W03-Halogenated Phenols,
      Cresols and Thiols

 W04-Halogenated Aliphatic
      Solvents

 W07-Heterocyclics and  Simple
      Aromatics
W08-Polynuclear  Aromatics

V09-0ther  Polar  Organic
      Compounds

WlO-Halogenated  Non-Polar
      Aromatic Compounds
Wll-Halogenated Non-Polar
     Aromatic Compounds
CAS Number
108-90-7
87-86-5
107-06-2
127-18-4

100-41-4
100-42-5
1330-20-7

120-12-7

67-64-1
117-81-7

7440-02-0
7440-47-3
7440-50-8

7439-92-1
7440-43-9
7440-66-6
Contaminants
Chlorobenzene
Pentachlorophenol
1,2-Dichloroethane
Tetrachloroethene

Ethylbenzene
Styrene
Xylenes

Anthracene

Acetone
Bis(2-ethylhexyl)phthalate

Nickel
Chromium
Copper

Lead
Cadmium
Zinc
3/89-41                                              Document Number:  EUZM
   NOTE:  Quality assurance of data may not be appropriate for all uses.

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   BOAT
AT THE JOH
        (
                                          OF CERCLA SARMS
                                        MPANY TEST FACILITY
                                      OJECT REPORT)
                                   Prepared by
                              PEI Associates, Inc.
                               11499 Chester Road
                             Cincinnati, Ohio  45246
                             Contract No.  68-03-3389
                               Work Assignment 1-7
                              Project No.  3724-7-1
                                  Prepared for

                      U.S. ENVIRONMENTAL PROTECTION AGENCY
                       OFFICE OF RESEARCH AND DEVELOPMENT
                HAZARDOUS WASTE ENVIRONMENTAL RESEARCH LABORATORY
                        ALTERNATIVE TECHNOLOGIES DIVISION
                                CINCINNATI, OHIO
                                  November 1987
THIS REPORT HAS BEEN PREPARED IN CONNECTION WITH THE DEVELOPMENT OF BOAT FOR
THE LAND DISPOSAL RESTRICTION RULES.  THIS REPORT IS A PRESENTATION OF DATA.
EPA'S ASSESSMENT OF WHETHER DATA REPRESENT TREATMENT BY BEST DEMONSTRATED
AVAILABLE TECHNOLOGY (BOAT) WILL BE PROVIDED IN THE TECHNICAL BACKGROUND
DOCUMENT FOR CERCLA SOIL/DEBRI WASTES.

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                                  CONTENTS


                                                                      Page



1.   Introduction                                                     1-1

2.   Summary of Results                                               2-1

     2.1  Critical  test burn parameters                               2-1
     2.2  Summary of operating conditions                             2-2
     2.3  Process sample data                                         2-4
     2.4  Treatment efficiency as measured by TCLP                    2-9
     2.5  Emission  test results                                       2-9

3.   Description of Incinerator and Process Operation                 3-1

     3.1  Incinerator description                                     3-1

4.   Sampling Locations and Test Methods Used                         4-1

     4.1  Sampling  locations and equipment operation specifications   4-1
     4.2  Process sampling procedures                                 4-1
     4.3  Stack gas sampling procedures                               4-5

5.   Quality Assurance Procedures and Results                         5-1

     5.1  Field sampling quality assurance                            5-1
     5.2  Continuous emission monitors                                5-1
     5.3  Laboratory quality assurance                                5-3

Appendices

A    Computer Printouts and Example Calculations                      A-l
B    Field Data Sheets                                                B-l
C    Laboratory Data and Analysis Report                              C-l
D    Stack Gas Sampling and Analytical Procedures                     D-l
E    Equipment Calibration Procedures and Results                     E-l
                                     ii

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                                   FIGURES

Number                                                                Page
 3-1      Rotary Kiln Incinerator Configuration for Solids            3-2
 4-1      The John Zink Company Rotary Kiln Incineration System and
            Feed and Residuals Sampling Sites for SARM I and II       4-2
 4-2      Operating Parameters Monitored by John Zink/PEI during
            SARM Test Burns                                           4-3
 4-3      Stack Gas Sample Location                                   4-6
                                     iii

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                                   TABLES
Number
Page
 1-1      Target Contaminant Levels for Synthetic Soils (SARMs)
            to be Used as Waste Feed for Incineration                 1-3
 2-1      Sumnary of Process Operating Data                           2-3
 2-2      Total  Waste Analysis for SARM Feed                          2-5
 2-3      Total  Waste Analysis for SARM Ash                           2-6
 2-4      Total  Waste Analysis for Scrubber Water                     2-7
 2-5      TCLP Values                                                 2-10
 2-6      Sunmary of Stack  Gas Sample and  Analytical  Procedures
            (SARM I  and  II  Test Burns)                                2-11
 2-7      Results for Critical  Emission Parameters  -  SARM I            2-13
 2-8      Results for Critical  Emission Parameters  -  SARM II           2-15
 2-9      Summary of Flue Gas  Conditions                               2-17
 2-10      Particulate Emission Data                                   2-19
 2-11      HC1  Emission Data                                            2-19
 2-12      Summary of Volatile  Organic Feed Rate Data                   2-21
 2-13      Summary of Volatile  Organic Stack Gas Concentration and
           Mass  Rate Data                                             2-22
 2-14      Summary of Volatile  Organic DRE  Data                         2-23
 2-15      Summary of Semi-Volatile  Organic Feed Rate  Data              2-24
 2-16      Summary of Semi-Volatile  Organic Stack  Gas  Concentration
           and Mass Rate Data                                         2-25
 2-17      Summary of Semi-Volatile  Organic DRE Data                    2-26
                                     IV

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                             TABLES (continued)
Number                                                                page
 2-18     Summary of Metals Emission Data                             2-20
 2-19     Summary of Continuous Emission Monitor Data SARM 1
            Test Number 1                                             2-31
 2-20     Summary of Continuous Emission Monitor Data SARM I
            Test Number 2                                             2-32
 2-21     Summary of Continuous Emission Monitor Data SARM I
            Test Number 3                                             2-33
 2-22     Summary of Continuous Emission Monitor Data SARM II
            Test Number 4                                             2-34
 2-23     Summary of Continuous Emission Monitor Data SARM II
            Test Number 5                                             2-35
 2-24     Summary of Continuous Emission Monitor Data SARM II
            Test Number 6                                             2-36
 2-25     Dioxin/Furan Results ng/g Feed                              2-37
 2-26     Dioxin/Furan Results ng/g Ash                               2-38
 2-27     Dioxin/Furan Scrubber Results                               2-39
 4-1      Process Sampling Locations, Equipment, and Methods           4-4
 4-2      Emission Sample Location, Equipment, and  Methods            4-8
 5-1      Field Equipment Calibration Data                             5-2
 5-2      CO Analyzer Calibration Data                                5-4
 5-3      C02 Analyzer Calibration Data                               5-5
 5-4      02 Analyzer Calibration Data                                5-6
 5-5      Volatile Organic Surrogate Recoveries  for Process Samples   5-8
 5-6      Volatiles Spike Recovery (Accuracy)  and Relative Percent
            Difference (Precision) for Feed Extract                   5-9
 5-7      Volatiles Spike Recovery (Accuracy)  and Relative Percent
            Difference (Precision) for Bottom Ash                     5-10

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                             TABLES (continued)
Number
 5-8      Volatiles  Spike Recovery (Accuracy)  and  Relative  Percent
            Difference (Precision) for Scrubber  Water                 5-10
 5-9      VOST Surrogate Percent  Recoveries                            5-11
 5-10     System Blank Data  for VOST Analyses                          5-13
 5-11     System Blank Data  for VOST Analyses                          5-13
 5-12     Semivolatiles Surrogate Percent  Recoveries                   5-14
 5-13     Semivolatiles Matrix  Spike Recovery  (Accuracy)  and
            Relative  Difference (Precision)  for  Feed                   5-17
 5-14     Semivolatiles Spike Recovery (Accuracy)  and Relative
            Difference (Precision)  for Ash                             5-17
 5-15     Semivolatiles Spike Recovery (Accuracy)  and Relative
            Difference (Precision)  for Scrubber  Water                 5-17
 5-16     System Blank Data  for Semivolatile Analyses                 5-18
 5-17     Semivolatiles Surrogate  Percent Recoveries                   5-19
 5-18     PEI  Waste Feed  Spike  Recoveries                              5-20
 5-19     PEI  Ash Spike Recoveries                                     5-21
 5-20     PEI  Scrubber Water Spike  Recoveries                          5-22
 5-21      PEI  Method  Spike Recoveries  Method 12  Train Samples          5-23
 5-22      Summary of  Method  12  Blank Analysis Data                     5-24
 5-23      Chloride Analysis Quality  Control Results                    5-26
 5-24      Dioxin/Furan  Results  Scrubber Surrogate  Recoveries           5-26
 5-25      Dioxin/Furan  Results  Feed  Surrogate Recoveries               5-27
 5-26      Dioxin/Furan  Results  Ash  Surrogate Recoveries                5-27

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                                  SECTION 1
                                INTRODUCTION

     The Hazardous and Solid Waste Amendments (HSWA) of 1984 prohibit the
continued land disposal of untreated hazardous wastes beyond specified dates.
The statute requires EPA to set "levels or methods of treatment, if any,
which substantially diminish the toxicity of the waste or substantially
reduce the likelihood of migration of hazardous constituents from the waste
so that short-term and long-term threats to human health and the environment
are minimized".  The legislation sets forth a series of deadlines at which
times further disposl of particular waste types is prohibited if the Agency
has not set treatment standards under Section 3004(m) or determined, based on
a case-specific petition, that there will be no migration of hazardous con-
stituents for as long as the wastes remain hazardous.
     In addition to addressing future land disposal of specific listed
wastes, the HSWA land disposal restrictions address the disposal of soil and
debris from CERCLA site response actions as well.  Sections 3004(d)(3) and
(e)(3) state that the soil/debris waste material resulting from a Superfund
financed response action or an enforcement authority response action imple-
mented under Sections 104 and 106 of CERCLA, respectively, will be subject to
the land ban beginning November 8, 1988.
     Because soil/debris waste often differs significantly from other types
of hazardous waste, the U.S. EPA is developing specific Section 3004(m) stan-
dards or levels for treatment of these types of Superfund wastes.  The stan-
dards will  establish Best Demonstrated and Available Treatment (BOAT) levels
through the evaluation of five readily available treatment technologies;
namely, soil washing, chemical treatment (KPEG), thermal desorption, inciner-
ation, and stabilization/fixation.  After November 8, 1988, Superfund wastes
in compliance with these regulations may be deposited in land disposal units;
wastes not in compliance will be banned from land disposal unless a variance
is issued.

                                     1-1

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     This report details part of the initial  work conducted from June to
November 1987 under Phase I of EPA's Superfund BOAT research program.  In
this segment of the program, a surrogate Superfund soil  bearing a wide range
of chemical contaminants typically occurring  at Superfund sites was subjected
to treatment by rotary kiln incineration.  A  complete series of test burns
was conducted, a battery of process and emission samples were collected and
analyzed, and the results are reported herein.
     The surrogate soil  is referred to throughout the text as SARM, which is
an acronym for Synthetic Analytical Reference Matrix.  It was prepared for
this test series under EPA Contract No. 68-03-3413, Work Assignment No. 7.
More than 27,000 pounds  of SARM were treated  by incineration during this
study.
     The SARM was composed of clay, sand, silt, topsoil, and gravel as
outlined below:
                    Percent by volume
                    Clay      30% (75% Kaolinite, 25% Bentonite)
                    Sand      20%
                    Silt      25%
                    Topsoil   20%
                    Gravel     5%
Chemicals were added to  the soil at two levels to produce SARM-I and SARM-II;
the target contaminant levels for each SARM are shown in Table 1-1.  Total
organic contaminants were expected to be present at high and low levels
(targeted at approximately 30,000 ppm and 3,000 ppm) as  shown in the table.
Metals were targeted at a total level of 1000 ppm in both SARM samples.
     The BOAT incineration testing was conducted at the  John Zink pilot plant
facility in Tulsa, Oklahoma using a rotary kiln incineration system capable
of handling 1000 Ib/h of low-Btu solids.  EPA provided more than 12,000
pounds of each SARM soil in order to conduct three 4-hour test burns (runs)
on each SARM.  Approximately one week prior to start up  of the test burns,
the soils were delivered to J. Zink in 48 55-gallon steel drums, each con-
taining 500-600 pounds of SARM I or SARM II.
                                     1-2

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TABLE 1-1.   TARGET CONTAMINANT LEVELS FOR SYNTHETIC SOILS (SARMs) TO BE
                 USED AS WASTE FEED FOR INCINERATION,
                                  ppm
Contaminant
Volatile*
Ethyl benzene
Xylene
Tetrachloroethylene
Chloro benzene
Acetone
1,2-Dichloroethane
Styrene

Semivolatiles
Anthracene
Bis(2-ethy1hexyl )phthalate
Pentachlorophenol

Metals
Lead
Zinc
Cadmium
Arsenic
Copper
Nickel
Chromium

SARM I

3,200
8,200
600
400
6,800
600
1.000
20,800

6,500
2,500
1,000
10,000

280
450
20
10
190
30
	 30
1,000
SARM II

320
820
60
40
680
60
100
2,080

650
250
100
1,000

280
450
20
10
190
30
	 30
1,000
                                  1-3

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                                  SECTION 2
                             SUMMARY OF RESULTS

     The results obtained for the test burns of SARM I  and II  are summarized
in this section.  Details on the process equipment and  operating conditions,
the sampling and analytical  procedures, and quality assurance  procedures and
results, can be found in succeeding chapters.  Calculations, field and lab-
oratory data reports, etc. are located in the appendices.

2.1  CRITICAL TEST BURN PARAMETERS
     The most important parameter studied was the degree to which the SARMs
were treated by incineration as measured by the Toxic Contaminant Leaching
Procedure or TCLP.  TCLP values for both the untreated  and treated SARMS are
compared and discussed in Section 2.4.  In addition to  TCLP, the following
chemical parameters were monitored throughout the test  burns:
     Stack Gases
          Volatiles (ethylbenzene,* xylene,* tetrachloroethylene, chloro-
          benzene, acetone, 1,2-dichlorethane, and styrene)
          Semivolatiles (anthracene,* bis(2-ethylhexyl)phthalate,* penta-
          chlorphenol, and dioxins)
          Metals (lead,* zinc,* cadmium, arsenic, copper, nickel, and chro-
          mium)
          Particulate*
          HC1*
          02, CO, and C02
*
  Critical parameter, per QAPP.
                                     2-1

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     Waste Feed
          Volatiles (same as above)
          Semivolatiles (same as above)
          Metals (same as above)
     Ash
          Volatiles (same as above)
          Semivolatiles (same as above)
          Metals (same as above)
     Scrubber Wastes
          Volatiles (same as above)
          Semivolatiles (same as above)
     Monitoring results for these chemical  measurements are summarized in
Sections 2.3 and 2.5 through 2.8.  Operating conditions throughout the tests
are discussed in Section 2-2.

2.2  SUMMARY OF OPERATING CONDITIONS
     Three 4-hour test runs were conducted  on each SARM, for a total  of six
runs.  The runs were conducted two per day  over the 3-day period of September
16-18, 1987.  Runs 1, 2, and 3 were conducted using SARM-I (high organics,
low metals) and Runs 4, 5, and 6 were conducted using SARM-11 (low organics,
low metals).  Equipment operations were normal  throughout each run.
     Table 2-1 summarizes the process operating data collected during each
test run, as well  as the average values for each test (i.e., for each group
of three runs).  Overall, the data in Table 2-1 show that the temperatures
and feed rates achieved were reasonably close to the goals (i.e., 1800F in
the kiln, 2000F in the secondary, and nominal  feed rate goal of 1000 Ib/h).
Excess air was maintained at about 3 percent in the kiln and about 5 percent
in the secondary during both tests.  Emissions  of 0, C0, and CO were steady
throughout, with CO remaining at less than  10 ppm at all times except for a
few brief excursions of 45 to 90 ppm, lasting for 1 to 5 minutes.
     A total of 13,932 Ib of SARM-I and 13,460  Ib of SARM-II were incinerated
over a course of 3 days involving 29 hours  and  22 minutes of testing.
     See Appendix B for detailed field data sheets recording process data at
30- to 40-minute intervals throughout each  run.
                                     2-2

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                    TABLE 2-1.  SUMMARY OF PROCESS OPERATING DATA
SARM-I
Location/Parameter
FEED
Time elapsed, h:min
Amount fed, Ib
Feed rate, Ib/h
KILN
Temperature, F
o2, %
SECONDARY
Temperature, F
o2, %
SCRUBBER
Flow, % max.
Slowdown, % max.
AP venturi , in. w.g.
STACK
0,, %
C02 %
CO, ppm
Run 1

4:23
4640
1059

1795
3.3
2004
4.1
72
0
23.0
5.8
10.1
<10
Run 2

3:45
3939
1050

1776
4.7
1997
6.0
70
0
24.8
6.3
9.6
<10
Run 3

4:54
5353
1092

1760
2.5
1995
4.6
76
0
23.9
6.1
10.2
<10
Avg.

4:21
4644
1067

1111
3.5
1999
4.9
73
0
23.9
6.1
10.0
<10
Run 4

4:06
4392
1071

1749
2.6
1985
4.1
72
0
26.2
5.1
10.9

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2.3  PROCESS SAMPLE DATA
     Tables 2-2, 2-3,  and 2-4 present the  results  of  chemical  analyses  (i.e.,
total waste analyses)  of the waste feed, ash  and scrubber water  samples  col-
lected during each test run.  EPA SW 846 Methods were used  to  develop these
analytical  values for  total  waste composition.  Samples  analyzed for semi-
volatiles and metals -vere collected as composites  over the  course of each
test; samples analyzed for volatiles were  collected as discrete  samples  at
the beginning, middle, and end of each run,  and composited  at  the time  of
analysis.
2.3.1  Feed Analyses (Table 2-2)
     The waste feed analyses show that the target  concentrations for most of
the contaminants were  reasonably  well achieved.  Some of the volatile com-
pounds were present at levels lower than desired,  but this  was anticipated.
Pentachlorophenol values were much lower than expected;  in  fact, pentachloro-
phenol was  found in measurable quantities  in  only  one of six SARM feed  samples
analyzed.  Semi-volatile surrogate recovery data  (Section  5.0  and Appendix  C)
for 2-fluorophenol and d5-phenol  are within expected  limits of the methodology
used which  would seem  to preclude poor extraction  recoveries as  the reason
for the non-detectable values.
2.3.2  Ash  Analyses (Table 2-3)
     The volatile compounds styrene, tetrachloroethylene,  and  chlorobenzene
were not detected in any of the ash samples.   Measurable quantities of  ethyl-
benzene, and xylene were found in the ash  of both  SARMs  and 1,2-dichloroethane
was found in the ash of SARM II,  but the amounts were small (in  the low
part-per-billion range) and typically at  levels within 2 to 3  times the
method detection limit.  Acetone was found in the  ash samples  of all  runs  for
both SARMs  at significant levels ranging from 190  to  790 pg/kg;  these  levels
are 24 to 99 times higher than the method  detection level  (8 vg/kg).
     On the average, the concentrations of acetone and phthalate found in  the
ash of SARM"I are similar to those found  in the  ash of SARM-II,  even though
the input waste feed levels for these compounds were  roughly 10 times  higher
in SARM-I than in SARM II.  This is suggestive of  sample contamination, and
the data should be interpreted with caution.  Significant  quantities of
phthalate were also found in several of the method blanks, and phthalates  are
known to be commonly encountered contaminants in  sample analysis.

                                     2-4

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                    TABLE 2-2.  TOTAL WASTE ANALYSIS FOR SARM FEED3


Parameter
VOLATILES, mg/kg
Ethyl benzene
Xylene
Tetrachloroethylene
Chlorobenzene
Acetone
1,2-Dichloroethane
Styrene
SEMIVOLATILES, mg/kg
Anthracene
Bis(2-ethylhexyl)
Method
detec-
limit

7.0
5.0
4.0
6.0
8.0
3.0
3.0

6.0
44.0


Run 1

3600
5800
b
340
3300
450
770

6200
2800

SARM I
Run 2

2400
4000
260
240
6000
140
580

8500
3300


Run 3

4000
6000
350
360
2700
340
810

5300
2200


Run 4

240
120
29
22
680
13
51

480
290

SARM II
Run 5

84
150
8.5
6.9
570
3.5
16

420
270


Run 6

330
520
36
30
270
28
67

440,.
NDC
   phthalate
  Pentachlorophenol

METALS, mg/kg

  Lead
  Zinc
  Cadmium
  Arsenic
  Copper
  Nickel
  Chromium

AVG. FEED RATE

  Ib/h
  kg/h

MOISTURE CONTENT

  Dean Stark Distil-
  lation % H20 only
3.3
4.2
0.12
0.12
0.04
 .42
 .30
0.
0.
0.30
        ND1
261
451
 26
 17
244
 28
 24
       1060
        482
       630
296
551
 25
 17
267
 30
 33
              1062
               483
292
526
 26
 20
261
 27
 39
             1092
              496
328
548
 26
 19
282
 30
 30
              1071
              487
                       ND1
301
508
 26
 19
250
 28
 27
              1086
               497
                        ND1
302
158
 26
 18
255
 28
 27
               1118
                508
              19.6
                                    22.9
  For target concentrations, see Table 1-1.
  Analytical result rejected for QA reasons.  See Section 5.2 for explanation,
  None detected.
                                     2-5

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                    TABLE 2-3.   TOTAL  WASTE  ANALYSIS  FOR  SARM ASH

Parameter
VOLATILES, yg/kg
Ethylbenzene
Xylene
Tetrachl oroethy 1 ene
Chlorobenzene
Acetone
1,2-Dichloroethane
Styrene
SEMIVOLATILES, vg/kg
Anthracene
Bis(2-ethylhexyl )
Method
detec-
tion
limit

7.0
5.0
4.0
6.0
8.0
3.0
3.0

37
63


Run 1

NDa
ND
ND
ND
440
ND
ND

ND
1600
SARM I

Run 2

19
34
ND
ND
420
ND
ND

ND
540


Run 3

ND
ND
ND
ND
630
ND
ND

ND
740


Run 4

8
11
ND
ND
190
ND
ND

ND
950
SARM II

Run 5

ND
6
ND
ND
210
5
ND

ND
710


Run 6

13
20
ND
ND
790
10
ND

ND
1300
   phthalate
  Pentachlorophenol      370       ND     ND     ND        ND       ND       ND

METALS, mg/kg
Lead
Zinc
Cadmium
Arsenic
Copper
Nickel
Chromium
VOLATILE PICs, ug/kg
2-Butanone
Methyl ene chloride
2-Chloroethyl vinyl
ether
4.2
0.12
0.12
0.04
0.42
0.30
0.30

25
2.8
5.0

56
217
<0.2
38
111
12
10

35
2.9
70

98
227
<0.2
36
132
15
14

ND
5.4
ND

107
250
<0.2
44
159
11
12

ND
4.2
ND

146
252
0.2
46
125
12
12

14b
ND
ND

75
199
<0.2
39
106
9.1
7

ND
ND
ND

88
237
<0.2
37
162
12
10

ND
ND
ND

a ND = Not detected.

  Estimated value less than method detection limit.
                                     2-6

-------
                    TABLE 2-4.   TOTAL WASTE ANALYSIS FOR SCRUBBER WATER

Parameter
VOLATILES, ug/liter
Ethyl benzene
Xylene
Tetrachl oroethyl ene
Chlorobenzene
Acetone
1,2-Dichloroethane
Styrene
SEMIVOLATILES, vg/liter
Anthracene
Bis(2-ethylhexyl)
Method
detec-
tion
limit

7.0
5.0
4.0
6.0
8.0
3.0
3.0

ND
3


Run 1

NDb
ND
ND
ND
ND
ND
ND

ND
ND
SARM I

Run 2

ND
ND
ND
ND
17
ND
ND

ND
5


Run 3

ND
ND
ND
ND
12
ND
ND

ND
2.3


Run 4

ND
ND
ND
ND
ND
ND
ND

ND
5
SARM II

Run 5

ND
ND
ND
ND
ND
ND
ND

ND
ND


Run 6

ND
ND
ND
ND
ND
ND
ND

ND
9

Influ-
ent3

ND
ND
ND
ND
ND
ND
ND



   phthalate
  Pentachlorophenol
METALS, yg/ml
0.4
ND
ND
ND
ND
Lead
Zinc
Cadmium
Arsenic
Copper
Nickel
Chromium
OTHER COMPOUNDS
DETECTED, yg/liter
Chloroform
Bromodichloromethane
0.105
0.003
0.003
0.001
0.011
0.008
0.008


1.6
2.2
1.8
2.1
2.4
0.15
0.6
0.32
2.4


5.7
ND
1.5
4.4
4.1
0.26
0.53
0.76
4.1


5.6
ND
2.3
1.8
1.9
0.15
0.48
0.27
1.9


4.8
ND
2.2
2.9
3.6
0.27
0.56
0.36
3.6


4.2
ND
2.0
1.7
2.0
0.18
0.59
<0.04
2.0


5.9
ND
4.8
3.3
5.8
0.41
1.1
0.27
5.8


8.6
2.4
NA
NA
NA
NA
NA
NA
NA


7.1
2.7
  Sample of scrubber water collected prior to the start of testing.
  organic content only.
  ND = Not detected
  NA - Not analyzed.
                                            Analyzed for
                                         2-7

-------
Compound
Average
 feed
 cone.
 mg/kg
                                          Ash cone.,  mg/kg
First
 run
Second
  run
Third
 run
Average
Acetone
  SARM I
  SARM II
Bis(2-ethylhexyl)
  phthalate
 4000
  506
0.440
0.190
 0.420
 0.210
0.630
0.790
 0.497
 0.397
SARM I
SARM II
2767
186
1.600
0.950
0.540
0.710
0.740
1.300
0.960
0.987
     The metals data for the ash samples are also interesting.   Prior to,the
testing, it was anticipated that most of the metals concentrations  in the ash
would be elevated compared to the waste feed due to combined  effects  of
retention of metals in the ash and losses of water and  organics  from  the  feed
during the incineration process; cadmium levels  in the  ash, however,  were
expected to be low due to volatilization of the  metal  in  the  kiln at  the  high
operating temperature of 1800F.  As expected, cadmium  levels in the  ash  were
quite low, at least 99.9 percent lower than the  waste feed  levels.  Surprising-
ly, all of the other heavy metal levels except for arsenic were  also  lower in
the ash (e.g., on the order 50 to 80 percent lower) than  in the  waste feed.
On the other hand, arsenic levels in the ash were more  than double  those  of
the feed levels, across the board.  An explanation for  these  unexpected
results is being sought.
2.3.3  Scrubber Water Analyses (Table 2-4)
     Scrubber water analyses indicate that it was essentially free  of all
organics fraw the SARM I and II feeds, except acetone,  which  appeared in  Runs
2 and 3 at low ppb levels, and bis(2-ethylhexyl)phthalate which  appeared  in 4
of the 6 runs, also at low ppb levels.  In both  cases,  the  amounts  detected
were only 2 to 3 times the method detection limits.  Pentachlorophenol was
also detected in the scrubber water from two of  the three runs on SARM I, at
4 and 8 ug/liter, levels which are 10 to 20 times higher  than the MDL. Two
                                     2-8

-------
volatile compoundschloroform and bromodichloromethane--were detected at low
ppb levels in the influent scrubber water (prior to any SARM testing)  and
throughout the test runs.  All of the metals were detected in the scrubber
water at low ppm levels for both SARMs.

2.4  TREATMENT EFFICIENCY AS MEASURED BY TCLP
     Toxic Characteristic Leaching Procedure (TCLP) test results are given in
Table 2-5 for the untreated and treated SARMS.
     (Discussion to be added when data are available.)

2.5  EMISSION TEST RESULTS
     Table 2-6 summarizes the sample and analytical methodology used for this
test program.  In summary, single modified Method 5 (semi-volatile organics)
and EPA Method 12 (metals) sample trains were run simultaneously over a 3- to
4-hour period during the incineration of SARM I and II.  Additionally, the
volatile organic sample train (VOST) was used to collect volatile samples
during the runs and continuous emission monitors (CEMS) were used to continu-
ously monitor gas stream composition for oxygen, carbon dioxide, and carbon
monoxide content.  All samples were collected after the venturi scrubbing
system to determine the concentrations and mass rates of the pollutants
listed in Table 2-6.
     Stack samples for the semi-volatile organics were  collected on XAD-2
resin.  The XAD-2, filter, and probe rinse residue were solvent extracted and
the concentrated extracts were analyzed by GC/MS.  Prior to the organics
analysis, probe rinse and filter samples were analyzed  gravimetrically to
determine particulate concentration per EPA Method 5 procedures.  An aliquot
from the 0.1 NaOH impinger of each MM5 train was also analyzed for chloride
content (as HCL) using ion chromatography.
     Metals samples were collected using an EPA Method  12 sample train.  This
train is identical to the standard EPA Method 5 train except that 0.1 N HN03
(nitric acid) is added to the impinger and used as the  sample nozzle and
probe rinse reagent.  Analysis for the listed metals was accomplished by
combining the probe rinse and filter fraction into a single sample and digest-
ing each sample using appropriate procedures in SW 846.  Analyses were per-
                                     2-9

-------
                          TABLE 2-5.   TCLP VALUES/
                                  rag/liter




VOLATILES
Ethyl benzene
Xylene (Total)
Tetrachloroethylene
Chlorobenzene
Acetone
1,2-Dichloroethane
Styrene
SEMIVOLATILES
SARM I
Untreatedb
(waste feed)
Run 1

49.7
84.6
3.59
6.47
282
18.9
2.10


Treatedb
(ash)
Run 1

0.65
1.05
0.04 1
0.04 1
0.74
0.10 u
0.11

SARM
Untreated0
(waste feed)
Run 4

7.31
15.8
0.68
0.79
26.1
0.48
0.58

II
Treated
(ash)
Run 4

0.19
0.23
0.10 u
0.10 y
0.14
0.10 y
0.10 y

 Anthracene
 Bis(2-ethylhexyl)
  phthalate
 Pentachlorophenol

METALS
Lead
Zinc
Cadmium
Arsenic
Copper
Nickel
Chromium
0.46
7.96
0.62
0.15 y
1.31
0.34
0.01 y
0.15 y
0.03 y
0.01 y
0.15 y
0.02 y
0.04 y
0.01 y
1.74
13.5
0.77
0.15 y
4.12
0.65
0.07
0.15 y
0.49
0.01 y
0.15 y
0.26
0.05
0.04
y = Detection limit.
1 = Less than detection limit; estimated value.


a Data generated by Lee Wan Associates, Atlanta, Georgia, under EPA Contract
  No. 68-03-3393.
b Waste feed:  Sample No. ZSARM-I-l-F, Seal No. 8303 and 8304.

c Ash (unquenched):  Sample No. ZSARM-I-l-A, Seal No. 8331 and 8332.

d Waste feed:  Sample No. ZSARM-II-4-F, Seal No. 8369.

e Ash (unquenched):  Sample No. ZSARM-II-4-A, Seal No. 8368.

                                     2-10

-------
TABLE 2-6.   SUMMARY  OF  STACK GAS SAMPLE AND ANALYTICAL PROCEDURES
                  (SARM I  AND II TEST BURNS)
Sample
Identification
Stack Gas
(after scrubbing
system)







Parameter
POHCS
- Volatiles
Ethyl benzene
Xylene
Chlorobenzene
Acetone
1,2-Dichloroethane
Styrene
Tetrachloroethylene
- Semi-volatiles
Anthracene
Pentachlorophenol
Bis(2-ethylhexyl )phtalate
"Particulate
HC1
Metals
Volumetric Gas Flow
- Temperature
- Moisture content
CO
co2
2
Sample Method
S012
(VOST protocol)
Modified Method
5
EPA Method 5
EPA Method 5
EPA Method 12
EPA Methods 1-4
EPA Method 10
EPA Method 3A
EPA Method 3A
Analytical Method
GC/MS
(VOST)
GC/MS
SW 846-8270
Gravimetric
(EPA 5)
Ion chromatography
(EPA 300.0)
SW 846
(ICP/AA)
  -
NDIR
NDIR
Zirconium
cell
No. of
Samples
18 pairs
6
6
6
6
"
continuous
continuous
continuous

-------
formed by either Atomic Absorption (AA) or Inductively Coupled Plasma Spectro-
scopy (ICP).
     Volatile organic samples were collected using the VOST sample train.
This train consists of paired sorbent traps using Tenax and Tenax-Charcoal
traps in series.  Three sample pairs were collected over each sample period.
Analysis was conducted by GC/MS.
     During each test, flue gas flow rate, temperature, and moisture content
were measured using EPA Method 1 through 4 procedures.  Additionally, CEM's
were used to continuously record 0^, C0?, and CO concentrations during each
test period.  The following subsections detail  the results of the sample
program.
2.5.1  Critical  Emission Parameters Results Summary
     Tables 2-7  and 2-8 summarize the critical  emission parameters for the
SARM I and SARM  II test burns.  In summary, the data show:
0    Particulate concentrations corrected to 7  percent (L were below the RCRA
     allowable limit of 0.08 gr/dscf for each SARM type.
0    Measured HCL emission rates in Ib/h were considerably less than the RCRA
     allowable of 4.0 Ib/h for each SARM type.
0    The average stack gas concentration of CO  was less than 23 ppm during
     each test.
0    The ORE performance standard of 99.99 percent was achieved for the
     designated  critical volatile POHC's for each SARM type.  The ORE data
     for the semi-volatile POHCs show that anthracene was effectively
     destroyed since the amount in each emission was less than the method
     detection limit (yg/sample) resulting in DRE's of greater than 99.99
     percent.  ORE data for bis(2-ethylhexyl)phthalate showed three of zinc
     sample runs meeting the 99.99 percent criteria.  Sample contamination
     (background level) problems make these data suspect as discussed in
     Subsection  2.5.4.
Overall, the sampling and analysis were conducted as described in the QAPP
for this project and no major field sampling problems were encountered which
could significantly impact test results.
2.5.2.  Summary  of Flue Gas Conditions
     Table 2-9 summarizes flue gas data as measured during this test program.
The modified Method 5 and metal sample trains were run simultaneously at the
same location using isokinetic and cross-sectional traverse sample techniques,
                                     2-12

-------
        TABLE  2-7.   RESULTS  FOR  CRITICAL  EMISSION  PARAMETERS  -  SARM  I
Parameter
Test date (1987)
Test time (24-h)
SARM I feed rate, Ib/h
Total ethyl benzene feed rate,
Ib/h
Total xylene feed rate, Ib/h
Total anthracene feed rate,
Ib/h
Total bis(2-ethylhexyl)
phthalate feed rate, Ib/h
Exhaust gas data
Volumetric flow, dscfm
Oq/3
2 *
rn 
-------
TABLE 2-7 (continued)
                                               Test No.
     Parameter
Average
Exhaust gas data continued.

  ORE, %C
Ethyl benzene
Xylene
Anthracene
Bis (2-ethylhexyl)
phthalate
99.999
99.999
>99.99
99.990
99.999
99.999
>99.99
99.999
99.998
99.998
>99.99
99.967
99.999
99.999
>99.99
99.985
   Dry basis, determined as average values  from 0^.  CCL.  and CO continuous
   monitors.

   ND = None  detected.

   Destruction removal  efficiency = 1b/h  jg Tn1b/h out  x 100
                                     2-14

-------
TABLE 2-8.  RESULTS FOR CRITICAL EMISSION PARAMETERS - SARM II
Parameter
Test date (1987)
Test time (24-h)
SARM I feed rate, Ib/h
Total ethyl benzene feed rate,
Ib/h
Total xylene feed rate, Ib/h
Total anthracene feed rate,
Ib/h
Total bis(2-ethylhexyl)
phthalate feed rate, Ib/h
Exhaust gas data
Volumetric flow, dscfm
0 %b
2* K
CO *
2' u
CO, ppm (dry)
Particulate concentration,
gr/dsct @ 7% 02
Emission rates, Ib/h
Particulate
HC1
Ethyl benzene
Xylene
Anthracene
Bis(2-ethylhexyl)
phthalate
(continued)

1
9/17
1655-2015
1071
0.22

0.11
0.45

0.27


1352
5.1
11.0

0.007


0.09
0.02
5.3 x 10"6
8.9 x 10"6
NDb
2.1 x 10"5


Test No.
2
9/18
0944-1308
1086
0.08

0.14
0.39

0.25


1456
5.6
10.8
<10
0.006


0.08
0.02
3.7 x 10"6
1.3 x 10"5
ND
1.0 x 10""5



3
9/18
1350-1718
1118
0.30

0.47
0.39

NDa


1413
5.4
11.1
<10
0.005


0.07
0.01
3.2 x 10"6
8.9 x 10"6
ND
6.2 x 10"5


Average


1092
0.2

0.24
0.41

0.17


1407
5.4
11.0
<10
0.006


0.08
0.02
4.1 x 10"6
1.0 x 10"5
ND
3.6 x 10"4


                               2-15

-------
TABLE 2-8 (continued)
Parameter
Exhaust gas data continued.
ORE, %c
Ethyl benzene
Xylene
Anthracene
Bis (2-ethylexyl)
phthalate
a ND = None detected.

Test No.
123 Average


99.998 99.995 99.999 99.998
99.992 99.990 99.998 99.996
>99.99 >99.99 >99.99 >99.99
99.992 99.600 - 99.796


   monitors.
   Destruction removal  efficiency = 1b/h jg Tnlb/h out  x 100
                                     2-16

-------
                                                 TABLE  2-9.   SUMMARY  OF  FLUE  GAS  CONDITIONS
ro
i

Run
No.
SAI-SV-1

SAl-f.-l
SAI-SV-2

SAI-M-2
SAI-SV-3

SAI-r,-3
SAII-SV-1

SAII-M-1
SAII-SV-2

SAII-M-2
SAII-SV-3

SAII-M-3

Date
Time

(1987) and
(24 hours)
9/16; 1020-1413

9/16;
9/16;

9/16;
9/17;

9/17;
9/17;

9/17;
9/18;

9/18;
9/18;

9/18;

1020-1245
1625-2030

1628-1955
1041-1409

1044-1324
1655-2015

1700-1936
0944-1308

0933-1234
1350-1718

1337-1639

Sample
Type
Part. /HC1 /semi -
volatiles
Metals
Part. /HC1 /semi -
volatiles
Metals
Part./HCl/semi-
volatiles
Metals
Part./HCl/semi-
volatiles
Metals
Part./HCl/semi-
volatiles
Metals
Part./HCl/semi-
volatiles
Metals
SARM
I
Volumetric Flow Ratea
acfm
3387

3610
3403

3352
3512

3767
34?"

3479
3693

3701
3761

3659
dscfm
1407

1525
1327

1357
1377

1477
1340

1364
1443

1469
1415

1411



Temperature Moisture

Gas


Composition
11 F Content, % 02% C02%
180

180
180

180
181

181
181

181
181

180
181

182
48.8

47,
51,

50.
52.

52.
52.

52.
52.

51.
54.

53.

,9
.9

1
0

0
3

0
4

7
1

0
5.4

5.4
5.8

5.8
5.4

5.4
5.1

5.1
5.6

5.6
5.4

5.4
10.8

10.8
10.4

10.4
10.6

10.6
11.0

11.0
10.8

10.8
11.1

11.1
CO-ppm
< 12

< 12
< 10

< 10
< 17

< 17
< 23

< 23
< 16

< 16
< 11

< 11
                   Volumetric gas  flow rate in actual cubic feet per minute (actm) at stock  conditions and dry  standard cubic feet  per

                   minute (dscfm)  at 68F, 29.92 in Hg, and zero percent moisture.


                   Gas composition data represents the average value obtained from CEMs for  each test period.

-------
     Flue gas flow rates were consistent throughout the test program ranging
between 3300 and 3800 acfm (1300 to 1500 dscfm).   Flue gas temperature av-
eraged about 180F with moisture contents of between 48 and 54 percent by
volume.  Since the gas stream appeared saturated  and contained water drop-
lets, two moisture determinations were made:  the first involved volumetri-
cally determining the amount of water collected during each test and the
second determination involved calculating the moisture content using the
vapor pressure of water at the measured stack temperature and pressure.  In
each case, the lower value was reported as specified in EPA Method 4.   During
three of the twelve sample runs (SAI-M-1 and 3 and SAII-SV-1), the silica gel
impinger broke under high vacuum as a result of the large quantities of
water collected in the impinger section of the sample training.  Sampling was
discontinued, the broken impinger changed, and sampling resumed after the
appropriate system leak-checks were performed.  Because a portion of the
silica gel was lost and could not be weighed, the volumetrically determined
                                                                        i
moisture contents for the runs are biased somewhat low.  No significant bias
in emission results is believed to have occurred  as a result of this problem.
     Gas composition data were continuously recorded throughout each test
using continuing emission monitors for 0,,, C02, and CO.  The strip charts
were reduced to 15 minute averages and reported values represent the average
value obtained over the 4 hour burn period.  The  gas composition data show 02
content ranging between 5.1 and 5.8 percent; C02  ranging between 10 and 11
percent; and CO values of less than 20 ppm (dry basis).  It should be noted
that during five of the six SARM burns excursions in CO concentration of
between 45 and 90 ppm were observed typically lasting less than 5 minutes.
2.5.3  Particulate and HC1 Emission Data
     Tables 2-10 and 2-11 summarize the particulate and HC1 emissions data
from this test program.  Concentrations are expressed in grains per dry
standard cubic feet (gr/dscf) and mass rate data in Ib/h.  The product of the
flue gas flow rate and concentration yields the mass emission rate.  Volumetric
flow rates (in dscfm) as measured by each individual sample train were averaged
and the resulting average value (see Tables 2-7 and 2-8) for each test period
was used in calculating mass rates.
     For the SARM I burns, the particulate concentration corrected  to  7
percent 0? averaged 0.0133 gr/dscf with a corresponding average mass rate of

                                     2-18

-------
        TABLE 2-10.  PARTICULATE EMISSIONS DATA
Test No.
SARM I
SAI-SV-1
SAI-SV-2
SAI-SV-3
Average
0 SARM II
SAII-SV-1
SAII-SV-2
SAII-SV-3
Average
Concentration
as measured, gr/dscf

0.0156
0.0166
0.0123
0.0148

0.0079
0.0061
0.0056
0.0065
Concentration
corrected to
7% 02 gr/dscf

0.014
0.015
0.011
0.0133

0.007
0.006
0.005
0.006
Mass rate,
Ib/h

0.19
0.19
0.145
0.175

0.09
0.08
0.07
0.08
            TABLE  2-11.   HC1  EMISSION  DATA

Test No.
SARM I
SAI-SV-1
SAI-SV-2
SAI-SV-3
Average
0 SARM II
SAII-SV-1
SAII-SV-2
SAII-SV-3
Concentration
gr/dscf

.004
.0045
.003
0.0038

.0016
.0014
.0009
Mass Rate
Ib/h

0.05
0.05
0.03
0.043

0.02
0.02
0.01
Average
0.0013
0.017
                           2-19

-------
 approximately  .175 Ib/h.  HC1 concentrations averaged 0.0038 gr/dscf with an
 average mass rate of 0.043 Ib/h.  For the SARM II burns, the average
 corrected participate concentration was 0.0065 gr/dscf with an average mass
 rate of 0.08 Ib/h.  HC1 concentrations averaged 0.0013 gr/dscf with an
 average mass rate of 0.017 Ib/h.
     It should be noted that run SAI-SV-1 was conducted at a non-isokinetic
 sample condition (approximately 85 percent) which would tend to bias parti-
 culate measurements on the high side.  Based on the relative consistency
 between concentration measurements, no significant bias in particulate mea-
 surements is believed to have occurred.  All other sample runs were conducted
 within the isokinetic sample specifications (between 90 and 110 percent)
 detailed in EPA Method 5.
 2.5.4  POHC Emission Data and Destruction Removal Efficiency (DRE)
     Tables 2-12 through 2-17 summarize the volatile and semi-volatile or-
 ganic feed and mass emission data as well as the DRE for each compound.  Also
 included for informational purposes are the Method Detection Limits (MDL) for
 the feed and stack samples.   Individual compound feed rates were determined
 using the waste composition  and incinerator feed rate data detailed in Sec-
 tions 2.2. and 2.3.  For the volatile organic data, (Tables 2-12 through
 2-14), concentrations in nanograms per liter (ng/1) represent the average
 concentration determined from the three VOST samples collected during each
 SARM burn.  Mass rates were  then calculated using the average concentration
 and volumetric flow rate data for each test.
     Per the QAPP for this project, ethyl benzene and xylene were chosen as
 critical  parameters to evaluate incinerator performance in effectively de-
 stroying volatile organic compounds.  For the SARM I tests, ethyl benzene
 stack gas concentrations ranged between 2.7 and 11.3 ng/1  with corresponding
                                       -5             -5
mass emission rates of between 1.4 x 10   and 6.0 x 10   Ib/h.  For the SARM
 II tests, stack gas concentrations ranged between 0.6 and 1.0 ng/1. with
 corresponding mass emission  rates of between 3.2 x 10"  and 5.3 x 10~  Ib/h.
 Overall, the DRE's for ethylbenzene were greater than 99.99 percent for each
 run.  SARM I xylene stack gas concentrations ranged between 5.8 and 15.1 ng/1
                                                          -5             -5
with corresponding mass emission rates of between 3.1 x 10   and 8.0 x 10
 Ib/h, respectively.  SARM II xylene concentrations ranged between 1.7 and 2.5
ng/1 with corresponding mass emission rates of between 8.9 x 10   and 1.3 x

                                     2-20

-------
                                   TABLE 2-12.  SUMMARY OF VOLATILE ORGANIC FEED RATE DATA
ro
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Test No.



1
Feed Rate Ib/h 1060


Analyte
Ethyl benzene
Xyleneb
Tetrachloro-
ethylene
Chlorobenzene
Acetone
1,2-Dichloro-
ethane
Styrene
a
Feed rate =
L
Concen-
tration
ppm
3600
5800
ND

340
3300
450

770
Feeda
rate
Ib/h
3.4
5.5
_

0.32
3.1
0.42

0.73
Total SARM Feed
Analyte
Critical parameters


SARM
2
I
SARM II
3
1062
Concen-
tration
ppm
2400
4000
260

240
6000
140

580
Rate (Ib/h)
Feed
rate
Ib/h
2.3
3.8
0.24

0.23
5.6
0.13

0.55
1092
Concen-
tration
ppm
4000
6000
350

360
2700
340

810
Feed
rate
Ib/h
3.7
5.5
0.32

0.33
2.5
0.31

0.74
1
1071
Concen- Feed
tration rate
ppm Ib/h
240 0.22
120 0.11
29 0.03

22 0.02
680 0.6
13 0.01

51 0.05

2
1086
Concen-
tration
ppm
84
150
8.5

6.9
570
3.5

16
Feed
rate
Ib/h
0.08
0.14
0.01

0.01
0.5
0.003

0.015
Minimum Method Detection Limits:
3

1118
Concen-
tration
ppm
330
520
36

30
270
28

67
(Total ppm)
Feed
rate
Ib/h
0.3
0.47
0.03

0.03
0.24
0.03

0.06

concentration (ppm)
per QAPP

*







- Ethyl benzene
- Xylene
7
5
- Tetrachloroethylene 4














- Chlorobenzene
- Acetone
6
8
- 1,2-Dichloroethane 3







- Styrene
3
.0
.0
.0
.0
.0
.0
.0















-------
                  TABLE 2-13.  SUMMARY OF VOLATILE ORGANIC STACK GAS CONCENTRATION AND MASS RATE DATA
                                   SARM I
                                                                  SARM II
   Test No.
                                                    1
   Analyte   ng/lc
Ib/h     ng/1      Ib/h     ng/1      Ib/h       ng/1      Ib/h      ng/1      Ib/h      ng/1      Ib/h
   Ethyl-5~42.9 x 10"5  2.71.4 x 10"5  11.36.0 x 10"5  1.05.3 x 10"6  0.73.7 x 10"6  0.63.2 x 10"6
   benzene

   Xylene     6.3   3.3 x 10"5  5.8   3.1 x 10"5  15.1   8.0 x 10"5  1.7   8.9 x 10"6  2.5   1.3 x 10"5  1.7   8.9 x 10"6

   Tetrachlo- 0.04  2.1 x 10"7  0.25  1.3 x 10"6   1.7   9.0 x 10"6  0.1   5.3 x 10"7  0.2   1.1 x 10"6  0.5   2.6 x 10"6
   roethylene

   Chloro-    0.8   4.2 x 10"6  0.3   1.6 x 10"6   3.3   1.7 x 10"5  0.17  8.9 x 10~7  0.23  1.2 x 10"6  0.2   1.1 x 10"6
   benzene
?  Acetone    5.8   3.1 x 10"5  3.9   2.1 x 10"5   5.1   2.7 x 10"5  NDb

                                0.25  1.3 x 10"6   1.3   6.9 x 10"6  NDb
ro
ro
                                                                                       NDL
                                                                                       NDL
                                                                                  0.4   2.1 x 10

                                                                                  0.1   5.3 x 10
                                                                                                                       -6
                                                                                                                    -7
1,2-Dich-  NDU
1oroethane

Styrene    3.4   1.8 x 10"5  1.7   9.0 x 10"6  20.3   1.1 x 10"4  4.0   2.1 x 10"5  0.2   1.1 x 10"6  0.3   1.6 x 10"6
   ? Concentration  in nanograms per liter (ng/1).
     None detected.
                                         Minimum Method Detection Limit (MDL):
                                                               Total Nanograms
                                         -  Ethylbenzene:            2.0
                                         -  Xylene:                  4.0
                                         -  Perchloroethane:         1.0
                                         -  Chlorobenzene:           0.7
                                         -  Acetone:                 5.0
                                         -  1,2-Dichloroethane:      1.0
                                         -  Styrene:                 2.0

-------
                     TABLE 2-14.   SUMMARY OF VOLATILE ORGANIC  ORE DATA









ro
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CO





Test No.


Analyte
Ethyl benzene
Xylene
Tetrachloro-
ethylene
Choloro-
benzene
Acetone
1,2-Dfchloro-
benzene
Styrene
SARH 1
1 2 3
Mass Mass Mass
Feed emission Feed emission Feed emission
rate rate ORE* rate rate ORE rate rate ORE
Ib/h Ib/h S Ib/h Ib/h S Ib/h Ib/h S
3.4 2.9 x IO"5 99.999 2.3 1.4 x IO"5 99.999 3.7 6.0 x 10"5 99.998
5.5 3.3 x 1C'5 99.999 3.8 3.1 x IO"5 99.999 5.5 8.0 x 10"5 99.998
HDb 2.1 x 10"7  0.24 1.3 x 10"6 99.999 0.32 9.0 x ]0"6 99.997

0.32 4.2 x 10"6 99.998 0.23 1.6 x 10"6 99.999 0.33 1.7 x 10"5 99.995

3.1 3.1 x IO"5 99.999 5.6 2.1 x IO"5 99.999 2.5 2.7 x 10~5 99.999
0.42 NO  0.13 1.3 x 10"6 99.999 0.31 6.9 x IO"6 99.998

0.73 1.8 x IO"5 99.998 0.55 9.0 x IO"6 99.998 0.74 1.1 x 10"* 99.985


Feed
rate
Ib/h
0.22
0.11
0.03

0.02

0.6
0.01

0.05

1
Mass
Mission
rate
Ib/h
5.3 x 10*6
8.9 x 10'6
5.3 x 10"7

8.9 x 10"7

ND
NO

2.1 x IO"5


Feed
ORE rate
X Ib/h
99.998 0.08
99.992 0.14
99.998 0.01

99.996 0.01

 0.05
 0.003

99.958 0.015
SARM 11
2
Mass
emission
rate
Ib/h
3.7 x 10"6
1.3 x IO"5
1.1 x IO"6

1.2 x 10"6

NO
NO

1.1 x 10"6





3

ORE
t
99.995
99.990
99.989

99.988


-._

99.993
Feed
rate
Ib/h
0.3
0.47
0.03

0.03

0.24
0.03

0.06
Mass
emission
rate ORE
Ib/h 1
3
8
2

1

2
5

1
.2 x
.9 x
.6 x

.1 x

.1 x
.3 x

.6 x
IO"6 99.999
IO"6 99.998
IO"6 99.991

IO"6 99.996

IO"6 99.999
IO"7 99.998

IO"6 99.997
I ORE
* OKt
       1b/h(ln) - Ib/h (out)
ln) -
 1b/h
               (In)
None detected.

-------
                              TABLE 2-15.   SUMMARY OF SEMI-VOLATILE ORGANIC FEED RATE DATA
ro
i
ro

Test No.
Feed Rate, Ib/h
Analyte
Anthracene
Pentachlorophenol
Bis(2-ethy1-
hexyl)phthalateD


Concen-
tration
ppm
6200
NDC
2800

1
1060
Feed
rate
Ib/h
5.8
2.6
SARM
2
1062
Concen-
tration
ppm
8500
630
3300
I

Feed
rate
Ib/h
8.0
0.59
3.1

3
1092
Concen-
tration
ppm
5300
NDC
2200


Feed
rate
Ib/h
4.85
2.0


Concen-
tration
ppm
480
NDC
290

1
1071
Feed
rate
Ib/h
0.45
0.27
SARM
2
1086
Concen-
tration
ppm
420
NDC
270
II

Feed
rate
Ib/h
0.39
0.25

3
1118
Concen-
tration
ppm
440
NDC
ND


Feed
rate
Ib/h
0.39
    c  A -,* /ik/k\       Concentration (ppm)
    Feed rate (Ib/h) = Total SUM Feed RateTlb
  " Critical parameters per QAPP.

    None detected.
Minimum Detection Limit (MDL-ppm)


Anthracene:                  6

Pentachlorophenol:           3.3

Bis(2-ethylhexyl)phthalate: 44.0

-------
TABLE 2-16.  SUMMARY OF SEMI-VOLATILE ORGANIC STACK GAS CONCENTRATION AND MASS RATE DATA
SARM I


ro
i
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en
Test No. 1
Concen- Mass
tration rate
Analyte yg/m3 Ib/h
Anthracene NDa 	
Pentachloro- ND 	
Bis(2-ethyl- 46.2 2.5 x
hexyl ) 10"1*
phthalate
a None detected.
2 3
Concen-
tration
yg/m3
ND
ND
3.0

Mass Concen-
rate tration
Ib/h yg/m3
	 ND
	 ND
1.5 x 124.2

Mass
rate
Ib/h
	
	
6.6 x
10"1*

Concen-
tration
yg/m3
ND
1.5
4.2
MDL
1
Mass
rate
Ib/h
	
7.6
2.1
10"5
(total
SARM
2
Concen-
tration
yg/m3
ND
x ND
x 190.5
yg/sample):
II

Mass
rate
Ib/h
	
	
1.0 x
10" 3


3
Concen- Mass
tration rate
yg/m3 Ib/h
ND 	
ND 	
11.3 6.2 x
10"5

                                                 Anthracene:          0.4  -  2.9  yg
                                                 Pentachlorophenol:   0.3  pg
                                                 Bis(2-ethylhexyl)-   0.4  yg
                                                   phthalate

-------
ro
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cr>
                          TABLE 2-17.   SUMMARY OF  SEMIVOLATILE  ORGANIC ORE  DATA

Test No.


Antlyte
Anthracene
Pentachloro-
phenol
B1s(2-ethyl-
nexjl)
phthalate


Feed
rate
Ib/h
5.6
ND

2.6



1
Hast
rate ORE
Ib/h t
ND* >99.99
NO

2.5 X10~* 99.990




Feed
rate
Ib/h
B.O
0.59

3.1


SARH I
2
Mass
rate
Ib/h
ND
ND

1.5 x





ORE
I
>99.99
>99.99

ID"5 99.999




Feed
rate
Ib/h
0.45
ND

2.0



3
Mass
rate
Ib/h
ND
ND

6.6 X10"4




Feed
ORE rate
* Ib/h
>99.99 0.39
ND

99.967 0.27



1
Mass
rate ORE
Ib/h t
ND >99.99
7.6 x 10"6 

2.1 x 10"5 99.992




Feed
rate
Ib/h
0.39
ND

0.25


SARH II
2
Mass
rate ORE
Ib/h X
ND >99.99
ND

1.0 x 10"3 99.600




Feed
rate
Ib/h
0.39
ND

NO



3
Mass
rate
Ib/h
NO
NO

6.2 x





ORE
t
>99.99


ID'5 -


           * None detected.

-------
10   Ib/h.   The calculated DRE's  for xylene were at least  99.99 percent  for
each test period.
     Analyses for  volatile organic compounds including perchloroethane,
chlorobenzene, acetone, 1,2-dichloroethane, and styrene were  also  conducted.
With the exception of those samples (either feed or stack  gas in which  com-
pound concentrations were below the MDL)  DRE's of at least 99.99 percent were
achieved.  Note that the calculated ORE for styrene was less  than  99.99
percent for SARM I run number 3 and SARM II run number 1.   However,  the
overall ORE average for each SARM level is 99.99 percent for  this  compound.
     All samples contained at least one analyte at a level five times the
detection limits reported in the  tables.   Levels of analyte ranged from the
detection limit to more than 100  times the detection limit.  In view of the
extremely high surrogate recoveries encountered for bromoflurobenzene (see
Section 5.0, Appendix C), values  for the late-eluting compounds (most espe-
cially ethyl benzene, styrene, and the xylenes) may be high by the  factor
about 100% exhibited by the bromoflurobenzene.  Since response factors remain
stable  (as demonstrated by the initial calibration check at the beginning of
the day and an additional calibration check as the end of the day) and, in
general, the blanks do not exhibit these inflated surrogate compound recov-
eries, the occurrence of elevated surrogate compound recoveries in the course
of the performance of VOST analyses must be considered a matrix effect.   The
classic means of demonstrating the operation of a matrix effect, namely,
repeated analysis of the same sample, repeated preparation and analysis of
the same sample, and occurrence of the matrix effect throughout all  analyses
of the  sample, cannot be performed in the VOST assay, since the VOST sample
consists only of a single set of sampling tubes and the compounds  which are
desorbed from the sampling tubes are analyzed in the initial  analysis.  No
VOST sample can be re-analyzed.  VOST samples are know to contain high levels
of water, since stack emissions contain high levels of water.  Large quan-
tities  of water introduced into a chromatographic analysis and/or into a mass
spectrometer will distort the chromatography and will cause  relative signal
levels  for  the compounds to be distorted.  Additional components of the stack
gases  such  as various acids can also have the effect of perturbing the chroma-
tography, and stack emissions are often highly acidic.
                                     2-27

-------
     The Method 5040 QC (VOST) measures were executed with  acceptable  results,
but sample surrogate recoveries are often seen to be above  the  50-150% cri-
terion for acceptability of the method.  No corrections  were applied to the
stack emission results to account for inflated surrogate compound recoveries;
particularly for ethylbenzene, styrene, and xylenes.  Uncorrected ethylben-
zene and xylene emission results and subsequent DRE's were  at least 99.99
percent making corrections unnecessary.  If styrene emissions from SARM I
test 3 and SARM II test 1 are corrected for the inflated surrogate recoveries,
DRE's of at least 99.99 percent would be achieved.
     Tables 2-15 through 2-17 summarize the semi-volatile organic feed, mass
rate, and ORE data.  Minimum method detection limits are also shown.   Analyte
feed rates were determined by dividing the measured concentration (ppm) by
the SARM feed rate in Ib/h.  Note that only one of six SARM feed samples
contained pentachlorophenol at detectable levels, therefore, development of
ORE data for this compound is not possible.  Also, the quantity of
bis(2-ethylhexyl)phthalate found in SARM II run 3 was below the method
detection limit.
     Non-detectable levels of anthracene and pentachlorophenol  were observed
in all modified method 5 samples with the exception of SARM II  run 1  in which
a pentachlorophenol concentration of 1.5 yg/m3 and mass  rate of 7.6 x  10"
Ib/h were observed.  Since non-detectable levels of pentachlorphenol were
observed for corresponding SARM feed for this run, this  result  is considered
an outlier and is less than 2 times the method detection limit  thus making
this value suspect.  The DRE's for anthracene are all greater than 99.99
percent based on the feed rate data and non-detectable stack gas concentra-
tion.  For the one test for which pentachlorophenol feed data are available
(SARM I, run 2), a ORE of greater than 99.99 percent was achieved based on
the non-detectable level in the corresponding stack gas  sample.  The ORE data
for bis(2-ethylhexyl)phthalate show that 3 of 5 sample runs achieved at least
a 99.99 percent ORE.  Results for bis(2-ethylhexyl)phthalate must be inter-
preted with caution, however.  Blanks which were analyzed show the presence
of this compound, with the filter blank, XAD-2 blank, and train blanks show-
ing the presence of bis(2-ethylhexylJphthalate at levels which range from a
factor of approximately 30 times the detection limit to 65  times the detec-
tion limit.  Contamination by this compound thus is observed to occur readily.

                                     2-28

-------
However, the levels of this compound in the actual  emission samples  is  an
additional factor of 50 to 70 times above the levels observed  in  the blanks.
A correction factor of 45 pg (representing the blank value obtained  from
analysis of the field train blank)  was applied to each run.
2.5.5  Metals Emission Data
     Table 2-18 summarizes the concentration and mass rate data  for  the
following metals:  arsenic, cadmium, chromium, copper, lead, nickel, and
zinc.  Concentrations are expressed in micrograms per cubic meter (yg/m3)  and
mass rates in Ib/h.  The volumetric flow rate measured by the  metals train
during each test period was used in calculating the mass emission rates.
2.5.6  Continuous Emission Monitor  Data
     Tables 2-19 through 2-24 summarize the CEM data for 0, COp, and CO
during each test burn.  These data  remained relatively consistent throughout
each sample period with short-term  (less than 5 minutes) excursions  in  CO
concentration as noted in the tables.  During the CO excursions,  the 02
content of the stack gas typically  dropped to near zero percent  for  less than
1 minute.
2.5.7  Dioxin/Furans Analytical  Data
     The determination of tetra-, penta-, hexa-, and octachlorodibenzodioxins
(PCDDs) and dibenzofurans (PCDFs) was performed on feed, ash,  and scrubber
water samples following the analytical methodology of EPA Method  8280
(SW-846, Third Edition).
     The results for the analysis of the dioxin/furan samples  are shown in
Tables 2-25 to 2-27.  No levels  of  dioxins or furans above the Method
detection limit were observed in any of the samples, while all surrogate
compound recoveries were within  the limits specified by Method 8280  (SW-846,
Third Edition).
                                     2-29

-------
TABLE 2-18.  SUMMARY OF METALS EMISSION DATA

Metal
Arsenic
Cadmium
Chromium
Copper
Lead
Nickel
Zinc
Arsenic
Cadmium
Chromium
Copper
Lead
Nickel
Zinc

Run
vg/m3
19.3
2051
80.6
217
840
362
454

Run
6.3
1353
35.2
104
415
45
185

1
Ib/h
.0001
.012
.0005
.001
.005
.002
.003

4
.00003
.007
.0002
.0005
.002
.0002
.0009
SARM
2
yg/m3
23.3
1411
69.8
274
1018
52
311
SARM
5
6.0
1347
20.3
51
374
33
129
I

Ib/h
.0001
.007
.0004
.001
.005
.0003
.002
II

.00003
.007
.0001
.0003
.002
.0002
.0007


ug/m3
11.5
2595
60.1
303
1074
38
490


9.8
1016
15.4
38.8
351
27
70

3
Ib/h
.00006
.014
.0003
.002
.006
.0002
.003

6
.00005
.005
.00008
.0002
.002
.0001
.0004

3 Test
average
Ib/h
.0001
.0110
.0004
.0014
.0053
.0009
.0023


.00004
.0066
.00012
.00034
.002
.00018
.00068
                     2-30

-------
      TABLE  2-19.
SUMMARY OF CONTINUOUS EMISSION MONITOR DATA
            SARM I
         TEST NUMBER 1
Time
Period (24h)
1030
1045
1100
1115
1130
1145
1200
1215
1230
1245
1300
1315
1330
1345





I
Net time,
(minutes)
15
15
15
15
15
15
15
15
15
15
15
15
15
15






Average concentration
o2, %
6.6
5.8
6.2
5.8
5.5
5.3
5.5
5.1
5.3
5.5
5.3
4.7
4.7**
4.7






co2%
10.1
10.5
10.1
10.9
10.7
11.6
11.0
11.0
10.7
11.0
11.2
11.2
11.0
11.0






CO, ppm
10
10
10
10
10
10
10
10
10
10
10
10
10*
45






Comments












*
Peaked off
scale for
1 min.
**
Dropped to
zero for
1 min.
1400
1415
1430
15
15
15
5.0
5.0
5.8

5.4
11.0
10.5
10.1

10.8
 2.5
10
10

11.6
                                 2-31

-------
TABLE 2-20.   SUMMARY OF CONTINUOUS EMISSION MONITOR DATA
                         SARM I
                      TEST NUMBER 2
Time
Period (24h)
1630
1645
1700



1800
1815
1830
1845
1900
1915
1930
1945
2000
2015
2030




Net time,
(minutes)
15
15
15



15
15
15
15
15
15
15
15
15
15
15




Average concentration
o2, %
6.6
6.9*
6.9



6.3
6.1
5.5
4.7
5.3
5.1
5.3
5.5
5.5
5.8**
5.5




co2%
9.3
9.5*
9.5



9.3
9.7
10.9
11.2
11.2
11.2
10.7
10.5
10.9
10.7**
10.7




CO, ppm
10
10*
10



10
10
10
10
10
10
10
10
10
10**(a
10 la




Comments

*
Stop at
1700 re-
start at
1745









\ **
' Stopped
test at
2030 water
in line
(a) Peak at
                                                        2016

                          5.8       10.4       10
                           2-32

-------
      TABLE 2-21.
SUMMARY OF CONTINUOUS EMISSION MONITOR DATA
            SARM I
         TEST NUMBER 3
Time
Period (24h)
1050
1105
1120
1135
Net time,
(minutes)
15
15
15
15
Average concentration
o2.x
7.1
6.3
4 !7**
co2%
9.1
9.9
10.5
11.2
CO, ppm
10
10
45*
Comments
Peaked off
1150
1205
1220
1235
1250
1305
1320
1335
1350
1405
1420
15
15
15
15
15
15
15
15
15
15
15
5.3
5.5
6.3
6.0
5.5
4.5
6.3
5-5**
4.2
4.5
4.2
11.4
10.9
9.8
10.1
10.3
11.8
10.3
11.1
10.9
10.9
11.2
10
10
10
10
10
10
10
10*
45
10*
45
                                           scale at
                                           1134, 1401,
                                           and 1407
                                          **
                                             Dropped
                                           to zero at
                                           1134 and
                                           1401
5.4
                                          10.6
                                  17.0
               2-33

-------
      TABLE 2-22.  SUMMARY OF CONTINUOUS EMISSION MONITOR DATA
                               SARM II
                            TEST NUMBER 4
Time
Period (24h)
1715
1730
1745
1800
1815
1830








Net time,
(minutes)
15
15
15
15
15
15








Average concentration
o2, %
6.3
5.7
5.3
4.2
3.7
3.4a








CQ2%
9.2
10.0
10.9
11.6
12.0
12.3








CO, ppm
10
10
10
10
1*
92








Comments





a Dropped
to zero at
1819 and
1828
*
spike at
1819 and
off scale
at 1828
1845
1900
1915
1930
1945
2000
2015
2030
15
15
15
15
15
15
15
15
5.0
5.5
5.8
5.3.
5.3fc
11.4
10.9
11.1
10.3
10.7
5.5
5.3
5.5C
10.9
11.4
10.9
10
10
10
10.
69
**
10
10.
45
        Dropped
        to zero at
        1931
                                                             **
***
                                                                spike at
                                                              1931 and
                                                              off scale
                                                              at 1945
        Dropped
       to zero
       ar 202B
      ***
          spike
       at 2028
       and off
       scale at
       2028
                                5.1
                       11.0
                     22.6
                                 2-34

-------
     TABLE 2-23.
SUMMARY OF CONTINUOUS EMISSION MONITOR DATA
            SARM II
         TEST NUMBER 5
Time
Period (24h)
0945
1000




1015
1030
1045
1100
1115
1130




1145
1200
1215




1230
1245
1300




Net time,
(minutes)
15
15




15
15
15
15
15
15




15
15
15




15
15
15




Average concentration
2* *
6.3a
5.4a




5.2
4.9
5.2
5.7
5'4b
5.4b




5.7
6.3,.
5.4C




5.6
5.7.
5.4d




co2%
9.9
10.4




11.0
11.5
11.3
10.6
11.5
10.2




10.6
10.6
10.4




11.0
11.0
11.1




CO, ppm
10 *
12.4




10
10
10
10
10**
26




10
10***
45




10
10****
45




Comments

a Dropped
to 22
*
Spike at
0946




K
Dropped
to 15
**
Spike
at 1129


c Dropped
to zero
***
Spike
at 1208

A
Dropped
to zero
****
Spike
at 1250
1315
 15
5.7
                                5.6
10.8

10.8
10

15.9
                                 2-35

-------
TABLE 2-24.   SUMMARY OF CONTINUOUS EMISSION MONITOR DATA
                         SARM II
                      TEST NUMBER 6
Time
Period (24h)
1415
1430
1445
1500
1515
1530
1545
1600
1615
1630
1645
1700
1715
Net time,
(minutes)
15
15
15
15
15
15
15
15
15
15
15
15
15
Average concentration
o2, %
5.4
5.4
5.7
5.2
5.2
5.2
5.4
5.6
5.7
5.4
5.4
5.3
4.9
co2%
11.1
11.3
10.6
11.5
11.5
11.5
10.8
10.8
11.1
11.3
11.0
10.8
11.0
CO, ppm Comments
10
10
10
10
10
10
10
10
10
10
10
10
10
                          5.4         11.1       10.9
                           2-36

-------
                 TABLE 2-25.   DIOXIN/FURAN RESULTS  NG/G FEED
                     Reagent blank       ZSARM 1-2-F        ZSARM-II-5-F
                     A710018-Blank       A710003-07-A       A710003-08-A
Analyte                  37031               37034              37035
Total TCDD
Total TCDF
Total PCDD
Total PCDF
Total HxCDD
Total HxCDF
Total HpCDD
Total HpCDF
Total OCDD
Total OCDF
<0.2
<0.2
<0.2
<0.2
<0.5
<0.4
<0.6
<0.4
<1.6
<0.7
<0.6
<0.5
<0.4
<0.4
<1.0
<0.9
<0.6
<0.8
<1.6
<1.6
<0.6
<0.5
<0.5
<0.4
<1.1
<0.8
<0.6
<1.1
<2.2
<1.7
NOTE:  All  Surrogate recoveries are within method prescribed limits.   Each
       value listed represents the method detection limit (MDL)  for that
       particular dioxin and sample.  All values  are less than  the MDL.
                                     2-37

-------
                 TABLE 2-26.  DIOXIN/FURAN RESULTS NG/G ASH
                     Reagent blank       ZSARM 1-2-A        ZSARM-II-5-A
                     A710003-Blank       A710003-04-A       A710003-05-A
Analyte                  37022              37020               37021
Total TCDD
Total TCDF
Total PCDD
Total PCDF
Total HxCDD
Total HxCDF
Total HpCDD
Total HpCDF
Total OCDD
Total OCDF
<0.2
<0. 1
<0.2
<0.2
<0.4
<0.3
<0.5
<0.3
<0.6
<0.5
<0.2
<0.1
<0.2
<0.1
<0.3
<0.2
<0.4
<0.3
<0.5
<0.4
<0.2
<0. 1
<0.2
<0. 1
<0.3
<0.2
<0.4
<0.3
<0.6
<0.5
NOTE:  All  Surrogate recoveries are within method prescribed limits.   Each
       value listed represents the method detection limit (MDL)  for that
       particular dioxin and sample.  All values are less than the MDL.
                                     2-38

-------
                 TABLE 2-27.   DIOXIN/FURAN SCRUBBER RESULTS
                                 (rig/liter)


Analyte
Total TCDD
Total TCDF
Total PCDD
Total PCDF
Total HxCLD
Total HxCDF
Total HpCDD
Total HpCDF
13C-OCDD
13C-OCDF
Reagent blank
A710003-Blank
37017
<2
<1
<2
<1
<3
<2
<4
<2
<5
<4
ZSARM 1-2-S
A710003-01A
37018
<2
<1
<2
<1
<3
<2
<4
<2
<4
<4
ZSARM-II-5-S
A710003-02-A
37019
<1
<1
<1
<1
<3
<2
<4
<2
<4
<4
NOTE:  All Surrogate recoveries are within method prescribed limits.  Each
       value listed represents the method detection limit (MDL) for that
       particular dioxin and sample.  All values are less than the MDL.
                                     2-39

-------
                                  SECTION 3
              DESCRIPTION OF INCINERATOR AND PROCESS OPERATION

3.1  INCINERATOR DESCRIPTION
     The John Zink Co.  incineration test facility,  which was  used for this
test series, is located in Tulsa,  Oklahoma.   The test facility  is composed  of
several modular components which can be assembled in a variety  of configu-
rations.  Although the  test facility is outdoors, it operates during wet or
dry weather.  Minimum system input is 2 x 106 Btu/h, maximum  is 3 x 10
Btu/h.
     The rotary kiln system configuration which was used for  this test is
shown in Figure 3-1.  It consisted of a rotary kiln fitted with an auxiliary
natural gas fuel burner, screw conveyor for feeding solids, and a continuous
ash removal system; the kiln was followed by a secondary combustion chamber
fitted with a natural gas burner,  a cyclone separator for large solids, a
quench section, an adjustable venturi scrubber, and an induced-draft blower.
For this test, the rotary kiln was positioned for co-current  operation, i.e.,
solids/ash travel in the same direction as the gas.  In addition to this
equipment, a tertiary afterburner, required by the Oklahoma State Department
of Health for final thermal treatment of the combustion system's flue gas,
followed the air pollution control equipment.  All  source testing, process
monitoring, and sampling for the BOAT program were conducted  upstream of this
tertiary unit.
     The sample ports used for stack testing purposes were located in the
flue between the venturi scrubber and the afterburner (Sample Ports B of
Figure  3-1).  The ports were 4 inches in diameter, located on a vertical,
12-inch I.D. flue about 15 feet above ground; John Zink Co. supplied scaf-
folding for the equipment used to conduct stack tests at this location.  A
                                     3-1

-------
    SOLID
    WASTE
CO
I
tV)
   SCREW FEEDER  FUEL (NAT. GAS)

                        COMBUSTION AIR
<
                                                        SAMPLE PORT C
               FEED HOOD
                                                         INCINERATOR/AFTERBURNER
                                                                        SAMPLE
                                                                         PORTB
                                                                             h
                            NOTES:
                              KILN SHOWN IN COCURRENT
                              CONFIGURATION
                ROTARY
                 KILN
                                                                                 I.D. BLOWER
                                  KILN
                                 AFTER-
                                 BURNER
 .t

DISCHARGE HOOD
                VENTURI SCRUBBER WATER
                   TO STORAGE TANK
                                                           ADJUSTABLE
                                                             VENTURI
                      SAMPLE PORT A
                                                                             JOHN ZINK COMPANY
                                                    QUENCH SECTION
                     WET SOLIDS
                       TANK
                                           LARGE SOLIDS
                                            SEPARATOR
                          Figure 3-1.  Rotary kiln incinerator configuration for solids.

-------
conference roon, indoor storage/work area,  lab space,  ice  machines,  and
electricity located at the test site were available throughout the test.   The
55-gallon drums of SARM were staged for feeding from the hazardous waste
storage pad located adjacent to the test equipment.  Drums were transported
to the feed screw conveyor using a hydraulic drum lifter;  once the drums  had
been emptied of feed material  they were used to contain the ash which was
ultimately sent for disposal to U.S. Pollution Control, Inc.'s Lone Mountain
RCRA landfill in Oklahoma.
     John Zink provided standard system performance monitoring consisting of
continuous monitoring of temperature, gas flow, and (L through the kiln  and
secondary chamber, plus continuous monitoring of CO, C02,  and NOX in stack
gases exiting the afterburner.  PEI collected process samples of feed, ash,
and scrubber wastes throughout the testing for subsequent analysis, as well
as stack gas emission samples for volatiles (VOST), semivolatiles (MM5),
metals (EPA Method 12), HC1 (EPA Method 5), particulate (EPA Method 5),  CO,
C02, and 02 throughout each test burn.
                                     3-3

-------
                                  SECTION 4
                   SAMPLE LOCATIONS AND TEST METHODS USED

4.1  SAMPLING LOCATIONS AND EQUIPMENT OPERATION SPECIFICATIONS
     Figures 4-1 and 4-2 show the rotary kiln system configuration and asso-
ciated sampling and monitoring points for the SARM test burns.  Three test
runs were performed on each SARM.

4.2  PROCESS SAMPLING PROCEDURES (WASTE FEED, ASH, AND SCRUBBER WATER)
     Table 4-1 presents the sampling plan and methodology followed for col-
lecting the feed, ash, and scrubber water samples.  Basic sample collection
procedures followed were those described in Sampling and Analysis Methods for
Hazardous Waste Combustion, Arthur D. Little, Inc.  EPA-600/8-84-002, Febru-
ary 1984.  This reference was added as a revision to the 2nd Edition of
SW-846.
4.2.1  Waste Feed Sampling
     Feed samples were collected from the screw feed hopper at the beginning,
middle, and end of each run and composited into a 5-gallon metal container
which was covered between sampling events.  Samples were collected using
metal scoops which were wiped clean between samples.  Grab samples for vola-
tiles were collected at the same time and placed in appropriate containers
immediately.  The composite was mixed using the scoop, and aliquots were
placed in appropriate sample containers (see Table 4-1) for analysis.  Samples
were labeled and placed in coolers with vermiculite and ice for shipment to
the laboratory for analysis.
4.2.2  Bottom Ash Samples
     One composite sample of bottom ash was collected during each SARM test
run.  The ash was sampled at the beginning, middle, and end of each run
directly from the rotary kiln (prior to the quench), placed in a 5-gallon

                                     4-1

-------
                                                                                                     TO
                                                                                                 ATMOSPHERE
                                                                           SCRUBBER
                                                                            INFLUENT
                                                                          (MAKEUP AND
                                                                        RECYCLED WATER)
                                                        INCINERATOR
                                                       AFTERBURNER
                                        NATURAL
                                          GAS
                             SCREW FEEDER
                                                        KILN
                                                    AFTERBURNER
ROTARY
 KILN
i
ro
            DRUMS
                                                      BOTTOM
                                                       ASH
                                                                      SOLIDS
                                                                    SEPARATOR
  EFFLUENT
  RECYCLED
TO SCRUBBER
SAMPLE
ID
A
B
C
D
SITE
DESCRIPTION
Drums
Ash Bin
Sample Ports
Water Separator
SAMPLE
DESCRIPTION
Waste Feed
Bottom Ash
Stack Gas
Scrubber Effluent
                                  Figure 4-1. The John Zink Company rotary kiln incineration system and teed
                                               and residuals sampling sites for SARM I and II.

-------
WASTE 	 1
FEED
r>
KILN


^-


AFTERBURNER

fc.


CYCLONC
SOLIDS
SEPARATOR


fe

VENTURI
SCRUBBER

fe

CYCLONC
WATER
SEPARATOR


^snr\
*l FAN J 1 *
INCINERATOR/
AFTERBURNER

.... ^





SAMPLING
POINT
1
2
3
4
5
6
7
8"
PARAMETER


WASTE
FEEDRATE
X









WASTE
FEED
X









pua
FEEDRATE
X

X







AIR
FEEDRATE
X

X








ASH

X


X





SCRUBBER
WATER





X


CONTINUOUS
MONITORS
C02.
O2.CO.T






X
X


VOLUME
aow






X

VOST.MMS
(VOLATXES.
SEMIVOLATILES
AND METALS)






X

MS
(PARTCU-
LATE
AND HO)






X




T


X
X


X
X



p






X

T: Temperature
P: Pressure
a: MonHoring by John 3nk tor slate peimH requirement.
                  Figure 4-2.  Operating parameters monitored by John Zink/PEI during SARM test bums.

-------
                         TABLE 4-1.  PROCESS SAMPLING LOCATIONS,  EQUIPMENT,  AND METHODS
Sampling stream
identification
Solid feed

Access
Hopper
(screw feed)
Analytical
parameter
Semivolatiles
Volatiles
Sampling
container
8-oz glass
bottles
General
procedure/frequency
Subsamples collected at
beginning, middle, and
Reference
methods
S007
P003
Sampling
responsibility
PEI
-p*
I
    Ash
Hopper
    Scrubber
    water
Tap
                                       Metals

                                       TCLP
Semivolatiles
Volatiles
                                       Metals

                                       TCLP
Semivolatiles
Volatiles
                                       Metals
40-ml VOA
 vial
 (Teflon
 septum lid)
4-oz plastic
 jar
i-gal glass
 bottles

8-oz glass
 bottles
40-ml VOA
 vial
4-oz plastic
 jar
i-gal glass
 bottles
1-gal glass
 bottle
40-ml VOA
 vial
1-liter
 plastic
 bottle
                                                end  of each  4-h  test
                                                period; composited  into
                                                one  sample with  aliquots
                                                taken  for each analyti-
                                                cal  parameter  (volatile
                                                samples were not com-
                                                posited)
Subsamples collected at
beginning, middle, and
end of each 4-h test
period; composited into
one sample with aliquots
taken for each analyti-
cal parameter (volatile
samples were not com-
posited)

Subsamples collected at
beginning, middle, and
end of each 4-h test
period; composited into
one sample with aliquots
taken for each analyti-
cal parameter (volatile
samples were not com-
posited)
 S007
 P003
PEI
S004
P001
PEI

-------
metal container, mixed, and allowed to cool briefly before it was placed in
the final sample containers for shipment to the laboratory.
4.2.3  Scrubber Water Samples
     Prior to the start of testing, one sample of influent scrubber water was
taken for analysis to determine background levels.  Following one composite
scrubber sample was collected for semivolatiles and metals and three discrete
samples were collected for volatiles during each test run.  Aliquots were
collected at the beginning, middle, and end of each run from a tap in the
scrubber recycle system.  The aliquots taken for semivolatiles and metals
were composited in a 1-gallon glass container which was covered between
sampling events; aliquots of the composite were subsequently placed in appro-
priate containers for analysis, as outlined in Table 4-1.  Samples taken for
volatiles were placed in 40-ml VOA vials with septum lids, with care taken to
eliminate all headspace in the vials.  Samples were then labeled and placed
in coolers packed with vermiculite and ice for shipment for analysis.

4.3  STACK GAS SAMPLING PROCEDURES
     This section discusses the specific sampling procedures used for the
stack gas monitoring portion of this test  program.
4.3.1  Sample Location
     All emission sampling was conducted after the venturi scrubber control
system immediately after the  ID blower and prior  to the tertiary fume incine-
rator, as shown in Figure 4-1.  Figure 4-3 depicts in more detail the actual
sample location and ports used to extract  air emission samples.  Two sample
ports, 90 degrees off-center, were  located more than 8 duct diameters down-
stream and upstream from the  nearest flow  disturbance in  the  12-inch I.D.
round duct.   Eight sample points, four per port,  were used to  traverse  the
cross-sectional area of the  duct for the particulate/HCL/semivolatile and
metals sample  runs.  Two additional sample ports  located  a few feet down-
stream from  the particulate  ports  (See Figure 4-3) were  used  for  the VOST  and
CEM  sample probes.
                                      4-5

-------
                                                           CROSS SECTION
                       TRAVERSE
                       POINT NO.
                           1
                           2
                           3
                           4
                              DISTANCE FROM
                                OUTSIDE OF
                                NIPPLE, in.
                                   81/2
                                  10 1/2
                                  16 1/2
                                  18 1/4
                                                               12 in. i.d.
                                                         7 1/2 in. NIPPLE LENGTH
                    FLOW
      CEM
     PROBE
    LOCATION N
TO
                       VOST
                      SAMPLE
                      LOCATION
               =/
-96 in.
AFTERBURNER
                    PARTICULATE
                    SEMI-VOLATILE
                      SAMPLE
                      LOCATION
                             -104 in.
                                     FLOW
                                                          FLOW
                                    VENTURI
                                     WATER
                                    STORAGE
                                     TANK
                                                                                      GAS FLOW
                                                                                     FROM VENTURI
                                                                                     GROUND
                              Figure 4-3.  Stack gas sample location.
                                                4-6

-------
4.3.2  Sample Procedures
     Both high- and low-level  contaminated soils were incinerated during this
test program.  The same basic  emission sampling and analytical  methodology
was applied for both waste types as outline in Table 4-2.
     A modified Method 5 (MM5) sampling train (EPA-600/8-84-002,  Method S008)
was used to measure senrivolatile POHCs [anthracene, pentachlorophenol,  bis(2-
ethylhexyl)phthalate], particulate, and HC1 emissions.  Triplicate, inte-
grated 3-hour sample runs were conducted by traversing the cross-sectional
area of the stack.  Samples were collected isokinetically according to  the
procedures of EPA Method 5 (40 CFR 60, Appendix A).  Gas stream flow rate,
temperature, and moisture content were measured in conjunction with the MM5
sampling.
     The MM5 sampling train consisted of a stainless steel nozzle, a heated
glass-line probe, a heated glass-fiber particulate filter, a water-cooled
condenser, an XAD-2 sorbent trap, and a series of impingers.  The filter and
a methylene chloride rinse of the nozzle, probe, and connecting glassware
were recovered and analyzed for particulate content according to EPA Method 5
procedures.  The XAD-2 sorbent trap and a methylene chloride rinse of the
connecting glassware between the filter and the sorbent trap was recovered
and analyzed for the designated POHCs.  The recovered filter and the residue
from the probe rinse were analyzed for POHCs after completion of the particu-
late analysis.
     Initially, the first impinger in the train was empty, and condensate
collected was recovered for POHC analysis by rinsing the impinger with meth-
ylene chloride.  The second and third impingers each contained 100 ml of 0.1
NaOH solution; both were recovered and analyzed for HC1 content.  The fourth
impinger contained approximately 400 g of silica gel for moisture removal.
     Volatile organic emissions (ethylbenzene, xylene, 1,2-dichloroethane,
tetrachloroethylene, acetone, chlorobenzene, and styrene) were measured
according to the Volatile Organic Sampling Train (VOST) protocol (EPA-600/8-
84-007) with improvements that were developed through a recent field valida-
tion study.*  The sampling train consisted of a heated glass probe, a pair of
  Validation of the Volatile Organic Sampling Train (VOST) Protocol, Field
  Validation Phase.  EPA 600/S4-80-014, April 1986.
                                     4-7

-------
                                   TABLE  4-2.   EMISSION  SAMPLE  LOCATION,  EQUIPMENT,  AND METHODS
I
00
Sampling stream
identification Access
Stack gas (after Ports
scrubber and
prior to fume
incinerator)









Analytical
parameter
Semivolatiles


Particulate
HC1
Volatiles


Metals

Carbon monox-
ide (CO)
Oxygen (O,)/
Sampling
equipment
Modified Method 5
train



VOST


EPA 12 sample
train
NDIR-continuous
monitor
Continuous enris-
General procedure/frequency
Triplicate
sample run



Triplicate
sample pai
per pair
Triplicate
sample run
Continuous

Continuous
integrated 3-h




single-point
rs - 40 minutes

integrated 2-h

for each test run

for each test run
Reference
methods
S008
EPA 5



S012 VOST
protocol

EPA 12

EPA 10

EPA 3A
                                       carbon  dioxide
                                       (C02)
sion monitors

-------
water-cooled condensers, and a pair of sorbent traps in series.   The first
sorbent trap contained approximately 1.6 g of Tenax GC; the second contained
approximately 1 g of Tenax GC and 1 g of activated charcoal.   Each sample was
collected at a constant rate of 0.5 liter per minute over a 40-minute period.
Three 40-minute samples were collected during each 3-hour test run.   Conden-
sate collected in the sampling train was recovered after each 3-hour test run
and analyzed for volatile POHC content.
     Metals were collected using an EPA Method 12 sample train.   This train
consisted of a heated glass-line probe, a heated filter, and a series of
impingers containing 0.1 N HMO- (nitric acid).  Samples were collected iso-
kinetically by traversing the cross-section area of the stack.  Probe rinse,
filter, and impinger solution fractions were combined and digested into a
single sample and analyzed for the following metals:  lead, zinc, cadmium,
arsenic, copper, nickel, and chromium.  This sample train was run concurrent
with the MM5 sample train with a total test time of 2 hours for each run.
     Carbon monoxide (CO), carbon dioxide (COg). and oxygen (02) concentra-
tions measured continuously throughout the test periods by continuous emis-
sion monitors (CEM's).  A sample tap downstream from the MM5 sample location
was used to locate the CEM sample probe.  The sampling was performed accord-
ing to EPA Method 10 for CO, and EPA Method 3A for C02 and Og.
     Appendix D contains more detailed descriptions of the sampling and
analytical procedures used for collecting the stack gas samples.
                                     4-9

-------
                                  SECTION 5

                  QUALITY ASSURANCE PROCEDURES AND RESULTS


     The procedures described in the Quality Assurance Project Plan were
followed for all field sampling and analyses.  The following sections de-

scribe the quality assurance procedures and the results obtained.


5.1  FIELD SAMPLING QUALITY ASSURANCE

     Routine reference method quality control procedures were followed through-
out the test program  These included, but were not limited to, the following:

     0    Calibration of field sampling equipment.  Sampling equipment was
          calibrated according to the procedures of the "Quality Assurance
          Handbook for Air Pollution Measurement Systems, Volume III," EPA
          600/4-72-027B, August 1977.  The calibration data are summarized in
          Table 5-1.  Calibration guidelines are described in more detail in
          Appendix E.

     0    Onsite audits of dry gas meters, thermocouples, and digital indi-
          cators (See Appendix B).

     0    Train configuration and calculation checks.

     0    Onsite quality control  checks of the sampling train and leak checks
          of the pi tot tube and Orsat line.

     0    Use of designated equipment and reagents.

     The sampling equipment and procedures met all the guidelines established
in the reference methods to achieve accurate test results.


5.2  CONTINUOUS EMISSION MONITORS

     The following quality assurance procedures pertain to the use of the

carbon dioxide, oxygen, and carbon monoxide continuous emission monitors:

     0    Use of designated sampling equipment and procedures.  The CEM's met
          all performance requirements of EPA Methods  3A and 10.  All com-
          ponents in the sampling system were either 316 stainless steel
          (probes) or Teflon (sampling line and pump diaphragms).


                                     5-1

-------
                      TABLE 5-1.  FIELD EQUIPMENT CALIBRATION DATA
Equipment
Meter box










Pi tot tube



Digital
indicator


Stack
thermo-
couple
VOST Meter
console
Impinger
thermo-
couple
Balance
Barometer
Dry gas
thermo-



ID
No.
FT-3





FB-3




504
376


FT-3



409
103

VB-4

1-13
1-14

Mettler
No. 408
FT-3
FB-3


VB-4
Calibrated
against
Wet test meter



Critical orifice






Geometric speci-
ficatons


Millivolt signals



ASTM-3F


Bubble Meter

ASTM-3F


Type S weights
NBS-traceable
ASTM-3F



ASTM-3F
Allowable
error
Y 0.02Y
AH @ 0.15
(Y  0.05Y
post-test)
Y 0.05Y
AH @ 0.15





a



0.5%



2F


Y  0.05Y
post-test
2F


0.5g
0.10 in.Hg
5F



5F
Within
Actual allowable
error limits Comments
0.007
0.13
0.008

0.008
-0.04
0.001
0.0
0.027
0.014
0.03




0.0-0.18%



+1F
+1F


-0.034
0.0F
0.0F

0.0 g
0.01 in.Hg
+1F
+0F
+1F
+2F
+3F
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




Checked on si1
prior to test'



Checked on si'
prior to test
Visually inspi
ted on site


Check on sit'
prior to te
calibration
ranges










Inlet
Outlet
Inlet
Outlet
Inlet
See Appendix E.
                                         5-2

-------
      0     System  leak  checks and integrity checks.  Prior to the start of the
           first test,  the entire sampling system from the probe to the ana-
           lyzer inlet  was leak-checked by plugging the probe inlet and evacu-
           ating the system to 15 in. Hg.  The vacuum was observed for 5
           minutes to ensure that the system was leak-free.
           System  integrity and bias were measured by injecting calibration
           gases through a three-way valve at the probe outlet and comparing
           the response obtained to the response obtained when the gas was
           introduced directly to the analyzer.  System integrity test results
           are listed on the data sheets in Appendix B.  System bias was in
           all cases less than 2 percent of scale.
      0     Pre- and post-test calibrations.  At the beginning and end of each
           test, each analyzer was calibrated with three standards in the
           analytical range and zero nitrogen.  The calibration data were
           reduced by linear regression analysis and the linear equations were
           used for data reduction.  Calibration data are summarized in Tables
           5-2, 5-3, and 5-4.
      Pre-test calibration data was used to calculate gaseous concentrations
from  all test blocks.   In most cases, post-test calibrations drifted by less
than  2 percent from pre-test values.

5.3   LABORATORY QUALITY ASSURANCE

     The laboratory quality assurance procedures outlined in the Quality
Assurance  Plan were followed for each type of analysis.  Quality assurance
measures included replicate analyses, analyses of spiked samples, reagent and
field sampling train blanks, and reference standards (where applicable).  All
analyses for the process and stack gas samples were conducted by Radian
Corporation following  procedures describe in the appropriate analytical
methods as described in the QAPP for this project.   The following sections
describe the results of these measures by analysis type.  The laboratory
report for this project is contained in Appendix C.
5.3.1  Volatile Organics
     Process samples analyzed for volatile organics included waste feed,
scrubber water, and ash.  Quality assurance included matrix spikes and matrix
spike duplicates for each , as required by Method 8240.  The laboratory re-
ports in Appendix C indicate that data were acceptable based on EPA contract
limits and the specifications of Method 8240.  One value reported as ND (non-
detectable) for tetrachloroethylene in the SARM I waste feed of Run 1 was

                                     5-3

-------
TABLE 5-2.   CO ANALYZER CALIBRATION DATA

Test No.
SAI-CO-1
SAI-CO-2

T SAI-CO-3
-p.
SAII-CO-1

SAII-CO-2
SAII-CO-3

Standard
concen-
tration,
pmm
0
22
250
453.1
0
22
250
453.1
0
22
250
453.1
Analyzer
% of
Pretest
0.3
5.0
54.0
95.9
0
4.8
55.0
97.8
0
4.9
55.8
98.3
response,
scale
Post-test
0.2
4.8
54.0
94.5
0
4.5
54.2
97.0
0
4.2
54.2
96.3
Drift,
% of span
-0.1
-0.2
0.0
-1.4
0
-0.3
-0.8
-0.8
0
-0.7
-1.6
-2.0
Linear regression Correlation
equation coefficient
CO oom - CD--4748 -9999




 	 CD - .1852 0.9999
,t.luJ


Conner - CD - -1852 -9999
uoppcr - 5T7fi


-------
                                       TABLE 5-3.  C02 ANALYZER  CALIBRATION DATA
01
01



Test No.
SAI-CO,-!
c.
SAI-C09-2
2
SAI-CO--3

SAII-CO,-!
2
SAII-C09-2

SAII-C00-3
2
Standard
concen-
tration,
%
0
+ .01
7.98
16.09
0
4.01
7.98
16.09
0
4.01
7.98
16.09
Analyzer
% of

Pretest
4.0
26.0
44.5
89.0
3.2
26.5
45.8
92.0
4.2
27.5
47.0
94.0
response,
scale

Post- test
4.0
26.0
45.0
92.5
5.0
28.2
48.0
95.0
4.3
27.5
46.5
92.0


Drift,
% of span
0.0
0.0
+0.5
+3.5
+1.8
+1.7
+2.2
+3.0
+0.1
0.0
-0.5
-2.0


Linear regression
equation
rn  CD - 3.9906
CUi!% 5.254


CQ  _ CD - 3.375
^^ 5.4843


rn * CD - 4.2157
LU^ 5.5498




Correlation
coefficient
0.9996



0.9996



0.9996




-------
                                           TABLE  5-4.   02 ANALYZER CALIBRATION DATA
en
i
cr>



Test No.
SAI-0,-1

SAI-0,-2
2
SAI-09-3

SAII-09-1
.
SAII-0,,-2

SAII-00-3
L
Standard
concen-
tration,
%
0
4.09
8.08
15.09
0
4.09
8.08
15.09
0
4.08
8.08
15.09
Analyzer
% of

Pretest
11.5
28.6
43.3
67.6
11.2
28.3
43.5
68.2
11
28.2
42.8
66.0
response,
scale

Post-test
11.0
27.3
41.0
63.3
11.2
26.8
40.4
64.0
11
28.2
42.8
67.8


Drift,
% of span
-0.5
-1.3
-2.3
-4.3
0.0
-1.5
-3.1
-4.2
0.0
0.0
0.0
+1.8


Linear regression
equation
n  CD - 12.575
u** 3.694


n  CD - 12.181
U2* 3.7592


n  CD - 12.3408
"^ 3.6184




Correlation
coefficient
0.9590



0.9992



0.9980




-------
 rejected as a  reporting errorthe value is apparently confused with that
 reported for trichloroethylene.  Tables 5-5 through 5-8 summarize the vola-
 tile  surrogate recoveries and matrix spike data (including duplicates) for
 the process samples.
      For stack samples analyzed by the VOST procedure, quality assurance
 included field, laboratory, and trip blank analyses, surrogate spikes, and
 daily and weekly instrument calibration per the VOST protocol.  Table 5-9
 summarizes the surrogate recovery data and Tables 5-10 and 5-11 summarize the
 system blank and other pertinent field and laboratory blank check data.  The
 method blanks show surrogate recoveries ranging from 45 percent for bromo-
 fluorobenzene to 108 percent for d8-toluene.  Field blanks show a range of 81
 percent for d8-toluene to 206 percent for bromofluorobenzene.  Most of these
 recoveries are within the acceptable ranges stated in Method 8240.  Actual
 sample surrogate recoveries showed exaggerated ranges in some cases.  The
 presence of large quantities of water on the sampling tubes may therefore be
 inferred, indicating a matrix effect on these samples.  The field blank data
 show non-detectable levels of volatile analytes.
 5.3.2  Semi-Volatile Organics
     Analyses for semi-volatiles organics were conducted by Method 8270.
 Process sample quality assurance included surrogate and matrix spike re-
 coveries and replicate analyses on specific samples.  Tables 5-12 through
 5-17 summarize these data.  For stack samples analyzed by Method 8270, qua-
 lity assurance included blank train and reagent blank analysis as well as
 surrogate spike recoveries for each sample.  Tables 5-16 and 5-17 summarize
 these data.   Note that a blank train value of 45 pg of bis(2-ethyhexyl)
 phthalate was recorded (Table 5-17), thus each emission sample was corrected
 for this value.
 5.3.3  Metals
     Quality assurance for metals included matrix spike recoveries and dupli-
 cates for the process and stack samples as well as Method 12 blank data.
 Tables 5-18 through 5-22 summarize these data.
 5.3.4  Particulate and HC1
     One filter and one sample of methylene chloride probe rinse were submit-
ted for particulate analysis as blanks.  The filter blank yielded a total
particulate  value of 0.1 mg.  The blank level for the methylene chloride was

                                     5-7

-------
              TABLE 5-5.  VOLATILE ORGANIC SURROGATE RECOVERIES
                             FOR PROCESS SAMPLES


Feed Extract
Surrogates


SARM I
1 2 3


SARM II
1 2 3
SARM I
1
matrix
spike
SARM II
1
matrix
spike duplicate

-------
         TABLE 5-6.  VOLATILES SPIKE RECOVERY (ACCURACY) AND RELATIVE PERCENT
                        DIFFERENCE (PRECISION) FOR FEED EXTRACT
                   Determined Concentration (ug/kg)
Matrix Spike =
100 (yg/kg)
 ZSARM-
 I-l-F
0906102B
 ZSARM-
I-l-F MS
0906102C
 ZSARM-
I-l-F MSD
 0906102D
                     Relative
           Spike     percent
 Spike    recovery    diffe-
recovery  duplicate   rence
Acetone               220
1,2-Dichloroethane     30
Tetrachloroethane      36
Chlorobenzene          22
Ethlybenzene          240
Styrene                50
Total xylenes         380
              330
              160
              140
              130
              390
              160
              540
              340
              170
              140
              140
              400
              170
              550
              110
              130
              104
              108
              150
              110
              160
            120
            140
            104
            118
            160
            120
            170
9
7
0
9
6
9
6
ND = Not detected.
                                          5-9

-------
   TABLE 5-7.   VOLATILES SPIKE RECOVERY  (ACCURACY) AND  RELATIVE PERCENT
                  DIFFERENCE (PRECISION) FOR BOTTOM ASH
Matrix Spike 
100 (vg/kg)
Acetone
1,2-Dichloroethane
Tetrachloroethane
Chlorobenzene
Ethlybenzene
TABLE 5-8.
Matrix Spike =
100 (ug/kg)
Acetone
1,2-Dichloroethane
Tetrachloroethane
Chlorobenzene
i
Ethlybenzene
Styrene
Total xylenes
Determined Concentration
ZSARM-I-l-A ZSARM-I-l-A
0906104B 0906104C
440
NO
ND
ND
ND
1600
160
110
110
140
(vg/kg)
MS ZSARM-I-l-A MSD
0906104D
1100
130
120
no
140
Spike
recovery
1160
160
110
110
140
VOLATILES SPIKE RECOVERY (ACCURACY) AND
DIFFERENCE (PRECISION FOR SCRUBBER WATER
Determined
ZSARM-I-l-F
0906103B
ND
ND
ND
ND
ND
ND
ND
Concentration
ZSARM-I-l-F
0906103CR
50
110
85
92
85
85
49
(vg/kg)
MS ZSARM-I-l-F MSD
0906103D
54
120
96
100
98
96
56
Spike
recovery
50
110
85
92
85
85
49
Spike
recovery
duplicate
660
130
120
110
140
RELATIVE
Spike
recovery
duplicate
54
120
96
100
98
96
56
Relative
percent
diffe-
rence
55
?1
9
0
0
PERCENT
Relative
percent
diffe-
rence
8
9
12
8
14
14
13
ND = Not detected.
                                   5-10

-------
                TABLE 5-9.  VOST SURROGATE PERCENT RECOVERIES
Sample I.D.
SAI-V-1-A
OWA870271
SAI-V-1-B
OWA870272
SAI-V-I-C
OWA870273
SAI-V-II-A
OWA870274
SAI-V-II-B
OWA870275
SAI-V-III-A
OWA870299
SAI-V-III-B
OWA870300
SAI-V-III-C
OWA870301
SAII-V-I-A
OWA870302
SAII-V-I-B
OWA870303
SAII-V-I-C
OWA870304
SAII-V-II-A
OWA870316
SAII-V-II-B
OWA870317
SAII-V-II-C
OWA879318
SAII-V-III-A
OWA870319
p-Bromofluro-
benzene
585
258
212
223
219
257
281
279
199
220
203
245
267
197
264
d4-l,2-Dichloro-
ethane
158
112
104
93
94
101
101
141
91
108
103
84
79
85
94
d8-Toluene
393
155
139
139
131
141
134
103
117
110
109
171
155
157
148
(continued)





                                     5-11

-------
TABLE 5-9 (continued)
Sample I.D.
SAII-V-III-B
OWA870320
SAII-V-II-C
OWA870321
SAI-V-I
CONDENSATE
OWA870276
SAI-V-II
CONDENSATE
OWA870277
SAI-V-III
CONDENSATE
OWA870305
SAII-V-1
CONDENSATE
OWA870322
SAII-V-2
CONDENSATE
OWA870323
SAII-V-III
OWA870324
SAI-V-I-2
FIELD BLANK
OWA870325
SAII-V-1
FIELD BLANK
OWA870326
SAII-V-3
FIELD BLANK
OWA870327
METHOD BLANK 1
OWA870270
METHOD BLANK 2
OWA870298
p-Bromofluro-
benzene
203
260
220
207
211
279
292
299
206
119
101
45
87
d4-l,2-Dichloro-
ethane
88
89
92
88
102
96
97
98
95
101
94
105
108
d8-Toluene
148
158
127
124
94
158
166
169
154
81
95
69
78
                                      5-12

-------
            TABLE 5-10.  SYSTEM BLANK DATA FOR VOST ANALYSES (NG)


Analytes
Acetone
1,2-Dichlorethane
Perch! oroethy 1 ene
Chlorobenzene
Ethyl benzene
Styrene
Total Xylenes
Estimated
Limits of
Detection
5.0
1.0
1.1
0.7
1.8
1.6
3.8
28A
Method
Blank # 1
ND
ND
ND
ND
ND
ND
ND
29A
Method
Blank # 2
ND
ND
ND
ND
ND
ND
ND
ND = Not detected.
            TABLE 5-11.  SYSTEM BLANK DATA FOR VOST ANALYSES (NG)
Compound
Acetone
1,2-Dichlorethane
Perchl oroethy 1 ene
Chlorobenzene
Ethyl benzene
Styrene
Total Xylenes
Method
Detection
Limit
5.0
1.0
1.0
0.7
2.0
2.0
4.0
25
SAI-V-1-2
Field Blank
ND
ND
1
ND
ND
ND
a
26
SAII-V-1
Field Blank
ND
ND
1
ND
ND
ND
ND
27
SAII-V-3
Field Blank
ND
ND
ND
ND
ND
ND
ND
a = Tube broken
ND = Not detected at specified Method Detection Limit.
                                     5-13

-------
TABLE 5-12.  SEMIVOLATILES SURROGATE PERCENT RECOVERIES
Sample I.D.
Scrubber Water
ZSARM-I-l-S
F872139
ZSARM-I-2-S
F872142
ZSARM-I-3-S
F872143
ZSARM-II-4-S
F872144
ZSARM-II-5-S
F872145
ZSARM-11-6-S
FB872146
ZSARM-I-l-S
(MATRIX SPIKE)
F872147
ZSARM-I-l-S
(MATRIX SPIKE
DUPLICATE)
F872148
METHOD BLANK
F872138
ZSARM-I-l-INF
F872149
Bottom Ash
ZSARM-I-l-A
F872151
ZSARM-I-2-A
F872154
ZSARM-I-3-A
F872155
(continued)

2-Fluoro-
phenol

75
86
86
82
64
48
74
85
48
77

24
9
25

d5-
Phenol

84
101
96
96
78
61
93
91
73
88

46
39
55

d5-Nitro-
benzene

72
69
94
67
91
92
77
69
79
103

84
65
79
5-14
2-Fluro-
biphenyl

98
90
95
89
87
87
91
91
87
88

80
77
84

2,4,6-Tri-
bromophenol

114
64
97
105
87
77
48
55
69
87

12
13
30

d!4-
Terphenyl

101
94
109
92
95
90
95
91
102
88

91
89
93


-------
TABLE 5-12 (continued)
Sample I.D.
Bottom Ash Cont
ZSARM-II-4-A
F872156
ZSARM-II-5-A
F872157
ZSARM-II-6-A
F872158
ZSARM-I-l-A
(MATRIX SPIKE)
F872159
ZSARM-I-l-A
(MATRIX SPIKE
DUPLICATE)
F872160
METHOD BLANK
FB872150
Feed Extract
ZSARM-I-l-F
F872167
ZSARM-I-2-F
F872168
ZSARM-I-3-F
F872169
ZSARM-II-4-F
F872164
ZSARM-II-5-F
F872165
ZSARM-II-6-F
F872166
ZSARM-I-l-F
(MATRIX SPIKE)
FB872170
(continued)

2-Fluoro-
phenol

2
4
15
5
7
79

91
88
89
80
85
89
78

d5-
Phenol

10
13
40
38
25
90

96
91
94
92
91
87
78

d5-Nitro-
benzene

82
64
79
69
74
88

93
90
93
94
90
92
73
5-15
2-Fluro-
biphenyl

86
75
79
73
73
86

115
110
118
105
112
109
107

2,4,6-Tri-
bromophenol

ND
ND
ND
ND
ND
84

24
119
122
102
112
121
137

d!4-
Terphenyl

99
94
91
82
85
93

107
103
107
98
101
109
106


-------
TABLE 5-12 (continued)
                    2-Fluoro-   d5-     d5-Nitro-   2-Fluro-   2,4,6-Tri-   d!4-
Sample I.D.         phenol      Phenol  benzene     biphenyl   bromophenol  Terphenyl

     Feed Extract cont.

ZSARM-I-l-F
(MATRIX SPIKE
DUPLICATE)
F872171               84          85       84         109          142         101

METHOD BLANK
F872163               83          90       92         112          114          97
                                         5-16

-------
     TABLE  5-13.  SEMIVOLATILES MATRIX SPIKE  RECOVERY  (ACCURACY) AND
                  RELATIVE DIFFERENCE (.PRECISION) FOR FEED
                Determined Concentration (ug/kg)                            Relative
Matrix Spike =                                                  Spike     percent
100 (ug/kg)       ZSARM-I-l-F ZSARM-I-l-F MS ZSARM-I-l-F MSD   Spike   recovery    diffe-
                 F872167      F872170       F872171       recovery duplicate   rence
Pentachlorophenol
Anthracene
B1s(2-ethylhexyl)-
phthalate
NO
74
33

116
210
134

138
215
139

116
136
101

138
141
106

17
4
5

NO = Not detected.
    TABLE 5-14.   SEMIVOLATILES SPIKE RECOVERY  (ACCURACY)  AND RELATIVE
                     DIFFERENCE (PRECISION) FOR ASH
Determined Concentration (ug/kg)
Matrix Spike 
100 (ug/kg) ZSARM-I-l-A ZSARM-I-l-A MS ZSARM-I-l-A
F872151 F872159 F872160
Pentachlorophenol
Anthracene
Bis(2-ethylhexyl)-
phthalate
NO
ND
13
ND
90
200
ND
87
126
MSD Spike
recovery
0
90
187
Spike
recovery
duplicate
0
87
113
Relative
percent
diffe-
rence
0'
3
49
ND  Not detected.
   TABLE 5-15.   SEMIVOLATILES SPIKE  RECOVERY  (ACCURACY) AND RELATIVE
                 DIFFERENCE (PRECISION)  FOR SCRUBBER WATER
Determined Concentration (ug/kg)
Matrix Spike =
100 (ug/kg) ZSARM-I-l-F ZSARM-I-l-F MS ZSARM-I-l-F MSD Spike
F872139 F872149 F872148 recovery
Pentachlorophenol
Anthracene
Bis(2-ethylhexyl)-
phthalate
8
ND
ND
74
89
123
80
84
118
66
89
123
Spike
recovery
duplicate
72
84
118
Relative
percent
diffe-
rence
9
6
4
ND - Not detected.
                                    5-17

-------
          TABLE  5-16.   SYSTEM BLANK DATA FOR  SEMIVOLATILE  ANALYSES
                                 (TOTAL  yg)
Pentachlorophenol
Estimated Limits
of Detection
METHOD BLANK
F872138
METHOD BLANK
F872150
METHOD BLANK
F872163
REAGENT BLANK MeC12
F872178
REAGENT BLANK FILTER
F872179
REAGENT BLANK XAD-2
F872182
FIELD TRAIN BLANK
F872193
METHOD BLANK TRAIN
F872185
5
7
ND
ND ,
ND
ND
ND
ND
ND
Bis(2-ethylhexyl)-
Anthracene phthalate
0.4
ND
ND
ND
ND
ND
ND
ND
ND
0.7
ND
13
ND
ND
29
43
45
40
ND = Not detected.
                                     5-18

-------
                            TABLE 5-17.   SEMIVOLATILES SURROGATE PERCENT RECOVERIES
tn
i
Sample I.D.
SAI-SV-1
F872183
SAI-SV-2
F872186
SAI-SV-3
FB72187
SAII-SV-1
F872190
SAII-SV-2
F872191
SAII-SV-3
F872192
2-Fluro-
ptenol

77

52

68

64

65

69
d5-
Phenol

85

54

57

58

64

52
d5-Nitro-
benzene

88

66

68

55

63

57
2-Fluro-
biphenyl

95

97

97

90

93

96
2,4,6-Tri-
bromophenol

91

101

104

122

111

113
d!4-
Terphenyl

93

88

99

100

91

88
dlO-
Antracene

83

44

55

84

79

92

-------
                                      TABLE 5-18.  PEI WASTE FEED SPIKE RECOVERIES





in
i
ro
o
Analyte
Arsenic
Chromium
Zinc
Lead
Cadmium
Nickel
Copper
Analysis
Type
GF AAS
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
Method
Detection
Limit *
(ug/g)
0.040
0.300
0.120
4.200
0.120
0.300
0.420
Sample used Amount
for Spikes Spiked Matrix Spike
P7-09-023-19 in P7-09-023-25a
(ug/g) (yg/g) (yg/g)
16.9
24.2
451
261
26.3
27.5
244
20.0
100.0
800.0
300.0
100.0
100.0
600.0
28.8
115
1200
543
118
117
804
Matrix Spike Matrix Spike
Recovery Duplicate
P7-09-023-25a P7-08-023-26a
(% recovery) (wg/g)
78
93
96
97
93
92
95
30.3
121
1280
587
121
120
836
M S Duplicate Relative
Recovery Percent
P7-09-023-26a Differ-
(% recovery) ence (a)
82
97
102
105
96
94
99
5
5
6
8
3
3
4
MDL = Method Detection Limit
* Assuming 5 g samples in 100 ml total volume.
(a) Relative Percent Difference = (MS - MSD)/(0.5* (MMS + MSD).

-------
                                                TABLE 5-19.   PEI ASH SPIKE RECOVERIES
I
ro
Analyte
Arsenic
Chromium
Zinc
Lead
Cadmium
Nickel
Copper
Analysis
Type
GF AAS
I CAP
I CAP
ICAP
I CAP
ICAP
ICAP
Method
Detection
Li1t *
(yg/g)
0.040
0.300(a)
0.120
4.200
0.120
0.300
0.420
Sample used Amount
for Spikes Spiked Matrix Spike
P7-09-023-10a in P7-09-023-16a
(ng/g) (ug/g) (ug/g)
37.7
9.8
217
56.2
<1.48
11.8
111
20.0
100.0
1000.0
600.0
100.0
100.0
500.0
55.9
101
1130
610
87.7
102
604
Matrix Spike Matrix Spike
Recovery Duplicate
P7-09-023-16a P7-08-023-17a
(% recovery) (ug/g)
97
92
93
93
88
91
99
61.5
101
1170
604
87.6
103
585
M S Duplicate Relative
Recovery Percent
P7-09-023-17a Differ-
(% recovery) ence (a)
107
92
96
92
88
92
96
10
0
3
1
0
1
3
      MDL = Method Detection Limit
      * Assuming 5 g samples in 100 ml total volume.
      (a) Amount shown is a default value, but agrees with the amount found in the undiluted sample.
      (b) Relative Percent Difference = (MS - MSD)/(0.5* (MMS + MSD).

-------
                                         TABLE 5-20.  PEI SCRUBBER WATER SPIKE RECOVERIES
en
i
ro
Analyte
Arsenic
Chromium
Zinc
Lead
Cadmium
Nickel
Copper
Analysis
Type
GF AAS
I CAP
I CAP
I CAP
I CAP
ICAP
I CAP
Method
Detection
Limit *
(yg/ml)
0.001
0.008
0.003
0.105(a)
0.003
0.015
O.Oll(a)
Sample used Amount
for Spikes Spiked Matrix Spike
P7-09-023-01a in P7-09-023-07a
(pg/ml) (wg/ml) (yg/ml)
0.150
0.530
2.14
1.75
2.35
0.320
0.595
0.500
2.500
7.500
7.500
15.000
2.500
3.750
0.700
3.60
10.9
9.51
19.3
2.96
4.32
Matrix Spike
Recovery
P7-09-023-07a
(% recovery)
100
119
113
86
111
105
87
Matrix Spike
Duplicate
P7-08-023-08a
(yg/ml)
0.760
3.39
11.1
9.83
18.6
2.93
4.26
MS Duplicate Relative
Recovery Percent
P7-09-023-08a Differ-
(% recovery) ence (a)
117
112
115
89
107
104
86
8
6
2
3
4
1
2
     MDL = Method Detection Limit

     (a) Amount shown is a default value, but agrees  with the amount found in the undiluted sample.

     (b) Relative Percent Difference = (MS - MSD)/(0.5* (MMS + MSD).

-------
                                  TABLE  5-21.   PEI  METHOD  SPIKE RECOVERIES METHOD 12 TRAIN SAMPLES
in
i
ro
Analyte
Arsenic
Chromium
Zinc
Lead
Cadmium
Nickel
Copper
Analysis
Type
GF AAS
I CAP
I CAP
I CAP
I CAP
I CAP
I CAP
Method
Detection
Limit
W
0.200
1.50
0.600
21.0
0.600
1.50
2.10
Amount
Spiked
in
u9
10.0
500.0
1000.0
500.0
500.0
500.0
500.0
Method Spike
(total yg)
9.5
448
868
435
441
441
476
Method Spike
Recovery
(% recovery)
95
90
87
87
88
88
95
Method Spike
Duplicate
(total ug)
9.80
439
857
434
435
434
463
MS Duplicate
Recovery
(% recovery)
98
88
86
87
87
87
93
Relative
Percent
Difference
(a)
3
2
1
0
2
2
3
      MDL  =  Method Detection Limit
      * Assuming 100 ml  total  volume.
      (a)  Relative Percent Difference  = (MS - MSD)/(0.5* (MMS + MSD).

-------
            TABLE  5-22.   SUMMARY  OF  METHOD  12  BLANK  ANALYSIS  DATA
Analyte
Arsenic
Chromium
Zinc
Lead
Cadmium
Nickel
Copper
Analysis
type
GF AAS
I CAP
I CAP
ICAP
I CAP
ICAP
ICAP
Method
detection
limit
0.200
1.50
0.600
21.0
0.600
1.50
2.10
Sample 6750-A
nitric blank
P7-09-023-34a
(total vg)
0.300
<1.50
5.50
<21.0
<0.600
<1.50
<2.10
Sample 6750-B
filter blank
P7-09-023-35a
(total yg)
NA
NA
NA
NA
NA
NA
NA
Sample
method blank
P7-09-023-36a
(total yg)
<0.200
<1.50
3.00
<21.0
<0.600
3.20
<2.10
NA = Not available.
                                     5-24

-------
.003 mg/g.  Total particulate catch ranged between 40 and 100 mg and no blank
corrections were applied.  For the HC1  analysis, quality assurance included
matrix spikes, duplicate analysis, and  reagent blank analyses.  Table 5-23
summarizes these data.  Note that the 0.1 N NaOH blank analysis was inclusive
because of nitric interference.
5.3.5  Dioxin/Furans
     Quality assurance for analysis of  dioxin included system performance and
calibration checks, blank and duplicate matrix spike analyses.  These data
are summarized in Tables 5-24 through 5-26.
                                     5-25

-------
       TABLE 5-23  CHLORIDE ANALYSIS QUALITY CONTROL RESULTS
Description
ppm
Comments
Reagent blank
Method blank n               ND
Method blank #2               ND
Matrix.spike                 15.8
Matrix spike duplicate       15.1
Check sample #1 9.09 ppm      9.1
Check sample #2 9.09 ppm      9.0
          Nitric interferences
          98.1% recovery
          93.8% recovery
          99.89% agreement
          99.01% agreement
            TABLE 5-24.  DIOXIN/FURAN RESULTS SCRUBBER
                      SURROGATE RECOVERIES, %
Analyte
13C-2,3,7,8-TCDD
13C-2,3,7,8-TCDF
13C-1, 2, 3, 7,8-PCDD
13C-1,2,3,7,8-PCDF
13C-l,2,3,6,7,8-HxCDD
13C-l,2,3,4,7,8-HxCDF
Reagent blank
A710003-blank
37017
86
91
91
91
89
91
ZSARM 1-2-S
A710003-01A
37018
84
92
92
89
87
94
ZSARM-II-5-S
A710003-02A
37019
88
97
94
94
72
101
                                5-26

-------
TABLE 5-25.  DIOXIN/FURAN RESULTS FEED
        SURROGATE RECOVERIES, %


Surrogate
13C-2,3,7,8-TCDD
13C-2,3,7,8-TCDF
13C-1, 2, 3, 7,8-PCDD
13C-1,2,3,7,8-PCDF
13C-l,2,3,6,7,8-HxCDD
13C-l,2,3,4,7,8-HxCDF
Reagent blank
A710018
37031
86
89
89
86
80
78
ZSARM 1-2-F
A710003-07A
37034
71
68
95
82
77
76
ZSARM-II-5-F
A710003-08A
37035
78
80
91
87
76
92
 TABLE 5-26.  DIOXIN/FURAN RESULTS ASH
        SURROGATE RECOVERIES, %
Analyte
13C-2,3,7,8-TCDD
13C-2,3,7,8-TCDF
13C-1, 2, 3, 7,8-PCDD
13C-1,2,3,7,8-PCDF
13C-l,2,3,6,7,8-HxCDD
13C-l,2,3,4,7,8-HxCDF
Reagent blank
A710003-3540-BL
37022
83
89
92
89
74
88
ZSARM 1-2-A
A710003-04A
37020
86
94
94
93
86
96
SARM-II-5-A
A710003-05A
37021
86
98
93
91
86
94
                  5-27

-------
                APPENDIX A



COMPUTER PRINTOUTS AND EXAMPLE CALCULATIONS
                    A-l

-------
'Particulate,  HC1,  Senrivolatiles
                 A-2

-------
     NOMENCLATURE FOR SEMI-VOLATILE DESTRUCTION AND
             REMOVAL EFFICIENCY CALCULATIONS
ORE = POHC destruction and removal efficiency, %
FR  = SARM I or II feed rate, Ib/h
PC  = POHC concentration in MM5 sample, gr/dscf
PER = POHC emission rate, Ib/h
PFR = POHC feed rate, lb/ h
PF  = POHC concentration in SARM feed, wt. percent (Ib/lb)
PMS = POHC mass in MM5 sample, yg
      Stack volumetric flow rate, dscfm
SV  = Sample volume, dscf
                            A-3

-------
                           EXAMPLE CALCULATIONS


1)   SARM Waste  Feed Rate,  (FR) Ib/h


     (as determined for each individual run - see Section 2)


2)   POHC Feed Rate, (PFR),  Ib/h


          PFR =   PF  *  FR


3)   POHC Concentration in MM5 Sample  (PC), gr/dscf


     PC - P^ (yg) x io;La x iLpr  t sv (dscf}



4)   POHC Emission Rate (PER), Ib/h
     PER = P  (  gr.)    Q    .   60 min y    g       x    lb
            c  dscf   *  ssto  A    n~~ A 15.43 gr   *  453.6 g
5)   POHC ORE
                    (Ib/h)  -  PER  (Ib/h)     fl
                                        X 1UU
                      PFR  (Ib/h)
                                     A-4

-------
in
                              SUMMARY  OF  SEMI-VOLATILE  CONCENTRATION  AND  MASS  RATE  CALCULATIONS
                                                           SARM I
Test No.
Sample Volume (dscf)
Volumetric Flow (dscfm)
Analyte
Anthracene
Pentachlorophenol
Bis(2-ethylhexyl)
phtlate

1
141.243
1466
Total gr/
yg dscf Ib/h
ND
ND
185
a None detected
Method Detection Limit
Antracene: 0
Pentachlorophenol: 0
Bis(2-ethylhexyl)-: 0
a
2 X 2.5 X
10~5 10'"
(Total yg)
.4-2.9 yg
.3 yg
.4 yg
2
107.367
1342
Total gr/
yg dscf
ND 	
ND 	
9 1.3 X
10"6

3 Average
123.672 	
1427 1412
Total gr/ gr/
Ib/h yg dscf Ib/h dscf Ib/h
	 ND 	  	
	 ND 	 	 	
1.5 X 435 5.4 X 6.6 X 2.5 X 3.0 X
10"5 10"5 10'" 10"5 10~"

            phtlate

-------
                         SUMMARY OF SEMI-VOLATILE CONCENTRATION AND MASS RATE CALCULATIONS
                                                      SARM II
Test No.
Sample Volume (dscf)
Volumetric Flow (dscfm)

Analyte
Anthracene
Pentachl orophenol

Bis(2-ethylhexyl)
phtlate
Total
yg
NDa
5

14

1
117.072
1352
gr/
dscf
	
6.6 X
10"7
1.8 X
10 6


Ib/h
	
7.6 X
10"6
2.1 X
10"5

Total
yg
ND
ND

655

2
121.379
1456
gr/
dscf
	
	

8.3 X
10"5


Ib/h
	


1.0 X
10" 3
3
113.876
1413
Total gr/
yg dscf
ND 	
ND 	

38b 5.1 X
10"6
Average
1407
gr/
Ib/h dscf
	 	
	 	

6.2 X 3.0 X
10 5 10"5

Ib/h
	
	

3.6 X
10~"
a None detected

a Below MDL (44.0 yg/sample).

-------
              E I  ASSOCIATES.  INC.
             ; I G N  TEST   S E F 0 R T
                 I  ELD  DA T A

Test tisne '=4-a>-i--=--c;,
Sample tvpe 	
Bar. pressure (in-HE) ...
Static pressure in-H20)
F i 1 te" nuiTiDar ',5 	
Stack inside dia. un; ,.
c'itct tube coeff. .......
Total H20 csi leered >mlJ
Percent 02 b/ volume idr.,:
time
orin)
0.0
31. *
60.
0',.
' "! '
135.
is*:.
Io5.
ISO.
	 QUENCH OUTLET

	 FART.,rO EE^I-'OLS.
	 29.15

r  ;.-,_.,
,n
	 84

...:..
Gas mete'- velocity
reading head
r. -C
35'. 350 1.500
3S2.050 1.100
409. Er 1.400
433.531 i.100
447.000 l.''OC
455.400 0.9)0
470.20'! 0.950
480. 12S i.OO:
Run number .........

Leakage (cu-ft)
Mete1' calibration f&r
Data inter .-al ((nil
No'ile dia 	
Meter bo;; nusiter . . .
Number of traverse PO
Percent C02 bv volune
Percent CO by volume
Orifice Stack Dry g
drop-ac:. tenp. temp
Un. H20'1 !deg. F) inlet
2.93 179 82
2. 16 181 S'~
2.48 1S1 91
2.20 180 :;i
2.05 180 110
1.83 181 105
1.50 180 105
1.30 180 102
	 3AI-

0 '"'
to- 	 <<:

"Y|0

ints ....?
id-/. .,10.8
(dry! ...0.0
as meter
'deQ. F)
outlet
31
34
O.'i
94
109
105
IOC
0"
152.131
2.06
130
98
                          A-7

-------
                                              P E  I   ASSOCIATES.  INC.
                                       EMISSION  TEST  PEFORT
                                               TEST   RESULTS
FLANT: J. ZINK CD.
TEST: SAI-SV-1 / QUENCH OUTLET
TEST DATE: 9/16/87
TEST TIME: 1020-1413
          TT     	   Net tine of  test  lain.'

          NF     	   Net sampling pein.t=

          Y      	   Meter calibration  factor

          D-:	   Sampling nozzle oia  an!

          I-     	   Pilot tuts coe*ficier:

          PM	   Average orifice pressure drop (in-H20)

          VM     	   Volume o* dry  gas  saraplec
                              at nete' conditions  icu-ft'

          TM     	   Average gas  meter  temperature ideg f>

          VfiSTL  	   'vciurce e- dr.-  qe=  Sr'cisi
                              at standard  conditions  (set;

          VLC    	   Total H20 collected  :-;
                              iitiFingers and  silica gel (ml)

          VI4C    	   Volume of water vapor at
                              stindsrd conaitions  (scf

          BWC    	   Percent noisture  by  vol'.>n>e
                               (saturation  check  made)

          FMD    	   Mole  fraction  of  dry gas

          PCCC   	   Percent C02  by voiune  (dry

          fQI    	   Percent  02 b>  voljire '.dry)

          FZO	   Percent  CO by volume idry1

          PNI    	   Percent  N2 5y  volune 'Dry!

          !*!     	   r!:lecjiai-  weiht - a^v s:a:i- g?=
     180.0

         e

     0.999

     0.309

     0.840

      2.06

   152.181


      9o.6

   1-1,243


    2355.3


   134. 1"


     48.76
     10.800

      5.4'X

      0.00!'
      29.94
                                                              A-8

-------
                                       E S T  RESULTS
                                                                               PAGE NC: 2
                                                                               RUN NO: SAI-2V-1
 MS    	   Molecular weight - sta^  gas                          24.12

 PB     	   Barometric pressure 'in-Hv                            29.15

 PSI     	   Static c'-sssjr; o; =ta:l  gas 'i^-H"'                  7.600

 PS     	   Stac'r pressure - absolute 'in-HG                       29.41

 75     	   Average stact  temperature !deo  F                         180

 Vh     	   Average square root of  velocity  head  un-H20)         1.054

 VS     	   Average stack  gas velocity  ifpsj                        71.9

 A3     	   ttacfc area -sq ini                                       1:7

 GS     	   Actual stacl  How rate  iac-ir,!                          3,387

 OSS"   	   Stac! tioh rate - dry  iscfin'                           1,407

 I3C     	   Percent isounetic                                      84.1



 r     	   FIL'EFABLE =AFTICJLATE, MG                             142.8 /

CS      	   FILTERABLE PARTICULATE, GR/D5CF                       0.0156

FUR     	   FILTERAE^E-AFTI01A7E                                 6.156
                    Emission  rate,  Ifa/hr
MN     	    TOTAL  CHLORIDES AS HCL, CIG                              3o.6^/  "Z-"~>->
                                                                                      ~'     ^

Co    	     TOTAL  CHLORIDES A5 HCL, 3R DSCF                       3.9954E-C3     ^     -

PM?    	    70TiL  CHLORIDES AS HCL                                 0.048
                    Emission  rate, Ib/h-
                                                  A-9

-------
                               P E I   ASSOCIATES.  INC.
                         EMISSION  TEST  R  F 0 P T
                                  FIELD  D A T ft
Samp Imp location ......
Test tine (start-stop) ..

Bar. pressure (in-HG) , ..
^tot'c pressure (int^Q1'
Filter numbs*1'1) 	 	
c>,-> incide uia (in1
Pitot tube coeff. .......
Total H2C collected (ml!
Percent 02 by volute (dr>
Sample
time
on)
0.0
22.5
45.0
67.5
9i.O
112.5
135.0
157.5
180.0
	 QUENCH OUTLET
	 1625-2030
	 PART./HCL;'SEMi
, 	 29.11
+4.0
	 873004 ""
. 1"
	 ..84
	 2507.4
...5.8
6e5 meter
reading
(cu. ft.)
480. rt
493. 13*:
506.500
en* t -
535.664
551.080
56fc.7S:
581.580
596.738


[-VOLS.







velocity
heac
u.-,. K2-'
1.050
1.200
1.100
0.930
1.200
1.200
1.000
1.1 Ov
Run number ...............


Heter calibration factor .
Data interval (mir, i ......

Meter box number 	 	
Number C"f traverse Poi^fE
Percent C02 by volune iflry)
Percent CO by volume (dry!
Orifice Etac- Dr> gi= met
drop-act. temp. temp \deg.
	 SAI-S

	 O7
	 999


....FT"
n
..10.4
...0.0
F!
(in. K20) (de:. F) inlet outlet
0.88 177 100
1.00 179 96
1.25 179 '
1.12 181 100
1.37 1E1 CE
1.37 181 101
1.15 181 101
1.2t 181 102
co
97
w1"'
91
07
95
96
97
1BO.O
Hi. 362
is:
100
                                                                                   C-
                                             A-10

-------
                                              F  E  I   AS30CIflTE3.  INC.
                                       E  rl !  S S I 0  N   T  E  E  '   '  E  F 0  R  T
                                               TEST   RESULTS

PLANT:  j.  :iNf  ::.
TEST:  SAI-SV-:  / QUENCH OUTLET



          TT     	   Net  time of  test  (mm*

          NF     	   Net  sampling points

          K       	   Mete''calibration  factor

          [ft     	   Sampling nozzle d:a  (in)

          CP     	   :::::  :.: :3e*fiziart

          PM     	   H.e-age  on*ice pressure drop  dn-H20)

          v'F     	   Vc'luTie of dry ga;  samplej
                             at meter corsiuops  icii-ft;
                              'corrected for ieatace)

          TM     	   Avenge  gas meter  temperature  (deg P)

          '.'*5~I'   	   Volune of dry gas  sampled
                             at standard conainons  (scf)

          VLC     	   Total  H2C collected  in
                             impingers and silica gel (!)
                             'at  satiration1

          VWC     	   Volure 3* water vapor at
                             standard conditions  (set,
                             (at  saturation)

          Ml     	   Percent  noisture by volume
                             (at  saturation)

          PMD     	   Mole fraction of dry gss

          ::02    	   Percent  C02 by voluire !d>-y)

          PCI     	   Percent  02 Dy volume idr\'

          Flj     	   Percent  CC D> .'olume (dry)

          PN2     	   Percent  N2 by volume 'dry;

          MC      	   Molecular Height - dry stact. gaA-11
TEST DATE:  9, liT
TEST TIME:  1625-2030
     130.0

         e

     0.0
-------
                                     TEST  RESULTS
                                                                                PAGE NO:  :
                                                                                RUN NO:  SAI-Sv-2
MWS    ..........   Molecular weight - stack gas                           23.72

PB     ..........   Barcetric pressure un-HG)                            29.11

PSI    ..........   Static pressure of stack gas lin-H20)                   4.000

PS     ..........   Stack pressure - absclute  (in-HG)                      29.40

TS     ..........   Average stack temperature  (de= F)                        130

VH     ..........   Average square "oct o1 velocity  head (in-H20)         1.050

VS     ..... .....   Av6f53e staci. gas velo:ity dpsi                        72.2

Ai     , .........   Etrc  5"s= (sq in1                                       113

CE     ..........   Actual stscl-  flew rate (i'.iitti                          3,403

OSSTD  ..........   Stsci- flow rate - dry (scf n)                           1 , 32"

ISO    ..........   Percent i sonnet ic                                     103.6



MN     ..........   FILTERABLE PARTICULATE,  MB                             115. 6 "'

C?     ..........   FILTERABLE PARTICULATE,  6R/DSCF                       0. Ola6
                    F I^TERATLE FARTIZULATE                                 0. 189
                    Emssion rate, lfi/hr
                    TOTAL CHLORIDES AS HCL, Mt                              31.1 S    -
                                                                                         r-     \
CS    ..........    TOTA. CHLORIDES AS HCl. & 'D33F
PMF    ..........   TOTAL CHLORIDES AS HCL                                 0. 05!
                    Emission '"ate, lt>/lv
                                                   A-12

-------
                                P E  I  H3SGCIftTE5.  INC.


P'a't



Saflcl'ni Inrsti.T. 	
Test tine
^fl-]g K,
(start-stop ' . .
c 	
Bi-". pre5S"rP lTn-HIS> 	
Stati~ -re

= < rl-
Pi tot t:'De
TotM H2C
ps--:e-t 02











.- a ,__--!
bpr" ' =  ...


coilerted '.ml) .
by L.;L'T-e dry!
"'tii
Tin"
0.0
22.5
4!.C
o7.5
9( . 0
1*2.5
13:. ."
157.5
180.0
E K I  S I 3  T E
FIELD
' 'IN1 r"
	 QUENCH OUTLET

	 PAPT.HCL/ SEMI-VOLE.

44 i-.
;".-),- = '
,n

	 27".9.5
...5.4
3ii meter velocity
reading head
(cu. ft.' fin H2fli
597.654
611.250 1.000
=:".500 1.400
643.370 1.3!-.'
653.655 1.300
0^3.700 1,100
688. 48C 1.100
703.330 !.3'!0
718.546 1.000
5 T P E P C R T
[ATA
Date 	 9/1""


Leal-age (cu-ft) 	 	 	 0.0

D'ts interval 'iir/r. ' .......... I. c
Nozils dia. 	 	 ,..25
Metsr box number 	 	 FT"
Number of traverse pcir.t5 ,..,8
Percent 202 bv volume (cr, ,.;0.s
Percent CO by volume (dry) ..,(.,(
Orifice Stack Dry gas /peter
drop-act. temp, tec dej. ?'
(in. H20) ideg. F/ inlet outlet

1.09 178 84 83
1.53 PS 8" 33
1,42 181 91 5
1.38 182 94 88
1.21 183 92 91
1.22 182 95 91
1.35 179 93 :
-------
                                              P E I  ASSOCIATES. INC.
                                       EMISSION  TEST  REPORT
                                               TEST  RESULTS
PLANT: J. ZINI  CO.
TEST: SAI-SV-3 / QUENCH OUTLET
TEST DATE: 9/17/87
TEST TIME: 1041-1409
          TT     	   Net time o* test (Bin)

          NP     	   Net sampling points

          Y      	   Meter calibration +actor

          DN	   Sampling no::le dia  (in)

          CF     	   c;tct tutt coe-t:;:s-t

          PM     ..........   Average orifice pressure drop  (in-H20)

          W     	   Volume of dry gas sampled
                              et meter conditions  ice-ft'

          TM     ..........   Average gas aeter temperature  (deg F)

          VMSTD  	   Volume of dry gas sampled
                              at standard conditions  (scf,1

          VL!    	   Total H20 collected  in
                              impingers and silica gsl  (ir,i!
                              (at saturation)

          VWC    	   Volume oi water vapor at
                              standard conditions  is:t)
                              (at saturation;

          BWO    	   Percent Boisture :>'volume
                              (at saturation)

          FMD    	   Mole fraction o-f dry gas

          PCO:   	   Percent CK :> vclurs  'dr., 

          P02    	   Percent 02 by volume  (dry)

          PCO    	   Percent CO by volume idry,

          PNI	   Percent M tv volune  (d>r;,

          HD     	   HcleiL'.ar KS:9^t - dry  stac!  Q5S
                                                            '  A-14
     180.0

         8

     C.995

     0.250

     0.9J0

      1.29

   120.sc:


      90.6

   114.046


    2626.6



   123.672
      0.46

     10.60C

     5.400

     o.(o:

     84.00.;

     2r-.r-l

-------
                                     TE3T  RESULTS
                                                                                PAGE NO: I
                                                                                RUN NO: 3A!-S.'-3
MWS     ..........   1o.e:.:lar weight - stad gas                           2!. 71

PB      ..........   Barometric pressure  ( in-H5,-                            29. 37

?il     ..........   Stat:: pressure c* star- :  :r-N20                   4.000

F5      ..........   stact pressure - cDsslute  'ir,-H3>                      29.66

T      ........ .,   i,/e-'age sta;! temperature  ',deg F)                         1S1

VH      ..........   Average square root of velocity  head  dn-H20>         1.088

VS      .. ........   Average stacMas velocity  ffcs)                        74.5

HI      ..........   stack area (sq in;                                        113

OE      ..........   Actual stact  tiop. rats  'ac^v                          3,511

QE3TD   ..........   Sta:k How rate - dry 'sc*'                           1,377

ISC     ..........   Ferce-t i=olir,etic                                     106.0



MN      ..........   FILTERABLE P*TICUL-'E.  PIG                              90. 9  /

IE      ..........   FILTERABLE PARTICULATE,  GP-D5C-                       0.0123
                    FILTERABLE PARTICULATE                                 0.145
                    Emission rate, Ib/hr
UN     	   TOTAL CHLORIDES AS HCL. MG                              21.3  

15    	     TOTAL CHLORIDES AS HCL, GfvDSCF                       2.8813E-03

PUR    	   TOTAL CHLORIDES AS HCL                                 0.034
                    Emission rate. Ib/hr
                                                   A-15

-------

P
E I ASSOCIATES.
EMISSION TEST

Plant

Test time ietai*t-stop) . .
Ssflip le type

Cfat i r nroccj ire f i n H^Ol


Fitot tube coet*. .......
Total H20 collected (!>
Percent 02 by volume (Cry,1
Sample
tifre
O.v
-^ e
**. j
45.0
o".5
3, ,u
112.5
135. :
15". 5
172.1

J ZINK CO.
QUENCH OUTLET
	 1655-2015
FIELD CAT



.PART''HCL.'CE!*I-VCLS.
29 37
+4 '1

INC.
REPORT
i\
M
Datf=
Run

















	 -,17/S7
	 SAII-SV-1

	 0.0

Dats interval


1 " Nptpr hoy numher 	
	 84
	 2495
c <
Gas meter
reading
(cu. ?:.'
719.948
733.670
748.810
7c3.!?:
778.873
794. 190
Sv'JSO
825.450
835.270
~" C
	 25

Number of traverse points ....6
Percent C02 by volume (dr> ; ..11
Percent CO by volume (dry) ...0.0
'V.0::t>
heaa
!ir,. H20)

0.900
1.100
1. ':':'.
1.200
1.200
i.io:
1.300
1.300
Griuce Staci
drop-act. temp.
(in. H2Q) (deg. F-

1.01
1.24
1.13
1.35
1.35
1.22
1.45
1.45

180
178
IS!
182
181
IB!
182
181
Dry gas mate-'
tern? (deg. F,
inlet outlet

104
105
106
1'"'7
102
101
100
9=

102
102
1C2
i !'2
101
9s
"5
94
115.322
1.134
1.28
181
                                                                1'Ai
                          A-16

-------
                                               P  E  I   Ap50CIfiTE5.  IMC.
                                              SSION   T   E  -  ? E F  0 F T
PLANT: J. II* CC.
TEST: SAII-SV-i / QUENCH OUTLET
                                                TEST   RESULTS
TEST DATE: ?, IT, S7
TEST TIME: 1655-2015
          TT     	   Net ti.TS or  test  imin-

          NP	   Net rsmclina points

          Y      	   Meter calibration  tactar

          DN     	   Sampling no::le dia  un)

          CF     	   ::t:t t.L'5 zse+'ficient

          PM	   Average ontice pressure  drop  ur,-H20>

          W     	   v'ciu/ne c+ :_/ ;a;  sir^ieo
                              at meter c:nditior,=  (cj.-ft)

          TM     	   A/erage gss (nets-'  temperature  (deg  F)

          VMSTt  	   vein": o* dr/ ge;  saT^:52
                              at standard condition5  isct;

          'A.C    	   Total H20 :olle:tec  in
                              iin?inqe'is and silica gel  (ml)
                              (at saturation,

          VHC    	   Volune oi water vapor at
                              standard conditions  (scfi
                              vat saturation)

          BWO    	   Percent moisture bv volume
                              !at saturation

          CMD	   Mole fraction of dry gas

          PCOI   	   Fercent C02 by volume (or;, -

          PQ2    	   Percent 02 By volume (dry)

          PCD    	   Percent CO ay vclur.e  dry)

          P'	   F=rc=?t NI b> /oljff.s  dr..)

          MD     	   Mclecular Neisl-t - 2"v stC(- gas
                                                             A-17
     172.1
     0.250

     0.840

      1.26

   115.322


     iOl.3

   106. "1?
   117.V7:



     52.31


      0.46

    ll.'X)?

     5.100

     0.000

    83.900

     29. 5a

-------
                                     TEST  RE5ULTS
                                                                                FAGE  NO:  2
                                                                                RUN NO:  SA1I-SV
HUE    ..........    Molecular weight - stacl.  gas                           23.7!

F'B     ..........    Ba^onetric pressure (in-H6/                             29.37

F5I    ..........    Static Pressure of stack  sas un-H2G)                   4.000

F5     ..........    S:aa pressure - aosolute Un-HG!                       29.66

TE     ........ ..    v'e;a== stact  teir^erftjre ',deg F>                         181

VH     ..........    Average square root 2* velocity  nead dn-H20)         1.065

VS     ..........    Average stack gas velocity  ifps)                        73.0

AE     ..........    Etacl area (sq IP                                        113

Q3     ..........    Actual stacl  flow rate iscfir,                           3,439

QSSTD  ..........    Stac'r -flow ra:e - dry iscfT,!                           1,340

150    ..........    per:ent iso' ir
-------
1 1 1 -
ii _ i  m
    in  ,,.
          '"
                         i r   u i               l_r J
                         1 1    -  IT t  f "       -
                         O   i 1  f  j  t      o
                           -  i i    .  u_ co  '-*
                                                    -
                                           i_    -0
                                           r-      
                                           o  QJ
                                           CL  e  m

                                            .2  
                                           U>  O  * 
                                       u   v.  .>  o
                                       OJ   01      >
                                      -Q   .--  >-.
                                       6   01 .O  >-,
                     - -  . - <  at   r-.   x  - \- t_)
                          m  *  in   o   o
                      ai   u  c;      -o      -*->
                 cj


     t_   01  OJ  qj
                                        ;  , : a.
                     
                       III
                      m  >ii  4- -
                                       -I   -       Of
                                               o   e
                                               ni   r!
                                            _  4_>  ,.-
                                       iU  'V  1.1   O
                                       IU  LJ  Cl  3
 Qj       -*->  r- -   |i>
 i    i I   O  ni   i j
'    m   *>--   sL.
 . <   *    ,^  n   (XI
I j    i)   u.  t-   ci_
                                >
                              t.  ai  ai
                             CH  -4-*  .-
                                                                v^  y  jc
                              -  S  R
                              X  c  =
                              111  T3  --
                              is  n>
                                  an
                              ui  :--   n
                                                   -O  o-  i > r  i  J  ^o  OO r
                                                   -o  -o  t^v r-  r ~  r-  r- i ,
                                                                                     Cr-  -^*  ~i  <  ^-  '^> to i 4
                                                                                     r-cocucacorDCari)
                                                                                     -o  co to  cr-  t--  i-- t-> r-
                                                                                        -o  :>  o-  -^-"r4r4i<
                                                                                         8C' 'O  O  O  0 T-  O
                                                                                         O -  -O  O  O -  O'
                                                                                     f '  r-j r-j  r    o  -  f
                                                                                 n  cr-  f -.  -o  co  r ">  co i 4 r -
                                                                                  -i  cf   -o i    TO  o   . r -. -
                                                                                  r)  CO  ro CO  ro  O-  Cr- ir- Cr-

-------
                                              P E I  ASSOCIATES. INC.
                                       E H I  5 I 0 N  TEST  REPORT
                                               TEST  RESULTS
TEST:  SAII-SV-2 / CUENCH OUTLET
                                                                      TEST DATE:  9/18/37
                                                                      TEST TIME:  0944-1308
          TT     ..........   Net time of test (am)

          NP     .....,...,   Net sampling points

          V      ..........   Meter  calibration -factor

          D',     ..........   Sampling no::le dia  (in)

          CP     ..........   Pitot tube coefficient

          PM     ..........   Average orifice pressure drop  uri-hlD)

          ,'M     ...... ....   Volume :* dry ?a= sampled
                              at meter conditions  (cu-ft)

          TM     ..........   Average gas meter temperature  (deg  F)

          V"!:T[  ..........   VclifT:? ?* :;, sfi sair.PiE5
              '                at standard conditions  (set)

          C:    ..........   T::;l '-Cj C2".ls:te:  i-
                              impingers and silica gel  (ml)
                              (at saturation:

          VWC    ... .......   Volune of water vapcr at
                              standard conditions  is:*'
                              (at saturation)

          Bfl'C    ..........   cercent moisture By  volume
                               ',at saturation)

          FMI-    ..........   fcie  fraction o- dry gas

          PCCI   ..........   Percept CG2  bv  /cl'.Te 'dry'

          PCI    ..........   Percent 02 by volume (dr.,)

          PCI    ..........   Fe-cer.t C5 Q> volume '.dry
                                                                           1BO.O

                                                                               8

                                                                           0.99
-------
                                              F E 5 U L T 5
                                                                                PAGE ND: 2
                                                                                RUN NO: SAII-E.-2
HWS     	   Molecular iieignt - stad-gas                           23.6?

FB      	   Barometric pressure  -in-KG!                            29.50

FSI     	   Static Bistre o* =:?:' ;i;  (ir-u20;                  4.000

PS      	   Steel pressure - absolute  un-HG1                      29. ?9

TS	   Average start-' temperature  tdeq r>                        131

Vh      	   Averace square root o-f  /elccity  head  fin-H20)         1.1*5

'.'E      	   Average 5tac^ gas ',elocit>  '*?=>                        78.4

A3      	   St3Cl J-'ei  =q ID;                                       113

QS      	   Actual stacl- UOH rate  (acfi;                          3,693

GS3TE   	   Etact ^l;w rsts - 3.-.   =.:--"                           1,443

I5C1     	   '5i'c;rit isoHneti:                                      93.<;



UN      	   FILTERAELE FARTICXATE, H6                              43.4  /

CS    	    FL'tRABLE PATICULftTE, GF.'DSCF                       6.0673E-:3

FMF     	   FILTERABLE FA/TICULATE                                 0.075
                    Emission rate, Ib/hr



K'<      	   TOTAL CHLORIDES AS ria, M6                              10.2  /

CS    	    TOTAL CHLORIDES AS HCL, 3R/D5CF                       1.4259E-03

FMR     	   TOTAL CHLORIDES AS HCL                                 0.018
                    Emission rate.  Ib, nr
                                                   A-21

-------
           F E I  ASSOCIATES.  INC.
    E M I S  I D N  TEST  KE  F D P.T
              FIELD  D A T A
Sampling location ........
Test tun* (etart-stncT
Saio ' e
tvce 	 	 	 	
Bar. proseiiro lip-HRi 	

Filter
Stact
Pi tot
T-.tsl
preesure iiri-H''0! .

inside die. lini , . .
tube coef*. ........
H?0 rnllprtpri (ml i .
Eercert 02 by volume (dry!











Sample
time
'.Tin'1
0.0
nn c;
45.0
e7.5
:0.(
112.5
135.0
15". 5
180.0
....QUENCH
....rso-i?
OUTLET
IS






....PfiPT/HCi /SFMT-vni 5.

+4 f
87"0<">4C
....12

....2E55
...5.4





Ipakaop (en ft)
	 SAII

	 O.rt
Mptpr calibration factrir 	 999






Data interval (
Nr.TTlp riia. ..
mint ^ c


Nunfapr o^f traverse pninr= 	 P


Gas meter
readirq
!CU. (
947.
962.
"r7.
9^2.
10:?.
1022.
036.
1050.
::=5.
t . '
944
540
390
E'l
43i
210
815
BOO
-i.1


Velocity
head
in. K20>

1.350
1.400
1.45''
1.300
1.400
1.300
1.200
1.4'V




Orifice
drop-act.
.:-. r2u)

1
1
1
1
1
1
1
1

-!"*
.27
-^
.19
.28
.1"
.11
.29'
Percent C02 bv
Percent CO by v
Stack
teflP.
volume i.d'<) ..11.1
'OlUFi5 ',C'". i . . .".'"'

Dry gas mete''
temp ideo. -
(des. Fi ir.let ottiet

IB:
181
1=1
iSl
161
151
Ibl
182

75 75
73 73
91 75
84 77
BO "8
82 7E
35 "
87 80
II"1.700
1.349
1.24
82
                          A-22

-------
                                              P E i   ASSOCIATE;,
E * I  E
                                                     N   TEST. REPS  P  T
                                               TEST
PLANT:  J.I II :G
TEST:  SAII-SV-3 / QUENCH OUTLET
                                         TES~  DATE:  9/16/87
                                         TEST  TIME:  1350-FIB
          TT

          NF

          Y

          DM

          CF
        	   Net time of test  (mm;

        	   Net sailing points

        	   Meter calibration factor

        	   Sampling no::le dia (in)

        	   Fuct tubs coefficient

Ff      	   Average orifice pressure drop iin-H20)

/If      	   Volume of dry gas samplsfl
                    it nete-- :3nd:ticrE ':.  t>

TM      	   Average gas meter temperature (deg F)

WIsTD   	   voluiie of dr-y gas =?mplec
                    at standard conditions iscf)

VL:     	   Total H20 collected in
                    iflipingers and silica gel iml)

VWC     	   Volume of water vapor  at
                    standarc conditions (scf)

BWO	   Percent moisture by volume

FMD     	   Hole fraction of dry gas

PC::    	   Percent CC2 by volume  (dry)

P02     	   Percent 02 By volume '.dry,1

-'CO     	   pe-cent CG by volume '.dry)

PN2	   Percent N2 by volume (dry)

MD      	   Molecular weight - cry stacl gas
                                              180. 0

                                                  6

                                              0.999

                                              0.250

                                              O.S4C

                                               1.24

                                            117. 700


                                               79.2

                                            1 13.876
                                                                                  134.335


                                                                                    54.17

                                                                                     0.46

                                                                                   11.100

                                                                                    5.400

                                                                                    0.000

                                                                                   83.500

                                                                                    29.99
                                                            A-23

-------
                                     TEST  RESULTS
                                                                                FA6E NC;  2
                                                                                RUN NO:  SAII-E.
MWS    	    Molecular weight - stack gas                           23.50

PB     	    Baraietric pressure (in-HG)                             29.50

F5I    	    Static pressu-e of stack gas dn-H20)                   4.000

PS	    Stack pressure - absolute (in-HG)                       29.79

TE     	    Average stack temperature ideg F)                         181

VH	    Average square root ct velocity  hearf Un-H20)         1.161

V;     	    Average stack gas velocity (4ps)                         79.8

AE     	    Stack area *sq in)                                       113

OS     	    Actual stack  HOK rate (acfir,}                           3,7ol

C:TI'  	    StacJ' floh rate - dry (sc'm1                            1,415

!SI    	    Percent iscunetic                                     103.1



M:     	    FILTERABLE PARTICULATE.  MG                              41.3 %/

CE    	     FILTERABLE PARTICULATE,  GR/DSCF                       5.5961E-03

PMF    	    FlLTERhSLt PARTICULATE                                 0.068
                    Emission rate, Ib/hr



MN     	    TBTflL CHLORIDES AS HCL.  MG                               e.9  ^

C    	     TOTAL CHLOF:IDEE AS HC.,  3='ZECF                       9.349E-OA
                    TOTAL CHLORIDES AS HCL                                 0.011
                    Emission rate, Ib 'hr
                                                   A-24

-------
                         Nomenclature and Dimensions
   A  = cross-sectional area of stack, ft2
  B   = proportional by volume of water vapor in the gas stream,  dimension-
   ws   less
   C  = pitot tube coefficient, dimensionless
 % CO = percent of carbon monoxide by volume, dry basis
% C0? = percent of carbon dioxide by volume, dry basis
   M . = dry molecular weight, Ib/lb-mole
   K  = molecular weight of stack gas (wet basis), Ib/lb-mole
 % N,, = percent of nitrogen by volume, dry basis
 % Qr - percent of oxygen by volume, dry basis
   AP = velocity head of stack gas, in. H-O
   P  = absolute stack gas pressure, in.Hg
   Q  = volumetric flow rate, wet basis, stack conditions
Q     = volumetric flow rate, dry basis, standard conditions
 sstd
   T  = average temperature of stack gas, R
   V  = stack gas velocity at stack conditions, fps

Note:  Standard conditions s 68F and 29.92 in.Hg.
                                     A-25

-------
              Fxample Calculations for Participate  Emissions
1.    Volume of dry gas samples corrected to standard  conditions.   Note:

     V  must be corrected for leakage if any leakage  rates  exceed  L..
      m

                  17.65 x Vm x Y
2.   Volume of water vapor at standard conditions, ft3.
           w
                  0.04707V
            std
                          1.
3.   Moisture content in stack gas.


                    V.
                     w
                      std
           ws
                          .
                          std
4.   Dry molecular weight of stack gas.



          Md = 0.440 (% C02) + 0.32C (% 02) * 0.280 (% N + % CO)






5.   Molecular weight of stack gas.



             K_ L/l  /ID  N u. 1 O D
             = HJ I 1-15 _ ) * io D.
           s    d     ws'       ws




6.   Stack velocity at stack conditions, fps.





          Vr  85.49 Cp
                                  avg.
 7.   Stack gas  volumetric  flow  rate  at  stack  conditions,  cfm.
           Qs    60  x  Vs  x
 (continued)
                                         A-26

-------
Example Calculations for Participate Emissions (continued)
8.   Dry stack gas volumetric flow rate at standard conditions, cfm.
Q,    = 17.65 Q
 sstd          s
                                 -B
                                   ws
9.   Concentration in gr/dscf.

                            M
          C's = (0.01543)
                           m
                            std
10.  Participate mass emission rate, Ib/'h.
              =  7(30% x Qsstd x 60
11.   Isokinetic variation.
               100 T.
              0.002669  'c + 'm  Y

                     60  e Vs Ps An
                                                bar 4
 12.   Particulate  concentration  correction to 7%
                n  o2  -             ,21-7   ..;
                                    cl-  A U,j
                                     A-27

-------
                    SAMPLE CALCULATIONS FOR HC1 EMISSIONS
1.   Volume of dry gas sample corrected to standard conditions  (68F,  29.92
     in.Hg, and zero percent moisture)
          VMstd = ^see MM5 ComPuter Data Sheet)



2.   Concentration of Cl" in sample, gr/dscf
          CP1- = (0.01543)     Mn
           Li                y

                             vmstd
     where Mn = total  chloride in sample, mg



3.   HC1 Mass Emission Rate, Ib/h
     Pmr = Cur.. v  Q--4.J v 60 min  v      q      v     Ib
                x   sstd x    x             x
                                        >    gr         >   g
                                       A-28

-------
 I
ro
                                                                                                                          o


                                                                                                                         O
                                                                                                                         m
                                                                                                                         co

-------
             Example Calculations for Volatile  Organics  (POHC's)
POHC Feed Rates, Ib/h
          POHC feed rate, Ib/h = PC * FR
where
     F.R. = measured feed rate of SARM I or II, Ib/h
     PC = POHC compound concentration expressed as  a  weight fraction  (Ib/lb)
VOST Sample Data
               Vstd = Vm X Y X 17-647 x ~
                                         m
where
     V   , = sample volume at standard conditions, liters at 20C,  760 mm Hg
      sta   (68F, 29.92 in.Hg)
       V  = volume metered, liters
        m
        Y = dry gas meter calibration factor
       Pb = barometric pressure, in.HG
       T  = meter gas temperature, R
   17.647 = conversion to standard conditions, 528R/29.92 in.Hg
POHC cone, ng/liter = total ng in sample/V ..
POHC emission rate Ib/h = ng/liter X 10"9 g/ng X  11b    X 28.317  liters /ft3
                                                 453.6 g
                         x Q .., dscfm X 60 m/h
% ORE -lb/n ^eed " ^b/h emission rate  x
                 Ib/h feed
                                     A-30

-------
                                  CALCULATION OF  VOST SAMPLE CONCENTRATIONS
                                                       SARM  I
                                                CALCULATION OF VOST SAMPLE CONCENTRATIONS
                                                               SARM I
Samples Nos. and Volumes, dNl




i
CO


Compound 10
Acetone
Cholorobenzene
1.2-01chloro-
e thane
Ethyl benzene
Styrene
Perchloroe-
thylene
Xylene
1A IB 1C
21.016 19.357 18.659
ng ng/1 ng ng/1 ng ng/1
N0b
28
NO
230
130
NO
230
120
1.3 13
NO
10.9 74
6.2 53
NO
10.9 83
6.2 210
0.7 7
NO
3.8 29
2.7 22
2
4.3 71
11.3
0.4
--
1.6
1.2
0.11
3.8
Run 1
average
ng ng/1
110
16
NO
111
68
0.7
128
5.8
0.8
--
5.4
3.4
0.04
6.3
2A
19.887
ng ng/1
76
9
10
97
40
9
190
3.8
0.5
0.5
4.9
2.0
0.5
9.6
28 2Ca Run 2 3A
19.125 18.896 average 20.432
ng ng/1 ng ng/1 ng ng/1 ng ng/1
75
2
NO
7
24
ND
37
3.9 Tube broke 76
0.1 -- -- 5.5
- 5
0.4 -- -- 52
1.3 --  32
   4.5
1.9 -- -- 114
3.9 67
0.3 60
0.25 16
2.7 120
1.7 340
0.25 24
5.8 180
3.3
2.9
0.8
5.9
16.6
1.2
8.8
19
ng
110
130
17
170
760
29
180
38
.207
ng/1
5.7
6.8
0.9
8.9
39.6
1.5
9.4
3C
19.283
ng ng/1
120
6
45
370
90.0
48
520
6.2
0.3
2.3
19.2
4.7
2.5
27.0
Run 3
average
ng ng/1
99
65
26
220
397
34
293
5.1
3.3
1.3
11.3
20.3
1.7
15.1
' Tube broken In shpiment, sample void.

b NO * Non-detectable (See Section 2.0 for Detection Unit Data)

-------
CALCULATION  OF VOST  SAMPLE CONCENTRATIONS
                   SARM II
              CALCULATION OF VOST SAMPLE CONCENTRATIONS
                           SARN II
Samples Nos. and Volumes,





>
i
CO
ro



Compound ID
Acetone
Cholorobenzene
1,2-Dlchloro-
e thane
Ethyl benzene

Styrene
Perchloroe-
ethylene
Xylene
1A IB
19.471 19.875
ng ng/1 ng ng/1
NO
NO
ND

U

NO
2

17
ND
10
ND

0.6 47

240
0.1 3

0.9 82

0.5


2.4

12.1
0.2

4.1
1C Run 1
20.142 average
ng ng/1 ng ng/1
ND
NO
ND

NO

ND
ND

ND
ND
3.3
ND

20

80
1.7

33

.17


1.0

4.0
0.1

1.7
2A
21.653
ng ng/1
NO
4
ND

14

7
7

47

0.2


0.7

0.3
0.3

2.2
28 2C*
20.724 19.229
ng ng/1 ng ng/1
ND
9
NO

20

ND
5

78
 ND
0.4 2
 ND

1.0 6

3
0.2 3

3.8 30

.10
	

0.3

0.2
0.2

1.6
dNl
Run 2
average
ng ng/1
ND
5 .23


13 0.7

3.3 0.2
5 0.2

52 2.5


3A
20.497
ng ng/1
13
5
ND

16

7
21

49
0.6
0.24
__

0.8

0.3
1.0

2.4


38
20.590
ng ng/1
NO
2
2

7

3
6

18

0.1
0.1

0.3

0.2
0.3

0.9


3C
18.303
ng ng/1
11
6
2

12

6
5

35
0.6
0.3
0.1

0.7

0.3
0.3

1.9


Run 3
average
ng ng/1
8
4.3
1.3

12

5.3
11

34
0.4
0.2
0.1

0.6

0.3
0.5

1.7

-------
                             CALCULATION  OF VOST MASS  EMISSION  RATES
                                                 SARM  II
                                            CALCULATION OF VOST MASS EMISSION RATES
                                                         SARM II
SAMPLES NOS.
Compound ID
Acetone
Cholorobenzene
1,2-Dichloro-
ethane
Ethylbenzene

Styrene
' Perchloroe-
oo ethylene
Xylene
1A
ng/1
NO
NO
NO

0.6

NO
0.1

0.9
IB
ng/1
NO
O.S
NO

2.4

12.1
0.2

4.1
1C
ng/1
NO
NO
NO

NO

NO
NO

NO
average
ng/1
--
0.17
.-

1.0

4.0
0.1

1.7
Run 1*
average 2A
Ib/h ng/1
NO
8.9 X 10"7 0.2
D

5.3 X 10"6 0.7
c
2.1 X 10 0.3
5.3 X 10~7 0.3

8.9 X 10"6 2.2
2B
ng/1
NO
0.4
NO

1.0

NO
0.2

3.8
2C
ng/1
NO
0.1
NO

0.3

0.2
0.2

1.6
Run 2*
average average 3A
ng/1 Ib/h ng/1
0.6
0.23 1.2 X 10"6 0.24
NO

0.7 3.7 X 10"6 0.8
c
0.2 1.1 X 10  0.3
0.2 1.1 X 10"6 1.0

2.5 1.3 X 10"5 2.4
3B
ng/1
NO
0.1
0.1

0.3

0.2
0.3

0.9
3C
ng/1
0.6
0.3
0.1

0.7

0.3
0.3

1.9
average
ng/1
0.4
0.2
0.1

0.6

0.3
0.5

1.7
Run 3a
average
Ib/h
2.1 X 10"6
1.1 X 10"6
5.3 X 10"7

3.2 X 10"6
c
1.6 X 10"
2.6 X 10~6

8.9 X 10"6
Average exhaust gas flow rate  1407 dscfm.

-------
                                         CALCULATION OF  VOST MASS  EMISSION RATES
                                                             SARM  I
                                                          CALCULATION OF VOST MASS EMISSION RATES
                                                                        SARM I
 I
CO
SAMPLES NOS.

Compound 10
Acetone

Cholorobenzene
l.2-D1chloro-
ethane
Ethylbenzene
Styrene
Perchloroe-
ethylene
Xylene

1A
ng/l
NO

1.3
ND

10.9
6.2
ND

10.9

IB
ng/l
6.2

0.7
ND

3.8
2.7
ND

4.3

1C
ng/l
11.3

0.4
ND

1.6
1.2
0.11

3.8

average
ng/l
5.8

0.8
	

5.4
3.4
0.04

6.3
Run la
average
Ib/h
3.1 X 10~s

4.2 X 10"


2.9 X 10"5
1.8 X 10"5
2.1 X 10~7

3.3 X 10"5

2A
ng/l
3.8

0.5
0.5

4.9
2.0
0.5

9.6

26
ng/l
3.9

0.1
ND

0.4
1.3
ND

1.9

2C average
ng/l ng/l
3.9

0.3
0.25

Z.7
1.7
0.25

5.8
Run 2a
average
Ib/h
2.1 X 10"5
c
1.6 X 10 "
1.3 X 10'6

1.4 X 10"5
9 X 10'6
1.3 X 10"6

3.1 X 10"5

3A
ng/l
3.3

2.9
0.8

5.9
16.6
1.2

8.8

38
ng/l
5.7

6.8
0.9

8.9
39.6
1.5

9.4

3C
ng/l
6.2

0.3
2.3

19.2
4.7
2.5

27.0

average
ng/l
5.1

3.3
1.3

11.3
20.3
1.7

15.1
Run3a
average
Ib/h
2.7 X 10"b
c
1.7 X 10 s
6.9 X 10'6

6.0 X 10"5
1.1 X 10~4
9.0 X 10"6

8.0 X 10"5
Average exhaust gas flow rate  1412 dscfm.

Ib/h = pg/1 X lO'9 g/ug   Mb   28.317 L
                                                  x  Q x  60 m,n/h

-------
METALS
    A-35

-------
                      tsr,:.
A-36

-------


-------
l.J
I Li
 r
                       r l

                       *r
                       C >
                                       r i
                                       C
                                       l
                                                                                                                                                                                                              oo
                                                                                                                                                                                                              CO
                                                                                                                                                                                                               I

-------
se-v

-------
tl I


H-
         .-i  C-t
          -   o
         h-  -
         Lll  (IJ
              I

              1.
             i D

-------
A-41

-------
111
i->
nj
                                                                                                                                                                                                                                             00
                                                                                                                                                                                                                                             ^1"
                                                                                                                                                                                                                                               I

-------


-------
_
 I
 I
ft!
                                         I  -
                                           I
                                         til

-------
I  4
L"J
I  I
                                   ti       Ii t
                                                                                                                                     ID
                                                                                                                                     3-
                                                                                                                                      I
                                                                                                                                     a:

-------
 I  I
 i  m
' i  rn
 I   4

-------
 err
A-47

-------
 I
4s.
00
                                                                           I  *.-  i n  i  .
                                                                                   I    I   I    I
                                                                                                                                       ri  ti  in  ti

-------

-------
       r

       i'
       r t
r i
"C-
 I
                                                                                                                                                                  O
                                                                                                                                                                  in

-------
A-51

-------
f-

ro
1 1 1
>t> in




; in
Ml
"I "H
i . 1 I III
i m
 1 1
i H
i
' i i
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iii), i
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 1 1 . t MI
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1 1 ii i
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1 i > I .1 ii ! i
t 1 1 | 1 1 1M < M'
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t < 1 I 1 III ' f
t 1 1 . I 1 II Ml III
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tit - i j
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1 1 1 1 1 i ,1 i t . MII
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M TI." ' . ~ < i Tr~
in in i - i h ii  i m m
i -i .n ,n
- ' . + 11 I 0 Itl
11 i i ii . r CD
i  r i  . i HI  
1 . t "| IM >-' t 1
t i ,1 i - , t r
ri i! i . . TI 4.,
Ml i|| < >
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i i in - . 
i|i "t 1 1 - M
111 
: : : :
, . r i * M- -
 1 1 i i ( n ii
                                                                                                                                                                         1 r^i
                                                                                                                                                                         M i._ i .
                                                                                                                                                                           -H I i
                                                                                                                                                                            ~*

-------
es-v

-------
Supie Voluae,  dscf
Volumetric Flow,  dscfm



Metals
ARSENIC
CADMIUM
C3PPER
NIC'IL
ZINC





Metals
CHROMIUM
LE-I
ZIN;

uq Fer
r,
5AI-M-1 SA
40"
4250"
167"
450"
1740"
750"
940 "'



ug Fe^
Ru
Mim-1 *:
14""
3000^
78 x
23u""
920'"
411 '

Sample
ans
I-M-2 SAI-M-3
45 x 27"
2730"" 6090"
530 x 710X'
1070" 2520 '
100X 89X
602'x 1150 '



Sample
ns
T -M-*" nA* T_M_^
13" 21X
44^ '-.'
.,/ o- X
810 ^ 750 x
280 x 150 x
73. 183 ^8. 341 82.863
Concentration, ug
-------
   APPENDIX B



FIELD DATA SHEETS
     B-l

-------
PROCESS FIELD DATA SHEETS
          B-2

-------
                                                                                                c
, EST NO. :
DATE:
TIME BEGIN WASTE FEED:
TIME BEGIN TESTING:
                         .,<-
                                        SARM TEST BURN
                                JOHN ZINK ROTARY KILN INCINERATOR
                             TEST CONDITIONS:
                                    Rue Gas Oxygen
                                    Slowdown Rate
                                    Venturi Scrubber
^3~5
0
.?/^
%
gpm
m.WG
Feed Rate
Incinerator Temp.
/OOP Ib/hr
/ fr Of"* ^i A
3OD& z><- -
  PARAMETER
                                                   TIME
                      <)
                         **
                              to
                                 *
                                     /o
                                            ,/  5^
KILN
  Temperature, F

  Combustion Air, inches WC
                      ttef
                                      /r
                                             /. r
                                                    /. r
                                                                  /.S
A
  <~soi  j  f rj
  feed nate Indicator. lb
KILN AFTERBURNER
  Temperature, F

  Combustion Air, inches W6

  Continuous Oxygen, %

  Continuous CO, ppm


SCRUBBER
  Scrubber flow, % max.
                                                                            '5
                                                                                         J
                                                           my
                                                                                   7797
                                                             . -7
                                                                   t-7
                        ^
                              72-
  Slowdown, % max.

  A P Venturi, in. WG
STACK (W,,..-  ,o^
  Oxygen, %
                                      c?
                                               o
                                                      o
                                                                    O
                                                                                   O
                              J/.C
                                                                   37.
                                                            -r
NOTES:
                                    
-------
                                                                                                    c
                                                                                                   C
                                         SARM TEST BURN
                                 JOHN ZINK ROTARY KILN INCINERATOR

TEST NO. :  SftjiH -J~- J.     TEST CONDITIONS:
DATE:      y/xfr/d 7 '               FJue Gas Oxygen   vJ-5" %
                                     Slowdown Rate       n
                                     Venturi Scrubber    ,3
           y/xfr/d 7
TIME BEGIN WASTEFEED:
TIME BEGIN TESTING:
                    "y
                                                                    Feed Rate       / OOP Ib/hr
                                                                    Incinerator Temp.
  s
                                                            in. WG
                                                           J.ooo V  5trcc/-O4/?<7
   PARAMETER
                                                    TIME
KILN
  Temperature, F

  Combustion Air, inches WG
KILN AFTERBURNER
   Temperature, F

   Combustion Air, inches WG

   Continuous Oxygen, %

   Continuous CO, ppm

   Continuous C02, %
SCRUBBER
   Scrubber flow, % max.
AS"
                               /,JL
4
                                                     /.-L
/.r
                                                     3  (e
                                              5.3
                              2003-
                                                       "- 3
          0
   Slowdown, % max.

   A P Venturi, in. WG
STACK
   Oxygen, %
   CC ATV-w
  0
                                 o
                                                        o
                                                                              0
 1.1
                                      ^ /o
                                      //.i
                                                                     /P. 7
                                                               vV
                                                                              7o
NOTES:
                                                                         V^
                                                                         v^
           -- /O
       30
                                             <**>
                                                   7'*
                                                   7^
            -J.
                                                                           So
                                                                          o "7
                                                                                                   '

-------
    -- /Coo
  .ST NO. :
TIME BEGIN WASTE FEED:
TIME BEGIN TESTING:
                       3

                       / Q
                           . .
                           *
                                         SARM TEST BURN
                                 JOHN Z1NK ROTARY KILN INCINERATOR
TEST CONDITIONS:
        Rue Gas Oxygen
        Slowdown Rate
        Venturi Scrubber

   // J'J- 3 A, /*x -ewa^
3 -5"
0
3G
%
gpm
in.WG
Feed Rate
Incinerator Temp.
yooo
/ffoo
2ooo
Ib/hr
F k
"i- '
                                                        '  "
   PARAMETER
                                                     TIME
                       012
KILN
   Temperature,
I   Combustion Air, inches W6

.   rcoi5 Bate Indicator, ll>
I KILN AFTERBURNER
   Temperature, F

I   Combustion Air, inches WG

1   Continuous Oxygen, %

I   Continuous CO, ppm

   ContionuousC02,%
[SCRUBBER
   Scrubber flow, % max.
I   (U v(o<^f>r
   Slowdown, % max.

 .  A P Venturi, in. WG
.STACK
   Oxygen, %
                               /776
                                                                     A")
                                7-3
                                                         o
                                       3.1*
       .
   Gombugtibloc. % Co-,
                                                 /o
                                                       /r
                                                                                             76.
                                                                                             -73.?
                                                                                             U.I
                                                                                                . -L
 NOTES:
                 Full

    /M
      Z-Jo
                  t / o
                                    575"
                                                                          30

                                                                          3o
       r -a
         - 7
                                                              *
                   t-Uo
                                                                          Si
                                                                                         "799
                                                                                        n

-------
                    C/>/">
                                                                   Feed Rate
                                                                   Incinerator Temp.
nso
;?vi
  PARAMETER
                                                    TiMT
                                        oo


  Temperature, F

  Combustion Air, inches WC
                       /.
  AJ
          Indicator, Ib
KILN AFTERBURNER
  Temperature, F

  Combustion Air, inches WC

  Continuous Oxygen, %

  Continuous CO, ppm

  Continuous C02, %
SCRUBBER
  Scrubber flow, % max.
                               3  2.
                                      .2.0
                                                                                        -
                       J. 0
                                              /. 6
                                                                     r, o
                                                       V.
  Bbwdown, % max.

  A P Venturi, in. WG
STACK
  Oxygen, %
  C o,
                      7V?
                               70
                                                       7 JL
                                               O
                                                o
                                                                                     O
                                      I")
                        6*0
                        (/ 3
                               C/o
         
-------
                                                        c_

                                                                                           / 76
           30
    NO. :
JATE:        ^ - , a - e ->
TIME BEGIN WASTE FEED:    *f :
TIME BEGIN TESTING:       ^
                                         SARM TEST BURN
                                 JOHN ZINK ROTARY KILN INCINERATOR
        TEST CONDITIONS:
               Rue Gas Oxygen    3 - <-  %      Feed Rate        / Co o   Ib/hr
    Do xa^    Slowdown Rate     Q    gpm     Incinerator Temp.   /ce>_0F/,c,
       -        Venturi Scrubber    3^   in.WG                  JOG-   c  *-
   PARAMETER
                                                    TIME
                                                                              OO
KILN
  Temperature, F

  Combustion Air, inches WC
    O> --/ ,"
  Feed Rate4fl*eetef^ib
KILN AFTERBURNER
  Temperature, F

  Combustion Air, inches WC

  Continuous Oxygen, %

  Continuous CO, ppm

  Continuous  C02, %
oCRUBBER
  Scrubber flow, % max.

  Slowdown, % max.

  A ? Venturi,  in. WG
STACK
  Oxygen, %
                                              a.
  <' v
                                                              3.3
  00"?
                                      3:1
                              3.0
                                       V'-V-
7o
           o
 n
        G,
5.JL
c.o
 -Combustotes, %
         '7.1
                                                                                   /0-Y
                                                                           Itf

NOTES:
     7- /L-  4
                      5-7 /
                      7/?
                                                          f.'oo
                                                               *^
        /'.r/;
         u/
         to
                                                             /V
                                                                                  */
            sr*fec,  i')*'//,
                      '* /P    ^fp*^
                                                       B-7
                                                                      /
                                                                      1?
                                                                                               rrzr
                                                                                                /1 /'
                                                                                                   j

-------
TEST NO.:  SAKH-ff-t
DATE:       t.-/-r>
TIME BEGIN WASTE FEi
TIME BEGIN TESTING:
           SARM TEST BURN
   JOHN ZJNK ROTARY KUJUNCINERATOR

TEST CONDITIONS:
       FJueGasOxygen    J-5"  %
       Slowdown Rate    _o___gpm
           iri Scrubber
                                                                  Feed Rate        /coo  Ib/hr
                                                                  Incinerator Temp.   jfro^ CF  /f, /.
   PARAMETER
KILN
  Temperature, F

  Combustion Air, inches WC
                                            nirt
  FuuJ Ble iHdmiur. Ib
KILN AFTERBURNER
  Temperature, F

  Combustion Air, inches WC

  Continuous Oxygen, %

  Continuous CO, ppm

  ContionuousC02,%
SCRUBBER
  Scrubber flow, % max.

  Slowdown, % max.

  A P Venturi, in. WG
STACK
  Oxygen, %
   CO ffrr-
  Combu jlibtofc. %
                         0
                              3.JL
        .3."?
3-3
                                     3. /
                       3 6
                      5.0
                                             41

                              (p.?
                               52
                                                    7o
                                                      70
                         0
   0
        O
                                       O
                                                                          71*
                                      tO.ic
                                                     /A/
NOTES:
       - n ~
                                            U'&
      ir-7
      G-n
     'L -
     TL- /3/3


    -r/:
    TT - 7
                                                           /
                                                            V*
                    tc J V
                               (fit
                                        rrr
                                                     a./

                                        ^<^       3/
                                                       B-8

-------
 ^ST NO.:
DATE:      9
TIME BEGIN W7
TIME BEGIN TESTING:
                                           SARM TEST BURN
                                  JOHN ZINK ROTARY KILN INCINERATOR
                               TEST CONDITIONS:
                                       Rue Gas Oxygen
                                       Slowdown Rate
                                       Venturi Scrubber

O
%
gpm
Feed Rate
Incinerator Temp.
in.WG J&i,,*.*,, /,
Ib/hr
PARAMETER
KILN
Temperature, F
Combustion Air, inches WC
KILN AFTERBURNER
Temperature, F
Combustion Air, inches WC
Continuous Oxygen, %
Continuous CO, ppm
, ContionuousC02,%
1 SCRUBBER
Scrubber flow, % max.
Slowdown, % max.
A P Venturi, in. WG
STACK
Oxygen, %
Combustibles, %
TIME
'/V
hfa
tfV
v\
w/
-W
'^
\
\ x
\
V
r-\
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\ '
\































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NU I ha:
                Its
                                                    B-9

-------
STACK TEST FIELD DATA SHEETS
            B-10

-------
                   TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
 Plant
 Date 	
          "7   7
 Sampling location
 Inside of far wall  to outside
  of nipple          '-''
 Inside of near wall  to outside of
,  nipple (nipple  length)
 Stack I.D.
 Nearest upstream disturbance
 Nearest downstream disturbance
 Calculated by
                                                          SCHEMATIC OF SAMPLING LOCATION
TMVEIBE
ftXHT
UMCT
f
5L
a
9








FMCTION
or STACK t.o.
0>7
0.ZL*
4>.7f
6.
u








TRAVUBC rOMT LOCATION
PROM OUTSAE OF NIPPLE
(SUM OF COLUMNS 4 I S)
//fc"
/^>/i"
M.
-------
                       GAS VELOCITY AND VOLUMETRIC FLOW  RATE
Plant and  City
Sampling Location
Run No.
                                                             Date
                                                             Clock Time
                                             Operator
Barometric Pressure,  in.Hg   Jgy. 15*       Static Pressure, in.hLO
Moisture,  %	Molecular wt., Dry	 Pitot Tube,  Cp
Stack  Dimension,  in.   Diameter  or Side 1      II "      Side 2
                 flELD DAU
  POJKT
  -
   T~
                   H[AO
                                   STAC
                                 Ttur.. *
                               /SLO
                                                                 CALCULATIONS
                                                               H,0 ,
                                                             1B '-TOT'
                                                                    loir
                                                                         -)  is <-
                                                                       R  CF  460)
                                                     rrt 
                                                          in.H;
                                              $  85.49  Cp
                                                  85.49
                                                         ft/s

                                                         ft'

                                                         _$
                                                          m

                                                            x

                                                         cfm
                                                                        60
                                                                    H-C '
                                               'ltd
                                                ltd
                                                            17.647 
                                                           dicfm
                                          B-12

-------
                       FIELD AUDIT REPORT:  DRY GAS METER
                               BY CRITICAL ORIFICE
DATE:
                                         CLIENT:
BAROMETRIC PRESSURE (Pbar): ?.%> 1n.Hg   METER  BOX  NO.
ORIFICE NO.     7                        PRETEST  Y:   ,
                                         AUDITOR:
ORIFICE K FACTOR:
                                                               AH@  /, 8?  in.H20
- - ^ 	
Orifice
manometer
reading
AH,
in.H20
w
Dry gas
meter
reading
ft3
/feT7
*//./
Temperatures
Ambient
Tai/Taf>
F
W
if
Average
V
*f
Dry gas meter
Inlet
F
SO*L
fa
Outlet
F
/'*
37
Average
Tm
F
/ffV
Duration
of
run
0
min.
'"%
Dry gas
meter
Vm ft3
/^:y
vm
mstd'
ft3
/V.3**-
v_
mact
ft3
/3.*ti.

Audit,
Y
,f^7
Y
devia-
tion, %
,.+ '
Audit
AH?,
in.H20
/.9HL.

AH(? Devia-
tion, in.H20
^-^,'-^_ ^
 m
  std
            17.647(Vm)(Pbflr + AH/13.6)
                  (T
                    m
                                                  ft3
 m
  act
            1E03( 0 )( K )(Pbar)
               (T  * 460)
                         172
                                                  ft3
Audit Y
             m
              'act
                              Y  deviation
             "std
Audit Y - Pretest Y
     Pretest  Y
x 100
Audit AH? * (0.0317)(AH)(Pbar)(Tm * 460)
Audit Y must be in the range, pretest  Y 0.05 Y.
Audit AH? must be in the range  pretest AH@ 0.15 inches H-0.
                                                                           in.HoC
                                   B-13

-------
                       FIELD AUDIT REPORT:   DRY  GAS METER
                               BY  CRITICAL  ORIFICE
DATE:
                                         CLIENT:
BAROMETRIC PRESSURE (Pfa  );^f.5g in.Hg  METER BOX  NO.

ORIFICE NO.     JL                      PRETEST Y;   .
                                                              AHP /
-------
                THERMOCOUPLE DIGITAL INDICATOR

                        AUDIT DATA  SHEET
Date
Indicator No.
Operator
(SL
Test Point
No.
sr*ji.
1
2
3
4
Millivolt
signal*




Equivalent
temperature,
op*
/<&
ji
Digital Indicator
temperature reading,
F
7?
/??
*-4f
39S
Difference,
%
?.*&> ^
0.1? "
0J'b- ^
0,-iX ^
Percent difference must be less  than or equal to 0.5%.

Percent difference:

  (Equivalent temperature eR- Digital indicator temperature reading eR)(100%)
                             (Equivalent temperature  R)
Where R -  F + 460F
  These  values are to be obtained from the calibration data sheet for the
  calibration jdevlce.
                              B-15

-------
 0PARTICULATE



SEMI-VOLATILES



    METALS
    B-16

-------
ss* S  R  is

-------
73 >.
        Plant   ^
                       PARTICULATE SAMPLE RECOVERY AND INTEGRITY SHEET
                                        Sample  date
Sample location
Run No.
                           - /
    Recovery date
    Recovered by
        Filter No(s). 	
        XAD-2 sorbent trap No.
Final volume wt.
Initial volume wt.
Net volume wt.
Description of
 impinger contents
                                 1st
                               impinger
                                  MOISTURE
                                    2nd
                                  impinger
            3rd
          impinger
                                          5W.6 9
                                          	 9
                                      Total moisture
                                      RECOVERED SAMPLE
   4th
impinger
                           9
                           9
                           9
Filter container number(s) _
Description of particulate on filter 
                                                            Sealed
Silica gel

         9
         9
         9
                                                                              % spent
       .  Probe  rinse
             Container No.
       .  Back rinse
             Container No.
                                               Blank Container No.

                                               Blank Container No.
         Condensate  Container No.
         Impinger Contents            A
              Container No.
 Liquid Levels marked
 Remarks
   j/*.ott
                                               Blank Container No.
                                   j/
Samples stored and locked
         Received by
         Remarks
                                      LABORATORY  CUSTODY
                                                  Date
                                             B-18

-------
                   TEb-uNC
                                                                          LD
                            *.*! i cm
s
        EE
iSTftiJi
          ).u..|..|..|..|..|?H..h..g
                    '
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                         Mil
                                _
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                                                UMTIIM. lOUIIIM
                                                                                     Qiti(i4d\  1 1  MI i M
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                                                                                                                    I I  I I I i I  I
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                             OTIMIOI
           1INP   Mlii.
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                                                                                  .....
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                                                                                               ^4 1111 i  A  i
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    iiin.     .o. luurulMiu |  mm
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                                                                    Mill Ui
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                                                                               IU CMC
                                                                             IH. ml  cm
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                                                                                                                MUI UI
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                                                                                                                       MUI Ml
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                                                                                          f
II COM
 MIA
 Mlrt

-------
                         LEAD SAMPLE RECOVERY AND INTEGRITY  SHEET
tit
Plant _/ oAv ^>/c/A ^ ,  7^
Sample location X>o^*vc ><^
Run number &A-Sf  /
u^Sa_
r7*r~
Sample date 7/ M/Sf/
Recovery date i/Jlr/jf')
'i\0 / /
Recovered by ^r '
Filter number(s) *&? ( & 2-z-~i
Impingers
Final volume (wt)
Initial volume (wt)/"&?.7'^%.f
\j -^
Net volume (wt)
Description of impinger water

Total moi
MOISTURE
Ug)
^f(g)
ml (g)


sture
Silica gel **
Final wt /J'^i^g
Initial wt ^31*1 ,_3/tf5D.3- g
Net wt / y^ 0 g
% spent
J^#r^ 5:/.^^,
        Filter container number(s)
RECOVERED SAMPLED
        -&  Sealed
Description of particulate
Acetone probe
rinse container no. /
Acetone blank
container no. /I
0.1 N HNOs probe
rinse container no. fe?
Impinger contents /ft
container no. Cr?^.
0.1 N HNOs blank
container no. 7
Samples stored and locked
Remarks /? Lief. DA*t :
on filter - fLtT L+hi^ -~

,~ Liquid level
v# marked A/*
Liquid level
'# marked /t//?
^ Liquid level
**i'~r\ marked
WftlfOjft Liquid level
r*f-n marked
. Liquid level /
'& -A marked r

-&&7&-&




I/
v/




Received by
LABORATORY CUSTODY
Date

Remarks
                                             B-20

-------
                                                     EMISSION  TESTING       LD
                                      4 (ill
         i|i|||(l'l|l4|n|lt|>||l|'||I |4]4lJ4|ji|M|j;|l>|vh%|>J))ilIJKljn|j|nj4J
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                                                                                                                                             im
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                                                                             mm CM.
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                                                                                                                              xl

                                                                                           /^.

-------
Plant
Sample location
Run No.        
               PARTICULATE SAMPLE RECOVERY  AND  INTEGRITY SHEET
                                       Sample date
                                       Recovery date
                                       Recovered by
Filter No(s). 	
XAD-2 sorbent trap No.
                             4V
                                 MOISTURE
                        1st        2nd        3rd        4th
                      impinger   impinger   impinger   impinger
Final  volume wt.
Initial  volume wt.
Net volume wt.
Description of
 impinger contents
                     ?**
                                        9
                                        9
                                        9
                                                  9
                                                  9
                                                  9
9
9
9
                             Total moisture
Filter container number(s) _
Description  of particulate on filter
                             RECOVERED SAMPLE
                                       '/
                                                  Sealed
                                           Al
                                                                 Silica  gel
                                                                 	% spent
Probe rinse         tsr*G' r\
     Container  No.   60 "O "HT
Back rinse
     Container  No.
Condensate Container No.
                            L   JO
Impinger  Contents
     Container No.
                     an
Liquid Levels marked
Remarks
                          t/
                                              Blank Container No.
                                              Blank  Container No.
                                       / &6
                                              Blank Container No.
                                                                        ft
                                  Samples stored  and  locked
                                                                   \S
                                       C*tOPY
                                                 Ottt
                                  B-22

-------
  i 4
i-i
Q
*K
         I 
      at

         si
      HE
       a
       3
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       i
       s
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         i
      i
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             i
            55

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               VI
                ( oJ
               -sj
              ?y
                III!
                 a/
                JU
            *^
              B-23
                      -
  r
 > j
CAS NCTC

NPLATUk
                         a*
                      sS";
                     L.
>j*

     Ue

-------
                         LEAD SAMPLE  RECOVERY AND  INTEGRITY SHEET
/Y57
Plant ^^vt
Sample location ^/ev^
Run number SA^-M-^-
Filter number(s) Y 7/0/3
Impingers
Final volume fwt) /T^5>
Initial volume (ut)f&rj<6#
Net volume (wt) / 2^4
Description of impinger wate
Total
Sample date
>cs-7~/e.7~ Recovery date
Recovered by X&
12,
MOISTURE
Silica gel
ml (g) Final wt i
ft P^nil" (g) Initial wt
ml (g) Net wt
r I$\J

moisture i^/^'7. 0 g
7//fysrx
f/fifa
1 /


**24>X g
Dl'LQ g
% spent

       Filter container number(s)

       Description of particulate on filter
                             RECOVERED SAMPLE

                                  2	Sealed
       Acetone probe
       rinse container no. 	

       Acetone blank
       container no.       	

       0.1 N HH03 probe
       rinse container no. 	
       Impinger contents
       container no.       	

       0.1 N HN03 blank
       container no.       	
       Samples  stored and  locked

       Remarks
                                     Liquid level
                                     marked

                                     Liquid level
                                     marked

                                     Liquid level
                                     marked

                                     Liquid level
                                     marked

                                     Liquid level
                                     marked
/
                                     LABORATORY  CUSTODY
Received by

Remarks
                                                           Date
                                           B-24

-------

-------
               PARTICULATE  SAMPLE  RECOVERY  AND  INTEGRITY  SHEET

Plant ~T7 t^/TVXL *>
Sample location ?*CT7&
Run No. 5/tt "5*//-
Filter No(s). b ~"? 0 0 ^^r
XAD-2 sorbent trap No. 5^^>
Sample date V////f /
~^^ Recovery date ,3 g
V3.J? g
% spent
/


  Probe rinse
       Container No.  _

  Back rinse
 If    Container No.  	
,V^
  Condensate Container No.
Impinger Contents
     Container No.
                           jfc"
                                               Blank Container No.
                                          /
                                          t-/u-.Blank Container No.
                                       / MM

                                               Blank Container No.
Liquid Levels marked

Remarks
                                   Samples stored and locked
Received by

Remarks
                             LABORATORY CUSTODY
                                                  Date
                                    B-26

-------

-------
Plant
                  LEAD SAMPLE RECOVERY AND INTEGRITY SHEET
                                            Sample date

Sample location

Run number
                      0 K-T/e J"
Recovery date  f//?/.?7
                                      Recovered by
5" oo
^/^
*'
y/s,
^0
Filter number(s) 0 /j^l/J)
' MOISTURE
Impingers Silica gel
Final volume (wt) ml (g) Final wt
Initial volume (wt) 5~7~7 00oltl ml (g) Initial wt 5"-
Net volume (wt) /5'J^ ml (q) Net wt
Description of impinger water
fflb <>!*<
Total moisture /J&0 [^(a'*/ g>

g
a^ 7?y,^ q
uS^1 g
/^^;% spent
-
                                      marked         \S
                                      Liquid level    *
                                      marked
                                      ^Liquid level
                                      marked
                             LABORATORY CUSTODY
Received by

Remarks
                                                    Date
                                      B-28

-------

-------
               PARTICULATE SAMPLE RECOVERY AND  INTEGRITY SHEET
 Plant
                                      Sample date
                                                       it'll
A
'W
f,} f
"l&o
'^
~x*
w
Samole location Ou*r/f*T~ Recovery date ^J ll'+ ti If)
Run No. j/\2t- tff~~ / Recovered by J5^
Filter No(s). ^75^6 ^ 6
XAD-2 sorbent trap No. JAM* J"/-/
MOISTURE
1st 2nd 3rd 4th
impinger impinger impinger impinger Silica gel
Final volume wt. 9999 D 7> - cr-Q
Initial volume wt. q g 9 9 fbl  ^-9
Net volume wt. 9999 ^J / 0 9
Description of
impinqer contents k %-sent
Total moisture A T*7^ 9 (^^i~/(t^^~
RECOVERED SAMPLE " ^/i>^ ^
Filter container number(s) & DC? 1 D Sealed
Description of particulate on filter

                                                                               i
                                                                                ,y
 Probe rinse          . -~   *
      Container No.    fe>6bv /T
 Back rinse
:/     ContaHitr No.
Condensate
                                                    Container No.    1/75/#
                                             Blank  Container No.    757*9
                    Ho.
                                         / &$?$
                                                     Container No.
Liquid Levtlf

Remarks
                            /      Samples stored and locked

  Received by

  Remarks
                              LABORATORY  CUSTODY
                                                 Date
                                     B-30

-------
                                            F.....-SJC..  -'ES
                                                                                                                                 UMTli MM         I
                                                                                                                         II|MH>|II|>I|M|'|>\||>I|)I|M[M|
                                                                                                                            ^F^^ l  I  I  I t III
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                                                                                 rtnu
                                                          3.7J ^-y?
] il il * I1*11| 11 M|.i|.iM|.*|it|
  *J t S~ f    ^	 .

-------
Plant
LEAD SAMPLE RECOVERY AND INTEGRITY SHEET



                      Sample date
ilnli?
Sample location Ou,^* @LMtf Recoverv date tfl/lf/f/
XOO
^t?
0-^
" X
#* ,
^V-
v><
XM i'
"^ /
Run number 5/Ol M " 1
Filter number (s) Q' J)(J\
Impingers
Final volume (wt)
^trl Recovered by J)^/-J
ioU '
MOISTURE
Silica gel
ml (g) Final wt "6^^
Initial volume (wt) Stftf &9tf7 ml (g) Initial wt^BS^f
Net volume (wt)
Description of impinger water
ml (g) Net wt ^^K


'W


Je&ft g
T~0, <} g
% spent

Total moisture / 7 9/t+* g
/
Filter container number(s)
Description of particulate on
Acetone probe
rinse container no.
Acetone blank
container no.
0.1 N HNOs probe
rinse container no. tsO/^
Impinger contents^,* //  x
container no. 1$ ' *** )5
0.1 N HNOs blank _ ,
container no. t-"~"~
Samples stored and locked
Remarks

Received by
Remarks
RECOVERED SAMPLE
L&M8 Sealed (/
filter T^J

Liquid level
marked
Liquid level
marked
^ Liquid level /
1 /r marked \/
- >, Liquid level /
H marked ^/ ^
f
^ Liquid level ' ^
VH ma/ked ^^
/


LABORATORY CUSTODY
Date














                                   B-32

-------






















1





















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-------
Plant
                PARTICULATE SAMPLE RECOVERY AND INTEGRITY  SHEET
                                         Sample date _   1
  Sample  location
  Run  NO.      5>4 nz:
Filter No(s).	
XAD-2 sorbent  trap No.
                         0 SI
                                       Recovery date
                                       Recovered by
                                   MOISTURE
  Final  volume  wt.
  Initial  volume  wt.
  Net volume wt.
  Description of
   impinger contents
L
1st

impinger



g
9
9
2nd

impinger



9
9
9
3rd

impinger



g
9
9
4th

impinger



g
g
g

Silica
57,
fryZ,
1 4

gel
^9
Q
< g


W-
fef*
l~L


S
%
t
7
/
                               Total moisture
                                RECOVERED SAMPLE
                                                23)3.1
 Filter container number(s)    j. if /
 Description of particulate on filter
                                                     Sealed
                                                                     % spent
 Probe rinse
     Container No.
 Back rinse
,     Container No.
 Condensate Container No.
   Inpinger Contents
       Container No.
  Liquid Levels marked
  Remarks
                                *
                                '\
                                            tfa. Blank Container No.
                                   A  /  
 Blank  Container No.
A/
                                               Blank Container No.
                       (:
                                   Samples stored and locked
   Received by
   Remarks
                               LABORATORY CUSTODY
                                                  Date
                                      B-34

-------

-------
LEAD SAMPLE RECOVERY AND INTEGRITY SHEET ,
/^ / /y i I f ^f
-^^& t s V i i * 1 1 ^y
Plant '^'JfJf- Sample date i Ifo/i *
Sample location ^^4^^^
Run number ^/^ J*~ W
Filter number(s) 0? 1 &
Impingers
Final volume (wt)
Initial volume (wt)
Net volume (wt)
Description of impinger wate
Total
r^f^rt*/-^"" Recovery date //
 y Recovered by J)^^
-L5T-
MOISTURE
Silica gel
ml (g) Final wt
ml (g) Initial wt
ml (g) Net wt
T

moisture //v iff1 ' g

/

.? 7^ ' g
cr^x^>g
^3,1- g
% spent

Filter container number(s)
RECOVERED SAMPLE
              Sealed
Description of particulate
Acetone probe
rinse container no.
Acetone blank
container no.
0.1 N HN03 probe ,<
rinse container no. *->? .
Impinger contents,, >K^
container no. $$!/ ^ J '.
0.1 N HN03 blank
container no. t- &
Samples stored and locked
Remarks
on filter //f/^

Liquid level
marked
Liquid level
marked
, , Liquid level
~h rV marked
., Liquid level
^ M marked
Liquid level
90> f\ marked
y





L/
/
//



Received by
Remarks
LABORATORY CUSTODY

Date

          B-36

-------
API)

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     r
     D
*.

-------
:?
          Plant
                         PARTICULATE SAMPLE RECOVERY AND INTEGRITY SHEET
                                                Sample date
          Sample location
          Run No.
                                                Recovery date
                                                Recovered by
          Filter No(s).	
          XAD-2 sorbent trap No.
                                            MOISTURE
        Final volume wt.
        Initial volume wt.
'00     Net volume wt.
') 0     Description of
00      impinger contents
1st 2nd 3rd 4th
impinger impinger impinger impinger Silica gel
g g g g ^c'-"j g
g
g
g
g
g
g
g &
g
3P/.1 g
g
                                        Total moisture
                                        RECOVERED SAMPLE
           Filter container number(s)	
           Description of particulate on filter
                                                                                % spent
         Probe rinse
             Container No.
         Back rinse
          ;  Container No.
                                    A.
                                /'
                                b 3
         Impinger  Contents
              Container No.
           Liquid  Levels marked
           Remarks
Condensate Container No.  L%*$ f^

                           TV
                                            ^-Blank  Container  No.

                                             ,  Blank  Container  No.
1 7 V fr
                                                         Blank Container No.
                                           Samples stored and locked
           Received by
           Remarks
                                        LABORATORY  CUSTODY
                                                          Date
                                              B-38

-------
III  I  I  I  I \  I  1  1  I "1

-------
                         LEAD SAMPLE RECOVERY AND INTEGRITY SHEET
 4>9
^_ L'
u/,
Plant -zT, /o/C..
Sample location (.^
Run number 5~/^ J
Filter number(s)
Impingers
Final volume (wt)
Initial volume (wt)
Net volume (wt)
Description of impinger


'(s\^': f ~~"
Sample date
Recovery date
i / /t/ IK /
1/)t/f7
Z" M^Jj Recovered by  *

,
fr/t & g
Aft ^^ g
^^X^ % spent
pr*j ^T) )Q/0.^ ((
Filter container number(s) 	
Description of particulate on filter _
                                     RECOVERED  SAMPLE

                                     X  V ^  P>     Sealed
       Acetone  probe
       rinse container no.

       Acetone  blank
       container no.

       0.1 N HN03  probe
       rinse container no.
       Impinger contents
       container no.

       0.1 N HNOs  blank
       container no.
        Samples  stored  and  locked
        Remarks
                                      Liquid level
                                      marked

                                      Liquid level
                                      marked

                                      Liquid level
                                      marked

                                      Liquid level
                                      marked

                                      Liquid level
                                      marked
                                     LABORATORY CUSTODY
Received by
Remarks
                                                           Date
                                               B-40

-------
VOLATILES
  B-41

-------
                                                  VOST
                                                          SAMPLING DATA
                                            Sampling Tran No.
Date
Test Condition

Trap Nos.
                                                                   Run No.
                                                                                              Operator
                                        Meter  Console No.
                                                                                                 Y-Factor
      Barometric PressureuPT)
                                                  Pretest Leak Check  O^Q   in.Hg/min at  /     on  Ice?       i/  Culture Tubes and Can Purged With Ng?
     Conments:
     Probe Leak  Check Data:
                             0.0
     Corresponding  Blank Nos.
    std
             liters x Y x 17'647
                                         m1
                                                                             i \

-------
                                                  VOST
Date
                Location  J&M/ %;/{ :
                                                               SAMPLING DATA
                                                               .         Run No.
                                                                                  ~ /6U
                                                                                              Operator
Test Condition
Trap Nos.
                                        Sampling Train No.   f/- 2-     Meter Console No.
                               From Can No.
                                                    Pretest  Leak  Check
                                                                                  in.Hg/min at
                                                                                                       Y-Factor
                                                                                                       in.Hg vacuum
Barometric Pressure HP.) 2,%.-l in.Hg Ambient Temperature 7S f Probe Purged /ZL minutes a
L_D__
Sampling
time,
min.
0
/&
2-0
3>;>
f^-f
Clock
time
(24-h)
:2t-
'O'JZ-
wpz-
/0. '2-
//.oz.
Vm
Keter
volume
reading,
liter
 t2$
7./7
&&$
pSs.?
%.2j&O
L-$fc$
Rota-
meter
setting
.<$/
-2^
34
3 * ^
~^/
Sampling
train
vacuum,
in.Hg
2. 0
2,0
2..O
Z-.O
/ Avg.
Dry
gas meter
tempera-
ture, F
96
ff)9^
/Q^
/>  ' ^7
cT '*?
,__
&*y
j
Probe
tempera-
ture, F
27 /
2.6>5
/
ZL7&







t /. 6> liters/min







03
-p.
CO
'   Post-Test Leak Check
                       &.Q
                                      in.Hg/min at
    Flow Direction Marked?
                                  Condensate  Recovered?
                                                    , ^>  in.Hg Vacuum    Trap Pair Label  No.
                                                          	    VGA Label Nos.
   Total Volume of Condensate in Vials, -"
   Traps and Vial Stored in Can No.      /
                                               ml Remaining Condensate        mls Total Condensate Vol.
                                               on Ice?      t/^  Culture Tubes and Can Purged With N2?
                                                                                                                ml
   CoflNents:
   Probe Leak Check Data:
                         O.o  " ^
                        	^JL.
   Corresponding Blank Nos.
1)  Vstd = Vm, liters x Y x 17.647  x

                                                             liters  /

-------
                                             VOST
                                                                SAMPLING DATA
Date
Location
Test Condition
Trap Nos. 	
                                             V-
                                                                    Run No.
                                                                                  - V~
                                                                                              Operator
                       Sampling Train No.
                                                                          Meter Console No.
                                From Can No.
                                                             Mi
                                                                                                    Factor
                                                   Pretest Leak Check   > D   in.Hg/min at  /4.&     in.Hg vacuum
Barometric Pressure (P. ) ;
Sampling
time,
min.
0
/O
2-0
-^Q
JLf/ / / I
^r^^^^ L/
Clock
time
(24-h)
//;zs
// -$

/J3,%$
^L-'^^f
l.J_5 in.Hg

Rota-
meter
setting
-"5' *~J
^mr r
^^ *^
3^
55
Ambient Temperature /f F Probe Purged ^,0 minutes at /, O liters/min

Sampling
train
vacuum,
in.Hg
2.0
z.o
&.O
^O
/ Avg.
Dry
gas meter
tempera-
ture, F
'//^
/ / ^""'
/ / ^j
/%/
/z
UZ*
Primary
condens-
er exit
temp., F
/ /
c $ /
^^,
f? J
fr2/
L^^ $
/
Probe
tempera-
ture, F
*9 ff /
jfLr Q /
^^P7
-2-^5"
?-tf<^
<7J














CD
I
Post-Test Leak Check
                          Q
    Flow Direction Marked?
in.Hg/min at
Condensate Recovered?
                                         in.Hg Vacuum    Trap  Pair Label No.   ($/\Z~V~
                                          --  VGA Label Nos.     *~
    Total Volume of Condensate in Vials,
    Traps and Vial Stored in Can No.
    Comments:
                                           ml  Remaining Condensate     mis Total Condensate Vol.
                                           on  Ice?
                                                      3 Conoje
                                                                                               ml
                                                              Culture  Tubes and Can Purged With N2?
    Probe Leak  Check Data:
                             0.0
    Corresponding  Blank  Nos.
    1) Vst(J = Vm,  liters  x  Y  x  17.647  x



-------
A//
vr
/v>
VOST SAMPLING DATA
^^ry Location C/J^k'/l xS^/^/^ ," ,X^
2V

Jb
Clock
time
(24-h)
/5.3?
/j;/Z-
/7:2
/5//^
y ^7 * ^ **^
X *J ^fc'^^--
\
t* Post-Test Leak C
en
Flow Direction M
Total Volume of 1
Traps and Vial S
Keter
volume
reading,
liter
/A-l^l
/*?,03
Z^ZZ
^O.CxJ
3^&t>
^/J^
Sampling
Rota- train
meter vacuum,
setting In.Hg
<3 $t
3^' 5^ 5
3^ s ^
,5V 5; ^
/ Avg-
Dry
gas meter
tempera-
ture. F
/^5"
/.2-
/^>3
/3^
/L3.QL'&>
Primary
condens-
er exit
temp., F
/ 6J>
o
^t-^. C-i* X
^"7 *f r
2-V&

Trap Pair







^5, O in.Hg vacuum
t /. ^ liters/min







Label No. S'AJ- V^^
^"^ VGA Label Nos. SAT'V-f <2&/Uj>AfS#rr
ensate ^^
mis Total Condensate
Vol. 4^2 -O ml
Culture Tubes and Can Purged With N??
Comments:
Probe Leak Check Data: (/ // / - (&) /Q /) "/
Corresponding Blank Nos.
r L ' u y r\ / xi. "
\\ V = V litor-c v V v 17 M7 v D ..!.P.'-VU r / X  S 9 \ i tore ., ^T\ V\


-------
                                              VOST
 Date
Location
T."st Condition	

Trap Nos.      &3O
                                  '
                                        Sampling  Train No.
                                                           SAMPLING DATA
                                                                    Run  No.
                                                                                               tor
                                           '\S-Z~
                                                                      Meter  Console No.
                            From Can No.
          	             	Pretest Leak Check   0. >   in.Hg/min at _

Barometric Pressure |(P.) ^'P./jS'l In.Hg Ambient Temperature jf)  F Probe Purged  /^ minutes
	.	.	I  b " , ~  I	r-	,	.	,	
                                                                                                   Y -Factor
                                                                                             at   /.
                                                                                      In.Hg vacuum

                                                                                      '  I1ters/m1n
 Sampling
  time,
  min.
  0
          Clock
          time
         (24-h)
   Keter
   volume
  reading,
   liter
                               Rota-
                               meter
                              setting
Sampling
 train
 vacuum,
 In.Hg

 2*0
                                         2,0
                                                    Dry
                                                  gas  meter
                                                  tempera-
                                                  ture, F
 Primary
 condens-
 er exit
temp.,  F
 Probe
tempera-
ture, F
                              ,34
                                                   6JL
                                                                         2-79
                            /
                                        Avg.
Post-Test Leak Check    fl. Q    in.Hg/min at
Flow Direction Marked?
                                 Condensate Recovered?
                                         In.Hg Vacuum    Trap Pair Label No.

                                          	   VGA Label Nos.
Total Volume of Condensate in Vials,

Traps and Vial Stored in Can No.    /

Comments:
                                                                         mis Total Condensate Vol.
                                           ml Remaining Condensate  
                                           on Ice?            Culture Tubes and Can Purged With
                                                                                               ml
Probe Leak  Check  Data:
Corresponding  Blank  Nos.
    std
            ., liters x Y x 17.647  x
                                             - /? ^/liters

-------
Date
                Location
Test Condition

Trap Nos.
                          ~T
                VOST           SAMPLING DATA

             *%eAm_.  <$fe^       Run No.Jj/^T-K
            "*" /       x          .
          Sampling  Train No.   f/~-/fjT-

                                                           <	   VGA Label  Nos.	~
Total Volume of Condensate in Vials, 	

Traps and Vial Stored in Can No.     /
                                           ml Remaining Condensate	mis  Total Condensate Vol.

                                           on Ice?      t^^ Culture Tubes  and  Can Purged With N2?
                                                                                                                ml
Comments:
Probe Leak Check Data:
Corresponding Blank Nos.
0 VetH = Vm, liters x Y x 17.647  x


-------
                                              VOST
                                                           SAMPLING DATA
Date fi/&'7 Location

Test Condition

Trdp Nos.

Barometric Pressure
                                                                    Run No.
                                                                                        : Operator
                                       Sampling Train No.   |/~2->   Meter Console  No.
                                                        Pretest Leak Check
                                                                              in.Hg/min  at
                                                                                                   Y-Factor
                                                                                                (j
                                 in.Hg Ambient Temperature
                                                                 F Probe Purged
                                                                                         minutes at
                                                               in.Hg vacuum

                                                                 I1ters/m1n
Sampling
 time,
 min.
  0
          Clock
          time
         (24-h)
                   Keter
                   volume
                  reading,
                   liter
                                   Rota-
                                   meter
                                  setting
Sampling
 train
 vacuum,
 In.Hg
  Dry
gas meter
tempera-
ture, F
 Primary
 condens-
 er exit
temp.,  F
 Probe
tempera-
ture, F
 /D
 20
                                                                        2&Z.
  10
                                         ^LO_
                            /
                                        Avg.
DO


CO
Post-Test  Leak  Check
                                 in.Hg/min at
                                                         In.Hg Vacuum    Trap Pair Label  No.
Flow Direction  Marked?
                          K
                                                                      VGA Label  Nos.   -6/4Z"- V"
                                                                         mis Total Condensate Vol. c
                                      Condensate Recovered? 	

    Total Volume of Condensate in Vials,  //r,  ml Remaining Condensate	
                                        /.*?
       	           on Ice?     ^"^   Culture Tubes and Can  Purged With N2?

    Comments:
                                                                                                                ml
Probe Leak  Check  Data:
                                                  . Q
Corresponding  BUnlc  Nos.
1)  Vst(j =  Vm,  liters" x Y *  17.647 x
                                    m1
                                                         liters
                                         .
                                      "/.G,

-------
                                   VOST
                Location
                                                                SAMPLING DATA
                                                          Run No.
Test Condition
Trap Nos.      R*/g
                                            Sampling Train No.   y~~~2L~'   Meter Console No.
                                                                                               Operator
From Can No.
                                                        Pretest Leak Check
                                                                    in.Hg/min  at
                                                                                         Y-Factor Z-L^L f
in.Hg vacuum
Barometric Pressure J(Pb) ^7.^2 in.Hg Ambient Temperature && F Probe Purged /'Z-nninutes a
Sampling
time.
min.
0
/
ZO
1*
'h.
m __
Clock
time
(24-h)
/J7
/3.ZJ
/ff^o
zy.fei
zmia
Rota-
meter
setting
33
33
.^5
^~?
Sampling
train
vacuum,
In.Hg
^. O
*^9
>.>
^* ijp j^*
/ Avg.
Dry
gas meter
tempera-
ture, F
/&4
/Of

//
/zz.
JJ2-2'
Prinary
condens-
er exit
temp., F
&%
61
0

^^
V
Probe
tempera-
ture, F
^72?
^72P
277
2-75







t /. cJ liters/min







    Post-Test Leak Check
    Flow Direction Harked?
                Q      in.Hg/min at   &. Q    in.Hg  Vacuum    Trap Pair Label No.
                ~^r~   Condensate Recovered?         ~. ..   VOA Label Nos.      ~~~_
    Total Volume of Condensate in Vials,  ~ -
    Traps and Vial Stored in Can No.     "Z---
                                 ml  Remaining  Condensate   	mis Total Condensate Vol.
                                 on  Ice?    .-^      Culture  Tubes and Can Purged With Ng?
                                                                                                                 ml
    Comments:
    Probe Leak Check Data:
    Corresponding Blank Nos.
0
m
m
            Y x 17.647  x
                                         b'
                                        T
                                        m*
                                                              liters
                                        - '<~\  '
                                        , ^ M

-------
                                                  VOST
Location
                                                           SAMPLING DATA

                                                                    Run No.
Test Condition

Trap Nos. 	
                                       '
                                                                                              Operator
                                            Sampling Train No.
                    Meter Console  No.
                                 From Can No.
                                                                    |Y -
                                                                                    Factor
                                                                                                            _fg 3|
     Barometric Pressure HPT)
                                          	Pretest Leak  Check  &.O   in.Hg/min at     /S.O   in.Hg vacuum
                                 in.Hg Ambient Temperature "%O  F  Probe Purged  /^> minutes at  /> O   liters/min
     Sampling
      time.
      min.
          Clock
          time
         (24-h)
   Meter
   volume
  reading,
   liter
 Rota-
 meter
setting
                                       Sampling
                                        train
                                        vacuum,
                                        in.Hg
  Dry
gas meter
tempera-
ture. F
 Prinary
 condens-
 er exit
temp.,  F
 Probe
tempera-
ture, F
                      Zo.oo
      to
                                        Z.o
                  /f
                                        2-.0
              m
                                             Avg.
CO
I
tn
o
Post-Test Leak  Check
Flow Direction Marked?
                 in.Hg/min at   S. o    in.Hg  Vacuum    Trap Pair Label No.
                 Condensate Recovered?     *		-  VOA Label Nos.    	
     Total  Volume  of  Condensate  in Vials,
     Traps  and Vial Stored  in Can No. 	
                                           ml  Remaining Condensate  *	mis Total Condensate  Vol
                                           on  Ice?     ^  Culture Tubes and Can Purged With N2
                                                                                               ml
     CoMMnts:
     Probe Leak Check Data:
     Corresponding Blank Nos.
M V$td =  Vm,  liters x Y x 17.647 x
                                                   /^/^/liters /
                                         m

-------
                                             VOST
Date $-/7'97  Location
Test Condition  SX?M- IL
Trap Nos.      -  

                                       Sampling Train No.
                                                                SAMPLING DATA

                                                                         Run No. SM?- / Jci Operator

                                                                  \/-~ZL-> Meter Console No.   ^*?- ZJv-Factor  /.MT^ft
     Barometric Pressure |(Pb)
                            From Can No. 	Pretest  Leak Check  &
-------
                                                   VOST
 Date tf"/7- //^Location
Test Condition

Trap Nos.
                                 ^

                             -Tf
                               SAMPLING DATA

                                        Run No.
                                                                                         Operator
            Sampling Train No.

From Can No.       jf-  Pretest Leak Check
                                                                      Meter Console No.
 Barometric Pressure |(P. ) Z^f .3L4jLD.Ha Ambient Temperature  && F Probe Purged
 	.	.	I  D    	HR^	,	,	,	
                                                                              In.Hg/min at
                                                           (-Factor
                                                                                                      , O
                                                                                          minutes at   /
                                                               In.Hg  vacuum

                                                                 liters/min
      Sampling
       time,
       min.
          Clock
          time
         (24-h)
                  Keter
                  volume
                  reading,
                  liter
   Rota-
   meter
  setting
Sampling
 train
 vacuum,
 in.Hg
  Dry
gas meter
tempera-
ture, F
 Prinwry
 condens-
 er exit
temp. ,  F
 Probe
tempera-
ture, F

Z&t
 2&.
                                                                                 tf?
                      90,0'
                                                            7
                                                                              ^77
              m
                            /
                                             Avg.
co
I
tn
     Post-Test Leak Check
Flow Direction Marked?
                                 In.Hg/min  at    ^.O   in.Hg Vacuum    Trap Pair Label  No.
                                 Condensate Recovered?     	VOA Label Nos.
Total Volume of Condensate in Vials,
Traps and Vial Stored in Can No.
Comments:
                                                ml Remaining Condensate  	mis Total  Condensate Vol.
                                                on Ice?      ^^  Culture Tubes  and  Can  Purged With N2?
     Probe Leak Check  Data:
     Corresponding Blank Nos.
1) Vst(J = Vm, liters x Y x 17.647
                                                                       R.MH

-------
                                                   VUbl
Date y //' ^   in.Hg Vacuum    Trap Pair Label No.

      Condensate Recovered?    "VGA Label Nos.
                                                                                                      Y~ Jfa
     Total Volume of Condensate in Vials,
     Traps and Vial Stored in Can No.
          nts:
                                           ml Remaining Condensate -""^  mis Total  Condensate  Vol.

                                           on Ice?     ^^^^  Culture Tubes and Can  Purged With N2?
                                                                                                               ~m\
     Probe Leak Check Data:
                             a o
     Corresponding Blank Nos.
1) Vst(j = Vm. liters  *  Y  *  17.647
                                                                 /

                                                                           t>.\ I

-------
Date
Test Condition

Trap Nos.  	
                                                 VOST
                                                           SAMPLING DATA
                                                                       No.
                                                                                             Operator
                                From Can No.
                                                                     Meter Console No.    j/J3~ 1-|Y-Factor/^^3l
                                                                                          	1             |
                                                   Pretest Leak Check  &O  in.Hg/min  at  /~*.  C.   in.Hg vacuum
                                            Sampl i ng Tra i n No.    {/-
Barometric  Pressure HP^T^
                                           Ambient Temperature
                                                                f Probe Purged
                                                            minutes at   / L?  llters/min
     Sampling
      time,
      min.
          Clock
          time
         (24-h)
                  Meter
                  volume
                  reading,
                  liter
                     ISJ3S
      Rota-
      meter
     settimj
Sampling
 train
 vacuum,
 in.Hg
  Dry
gas meter
tempera-
ture, F
 Primary
 condens-
 er exit
temp.,  F
 Probe
tempera-
ture, F
      J0_
              ;/- '
             //. i
                     Jz,g /.
                m
             m
i
                                /
                                        Avg.
DO
cn
4=.
Post-Test Leak  Check    
-------
                                                   VOST
                                                            SAMPLING DATA
Date
Location
                                           /
                                                                          Run No.
                                                                                           Operator
Test Condition
Trap Nos.     ',
                          t' 7~t-
                     /
                                             Sampling Train No.
                                  From Can No.
                                             .'    .-  -    Meter Console No.   V/'J"    |Y-Factor /.  ^
                                    Pretest Leak Check 	 in.Hg/min  at    /'". <  in.Hg vacuum
Barometric Pressurel(Pb) ^
Sampl ing
time,
min.
0



'. .c
Clock
time
(24-h)
/'"'




Vm
Keter
volume
reading.
liter
!?.44<




5
.go\ in.Hg
j
Rota-
meter
setting
X f




Ambient Tt
Sampling
train
vacuum,
In.Hg




/ Avg.
mperature F Probe Purged minutes at liters/min

Dry
gas meter
tempera-
ture. F



*
,24.4
Primary
condens-
er exit
temp., F




/
Probe
tempera-
ture, F

















CD
I
in
in
Post-Test Leak Check
Flow Direction Marked?
                                  in.Hg/min at    /_<.	 in.Hg  Vacuum    Trap Pair Label  No.   V  ''
                                  Condensate Recovered?                 VGA Label  Nos.
      Total  Volume of  Condensate  in Vials,
      Traps  and  Vial Stored  in Can No. 	
                                            ml  Remaining Condensate 	 mis Total  Condensate  Vol.
                                            on  Ice?             Culture Tubes  and Can  Purged  With N2?
                                                                                                                 ml
     foments:
     Probe Leak Check Data:
     Corresponding Blank Nos.
1) Vstd = Vm, liters x Y x 17.647 x
                                          (B*
                                                   = ZLl>S_3 liters  / -

-------
                                                   VOST
                                                            SAMPLING DATA
      Date
                Location  ' ..
                                   Run No.
                                 Operator
Test Condition S/^f ''-?-_.
Sampling
Trap Nos. <; ' ' ' From Can No.
Barometric Pressure |(PK), / jin.Hg

Sampling
time.
min.
0


. 
1* J'_
Clock
time
(24-h)
/;. <
il'-Of
II ; '

/,' ' -r
Vm
i u   i
Meter
volume
reading,
liter
/. ^
^ /- /
' O
-rs?  %
1 .'/
* * *
515
Rota-
meter
setting
/
'
'::.,'

Train No. ,' ' Meter Console No. ,fr- '-' |Y-Factor . |
Pretest Leak Check
in.Hg/min at /^. f> in.Hg vacuum
Ambient Temperature ' F Probe Purged ''JST minutes at /. O liters/min

Sampling
train
vacuum,
in.Hg
/ . ''

' i -''

/ Avg.

Dry
gas meter
tempera-
ture, F
^
/,- i:.

f ; '
2^L>
Primary
condens-
er exit
temp., F
*-'<*
>

A-tJ
/
Probe
tempera-
ture, F
Ztf?
" r, jf "*
i-

: ' ^'^














DO
I
cn
en
     Post-Test Leak Check
                                                      /
Flow Direction Marked?
                                  in.Hg/min at
Condensate Recovered?
in.Hg Vacuum    Trap Pair Label No.
             VGA Label  Nos.
     Total Volume of Condensate in Vials,
     Traps and Vial Stored in Can No.
     Comments:
                 mis Total  Condensate Vol.
                                            ml  Remaining Condensate
                                            on  Ice?            Culture Tubes and Can Purged With N2?
                                                                               ml
     Probe Leak Check Data:
     Corresponding Blank Nos.
1) Vst(J = Vm, liters K Y x 17.647 x
                                                               liters
                                          m
              \\

-------
                                                                  ..IPLI..- JAT/.
Date
                Location
                                                                     Run No.
Test Condition
Trap Nos.
                         //

                                                                                                Operator
                                             Sampling Train No.
                                  From Can No.
                                                                    	 Meter Console No.
                                                    Pretest Leak Check  &.Q   in.Hg/min  at
      Barometric  Pressure |{P.) Z:tf-'5.  I in.Hg Ambient Temperature  /&  F Probe Purged
      	.	   '   p    .     '        	.	,	_	,	,	
                                                            - 2Lhf-Factor /.go 3]
                                                            > v   . *~~	      t
                                                              <&     in.Hg vacuum
                                                    minutes at   / O   liters/min

Sampling
time,
min.
0
10
10

jj

Clock
time
(24-h)
//.'$&
JJ;M>
fl-llO

/z:2i>
if
Meter
volume
reading.
liter
tun
&?,&6
?3$
fj.fz
/04> 7?o
ZJL-lQt

Rota-
meter
setting
31}
?y
ft
^f ^^j
^y j
Sampling
train
vacuum,
in.Hg
&5
3.0
6.0
rp ^
9.*
7 Avg.
Dry
gas meter
tempera-
ture, F
/It
//I
//y
//y
//&
/Z3.-^
Primary
condens-
er exit
temp., F
+H&Z
?7
4
&&
fi^
*/

Probe
tempera-
ture, F
Zj<^
2.7^
Z.-75
Z77






















CD
I
cn
      Post-Test  Leak  Check
Flow Direction Marked?
                           S
in.Hg/min at   /O. O   In.Hg Vacuum    Trap Pair Label No.
Condensate Recovered?       ^       VOA Label Nos.
Total  Volume  of  Condensate  In Vials,
Traps  and  Vial Stored  in Can No.
Comments:
                                                                                                      - V~Z
                                                 ml Remaining Condensate  ^.  mis Total Condensate Vol.
                                                 on Ice?     \s^    Culture Tubes and Can Purged With N,?
                                                                                                                 ml
     Probe Leak Check Data:
     Corresponding Blank Nos.
                                     b*
   VctH = vm-  liters x Y x  17.647 x T*
    510    m                           *
                                                               liters /<-
                                          m*

-------
                                                    VOST
     f//'/7  Location
Test Condition
                                                           SAMPLING DATA
                                                                    Run No.
                                                                                                         /& MWtt
                                       Sampling Train No.
                                                                            Meter Console No.
                                 Operator
                                 /^-2~[Y^Factor
r rap Nos. f?^. From Can No. Pretest Leak Check fl.O In.Hg/min at /.3. O in.Hg vacuum
larometric Pressure |(Pb) g.1
ampling
time,
min.
0
to
to

fa*
Clock
time
(24-h)
j <4
/ ~" '-jf
tfjtf
/?>/*/
/fZ4
tf:3*t
Vm
Keter
volume
reading,
liter
Q4.225
/0.2<
/^/JZ-
& tfo
2.W7S
2.*$&o
^.<*c)l in.Hg Ambient Temperature 7^ F Probe Purged JZ- minutes at /- c) liters/min
1
Rota-
meter
setting
^7^
34
^Lf
5^

Sampling
train
vacuum,
In.Hg
3.0

to

*/.c>
/ Avg.

Dry
gas meter
tempera-
ture, F
_Jj *J_
//d
/ /S
_^2.L>
LL&&
Primary
condens-
er exit
temp., F
6*7
6>&
$&
g&
/

Probe
tempera-
ture, F
2.72
2.7%
_2J^
2~?o

-------
                                                  VOST
Date
                     Location
Test Condition

Trap Nos.  	
                                       Sampling Train No.
                                 From Can No.
                             SAMPLING DATA

                                      Run No.  5/4 ZT-V~3/70perator

                                        Meter Console No.  l/-Z.   [Y
                                                                                                        -Factor
                                                   Pretest Leak Check   Q.Q   in.Hg/min at
     Barometric Pressure I (P. )"2??_.Q\ in.Hg Ambient Temperature  ^Q  F Probe Purged  /j? minutes at	^
                                                                         in.Hg  vacuum

                                                                        >   liters/min
     Sampling
      time.
      win.
          Clock
          tine
                   Keter
                   voluae
                  reading,
                   liter
 Rota-
 meter
setting
Sampling
 train
 vacuum,
 In.Hg
  Dry
gas meter
tempera-
ture. F
 Primary
 condens-
 er exit
temp. , F
 Probe
tempera-
ture, F

^75-
      fO
                  tf
                                /
                                        Avg.

tn
     Post-Test Leak Check   O.O
     Flow Direction Harked?
                                 in.Hg/min at
                                 Condensate Recovered?
                                                         in.Hg Vacuum    Trap  Pair Label No.  .S*VlX

                                                           	    VGA Label Nos.	
     Total  Volume of Condensate  in Vials, _^
     Traps  and Vial  Stored  in Can No.     3
                                           ml Remaining Condensate      mis Total Condensate Vol.
                                           on Ice?      ^^^ Culture Tubes and Can Purged With N??
                                                                                                                ml
    Coments:
     Probe Leak Check Data:
     Corresponding Blank Nos.
                                         K     U         XI            /
     1) Vstd =  V  ,  liters  x  Y x  17.647 x Tb* ]p>Hg =-^.5?^ liters  /
                                         m*  

-------
CEM DATA SHEETS AND EXAMPLE
      STRIP CHART DATA
             B-60

-------
              DAILY CEM CALIBRATION AND PERFORMANCE EVALUATION
Plant
Location
Date
Operator Li
PN
Run No. "^4
Cal. gas
cone. ,

e,/W ~C"V --
Ou-lfT
''


Drift,
% of span

                ft
                                     10
                                                      o.
                                                                     0$
COMMENTS:
* Perform linear regression of pretest chart divisions vs cal.  gas concentra-
  tions to determine following equation:
          Cone.,
          Correlation coef.
Analyzer cal error =
          chart divisions x (
  ift   [Post-test - pretest] x 100
    l "        Chart div. span
Minimum detectable limit
                  or
% of span
Zero drift =
Cal. drift =
% of span
% of span
                                        B-61

-------
              DAILY  CEM  CALIBRATION AND PERFORMANCE EVALUATION
Plant
Location
Date
Operator
PN
Run No.
                G ^T
                                       Pollutant
                                       Monitor
                                       Span
                                       Chart scale
                                       Pbar, in.Hg
                                       Tamb, deg. F
                                       0,2.
                                      l.K
                                                     /,/
   Cal.  gas       Chart  divisions   /Concentration     Analyzer
    cone.,     -x<3(7<9O>   Post-.*^ predicted by     cal. error,     Drift,
  	      Pretest   test?^     equation*       % of span    % of span
                                                                       o
COMMENTS:

* Perform linear regression  of  pretest  chart divisions vs cal. gas concentra-
  tions to determine  following  equation:
          Cone.,
          Correlation coef.  -
Analyzer cal error = *   '
                           ~  chart  divisions  x  (
                                                       K  100
nrift - Ipost-test -  pretest]  x  100
      ~        Chart  div.  span
Minimum detectable limit =
                                     or
                                               % of  span
Zero drift =
Cal. drift =
                  _% of span
                   % of span
                                      B-62

-------
              DAILY  CEM CALIBRATION AND PERFORMANCE EVALUATION
Plant
Location
Date
Operator
PN
Run No.
Cal. gas
cone. ,

A
^A-VfiJ TT/7VC-
O^-rfer
 n 3
Pollutant C7-2-
Monitor Dfi^r^Q ^&7~~
Span  0-^5*x*
Chart scale * O-'/OQ
Pbar, in.Hg
Tamb, deg. F
.X
^Concentration Analyzer
predicted by cal. error, Drift,
equation* % of span % of span

'** ^ :;f
                                                      At
                                                        , 3
COMMENTS:
                                D ^
* Perform linear regression of pretest chart divisions vs cal.  gas concentra-
  tions to determine  following equation:
                            chart divisions x (	) + (	)
          Cone.,   	                      	
          Correlation  coef.  = 	
                     [Cal.  gas  cone. - cone, predicted] x 100
Analyzer cal  error -

Drift
                              High caK gas cone.
        [Post-test  -  pretest] x  100
               Chart  div.  span
Minimum detectable limit
                                    or
% of span
Zero drift
Cal. drift
                     of span
                   % of span
                                      B-63

-------
                               CO  CEM  DATA SHEET
 Date
        L 1*7
                   PN
              f  - /
 Ablent Temperature 	

 CRF	CO -^   CD "
                               Operator

                               Location
 Time
/ /
If 4$
Zero set
Chart reading
                          O
                          a
                           0
                10,
                           o
                               0
    CO
cone., ppm
                                      -s/0
                                     \\.  l
                                                     0 -S 0 0
                                                                             / n
                                        B-64

-------
       Date
       Pbar
                                      CEM DATA SHEET
                  PN
       Ambient Temperature 	
       CRF           COo    =.
                  Operator
                  Location
y
       Time
Chart reading
cone.,
       I! '
                                         IL
                              63
      B/T
                1L
                                        L
                                         JAA.
                                        ZUL
                                  O
                                           B-65

-------
                         :	CEM DATA SHEET
                                -^tr <^ -/
Date
Ptdr
           ?/i
                 PN

Ambient Temperature
CRF
                 Operator
                 Location
Time
Chart reading
                     37
                    3.L
                           CF
                                cone.,
                                  S.J
                                   5:6"
                                  5"J
                                                             0
                                    B-66

-------
                                CEH DATA SHEET
                                                           
Date
                                      PN
Ambient  Temperature
CRF
                                      Operator ^
                                      Location
Time
             77
                   Chart reading
                         0
                        77
                        0
                        6
                        0
                         0
                        A
                        6
                                                                             //
                                                                        Sfi6/y^
                                       B-67

-------
                                 CEM DATA SHEET
Date
Pbar
                    PN
f
Ambient Temperature
CRF
                    Operator
                    Location
                   Chart reading
                 cone. ,
                       63
                         /
                                        B-68

-------
                               CEM DATA  SHEET
                                                 3&T >j, -^
Date
Pbar
                                     PN
Ambient Temperature
CRF
Operator
Location
                  Chart reading
                                  cone. ,
                     57
                    3?
                    3?
                           O
                                     B-69

-------
             DAILY CEM CALIBRATION AND PERFORMANCE EVALUATION
Plant
Location
Date
Operator
PN
Run No. -5"
Cal. gas
cone. ,

O
-2z/>l/C^
<9cATjtrT
7//7/JP7
D'^di^^f^/
7?2i-7
A-Z^o--} \Sfr3-
-------
              DAILY  CEM  CALIBRATION AND  PERFORMANCE  EVALUATION
Plant
Location
Date
Operator
PN
Run No. <
Cal. gas
cone. ,
o
+ 01
7.W
COMMENTS:




-C.rf Pollutant L.Uz-
O*.~r)t'T Monitor ^Z/J-r//ied /M
Jnk7 Span 0-307C
O. 5cJ\*^Ksf Chart scale O  )<3Q
Pbar, in.Hg
; A JT'^'3 ; gt%.-0A.-'l Tamb, deg. F
Chart divisions ^ Concentration Analyzer
- b1f3 Post/r predicted by cal. error, Drift,
Pretest test/ equation* % of span % of span
H* tfl y.?7" "^ A > ^/7
MY W 7'7^ "1 % -v -> i
x^X , ' I ^ * 	
f^ f< /4.K ^^*j -f^c;
<5^t- *9J *= CiS  5./75> ^;^t. &i/61
5. y>y^  ^



* Perform linear regression of pretest chart divisions vs cal.  gas concentra-
  tions to determine following equation:
          Cone.,
          Corre1atlon coef.
        - chart divisions x (
.  .       .         [Cal. gas cone. - cone, predicted] x 100
Analyzer cal error * J	H   High cal  gas cone.	*	

      - [Post-test - pretest] x 100
    1 ~        Chart div. span
Minimum detectable limit
                  or
% of span
Zero drift

Cal. drift
% of span

% of span
                                       B-71

-------
              DAILY  CEM  CALIBRATION AND  PERFORMANCE EVALUATION
Plant
Location
Date
Operator
PN
Run No. s 'A
Cal. gas
cone. ,

^lAjCs Pollutant
0 Wr/ T" Moni tor
\l/lhl Span
Z). ^b^Ar"-/^* Chart scale
27PV~7 Pbar, in.Hg
jr-A-3 ' ZAjr-tk-/ Tamb, deg. F
Chan divisions Concentration
Oifo^ Post- ^.predicted by
Pretest testi^^L/ equation*

0-2,
DATA n
c^-^i'
0-{0


Analyzer
cal. error,
% of span


FST
y
c^


Drift,
% of span

     o
                 !/>      II,
                                          f
                                                      hi
COMMENTS:
                            ^    CZ>-;J.|>)
* Perform linear regression of pretest chart divisions  vs  cal.  gas  concentra-
  tions to determine following equation:
          Cone.,
          Correlation coef.  =
                             chart divisions x (
        .)  + (.
Analyzer cal error - [C1.   conc.^conc.  predlcttd]  x 100
        [Post-test - pretest] x 100
               Chart div. span
Minimum detectable limit
                                     or
% of span
Zero drift =

Cal. drift =
                   % of span

                   % of span
                                       B-72

-------
   Date
                tlnll
                                 CEM DATA SHEET
          PN
                       54XCO-3
      Ambient Temperature
      CRF
          Operator
          Location
.
tf Time
      J/t-0
      // a ,
                      Chart reading
16
                            rf
                           "0
                           y <;
                                       CO
        cone.,
                                      16
                                        0
                                      n.  o  .
                                      B-73

-------
Date
Pbar
tlnfal
                                 DATA SHEET
   PN
 7   '
Ambient Temperature
CRF
                          Operator
                          Location
Time
        Chart reading
cone.,
                     57 5"
                      63
                       .70,
                                       y/,/
                                 in
                                    B-74

-------
                            ^2- CEH DATA SHEET     5"A"3^  6>i -J
Date
                                       PN
Ambient Temperature
CRF
                                       Operator   L^
                                       Location
t
s
Time
                   Chart reading
cone. ,
                                      7/
                      3?
                      20
                                      1*7
                              ft
                                        B-75

-------
Date
                               CEM DATA SHEET
                                    PN
Ambient Temperature 	
CRF           0 Vnoto  ^   Cb "
                                    Operator
                                    Location
                  Chart  reading
                         0
                         0
                          (J
                                     OP
                                    It.
                                     /(/
                                    1,1
                                     / o
                                    45
                                                      -
                                      B-76

-------
                                     CEM DATA  SHEET    SV7-2ZT  C&} /
Date
                                           PN
     Ambient Temperature 	
     CRF            C0* c//  ^
                                      Operator
                                      Location
PS^
     Time
                   Chart  reading
                             *3-<-
                           L7
                           7
                                         S'.f
                                            -1
                                          //,*/
                                           \\.
                                 0
                                            B-77

-------
                                 CEM DATA SHEET   3V42Z ^7   /
Date
                                       PN
               I
 Ambient Temperature
 CRF
                                      Operator
                                      Location
/***
If/?
                        3 )
                              0
                                         B-78

-------
              DAILY  CEM  CALIBRATION AND PERFORMANCE EVALUATION
Plant
Location
Date
Operator
PN
Run No. ^
Cal. gas
cone. ,

"2-"J /v/C
^ / (C^
(3nty/$'7
or'
372Y-?
A-3E--C.0 ~ 2 *~Q ?
Chart divisions
Of$E> Post-.
Pretest test'y

Pollutant
Monitor
Span
Chart scale
Pbar, in.Hg
Tamb, deg. F
Concentration
V^ predicted by
\ equation*

C.O
fte./vJ
6- -zrt
e^ / t


Analyzer
cal. error,
% of span


i V-
5t>
? ^>


Drift,
% of span

      0
                              O
                                                         0.3
                                                                     0-7
COMMENTS:
                 (1
* Perform linear regression of pretest chart  divisions  vs  cal.  gas  concentra-
  tions to determine following equation:
          Cone.,  	  !
          Correlation coef.
                             chart divisions x (
Analvzer cal  error - [Cal.  gas cone.  - cone,  predicted]  x 100
Analyzer cal  error -           High cal.  gas  cone.

        [Post-test - pretest] x 100
               Chart div.  span
Minimum detectable limit
Zero drift *

Cal. drift =
                   % of span
                   % of span
                                     or
% of span
                                       B-79

-------
             DAILY CEM CALIBRATION AND PERFORMANCE  EVALUATION
Plant
Location
Date
Operator
PN
Run No. ^
Cal. gas
cone. ,

O
+ 0/
-CLjK)]\ Pollutant
^UT/ET Monitor
1//JP/^7 Span
4^r Chart scale
$73^-1 Pbar, in.Hg
'fitt 'Co**' ?-* 3 Tamb, deg. F
Chart divisions Concentration
(?7<>0 Post- predicted by
Pretest test/'T^ equation*
i "
*a ^ 0.0
C 6/ "2-
TXz^
^ -^
^> -y


Analyzer
cal. error,
% of span

tf
-f ; )

>9-cJ.
& %
06


Drift,
% of span

A.
                il
                               1,7)
                          
-------
              DAILY CEM CALIBRATION AND PERFORMANCE  EVALUATION
Plant -TTV/oA
Location Jivr/>'T~
Date l / frfaj
Operator I^>-"
PN %7?-1-'7
Run No. A ^T- **'-}- < 3
r , Chart divisions
ta i . gas r- 1 ^
cone., rOHIc/ Post-
Pretest testi-ip.
| 1 V
0 I! U
COMMENTS: <&JL % ^ C




Pollutant 6X7-
Monitor ii^f:^V'/::n'^' ""^"^
Span ^) -2-rt/*
Chart scale O>"l&(3
Pbar, in.Hg
Tamb, deg. F
Concentration Analyzer
predicted by cal. error, Drift,
0 equation* % of span % of span

-0,3-7 ^,c/ o
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^> i n ' Z., *- ^
/Vj^ " / 7 -r i V
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* Perform linear regression of pretest chart divisions vs cal.  gas concentra-
  tions to determine following equation:

                             chart divisions x (	) + (	)
          Cone., 	  
          Correlation coef.   	

Analvzer cal error = tCal.  gas cone, -cone, predicted] x 100
Analyzer cal error             High cal. gas cone.
Drift
        [Post-test - pretest] x 100
               Chart div. span
Minimum detectable limit
                                     or
% of span
Zero drift =
Cal. drift =
                   % of span
                   % of span
                                       B-81

-------
                              CEM DATA SHEET   ^-A_LU  C0~2-
Date
\nhi
                                   PN
 Ambient Temperature 	
 CRF               (LO
                                   Operator
                                  Location    f) t^r/t.T'
 Time
11*0
                 Chart reading
                      D
                         0
                         6
                           0
                                  12,
                                   i  0
                                   yc/
                                    O
                                                  /yu
                                                        04 Yt,   -
                                     B-82

-------
                                 EM DATA SHEET
Date
Pbar
H
 PN
Ambient Temperature
CRF
                          Operator
                          Location
            I)
                      XV
10
                                    //
                                        . B
                             0
                                      B-83

-------
                                   CEM DATA SHEET
     Date
     Pbar
                                        PN
      Ambient Temperature
      CRF             0>
  Operator
  Location
;)
      Time
      7/5D
*o
                      Chart reading
                          3
                         3 /
                                o
cone.,
                                       S3
                                      jT/7
                                               _^
                                          . Ic.
                                                                    40
                                         B-84

-------
                                CEM DATA SHEET    <&,  -^
Date
 bar
            PN
              L   '
Ambient Temperature
CRF
            Operator
            Location
                   Chart reading
         conc"
                                      10
                                        O
                          6
                         O
                         T?
 7
O
                         6
  fr
                                      CD
                                      B-85

-------
                             CEM DATA SHEET
 Date
  bar
                                 PN
Ambient Temperature 	
CRF           ayy
  Operator

  Location
                           CD  -
                                .
 Time
                 Chart reading
cone.,
                      L7
                                  1. 3
                      4,3
                      L
                                  //.
                      LL
                      7
                                /A?
A

                                 //.
                                 (\ .  \

                                    B-86

-------
                                  CEM DATA SHEET   5-A-It
                   * 7
                    PN
Ambient Temperature
CRF         ^>
                    Operator
                    Location
Time
Chart reading
cone.,
                      3/.
                                      ^L
                                         B-87

-------
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-------
            APPENDIX C



LABORATORY DATA AND ANALYSIS REPORT
              C-l

-------
RADIAN
CORPORATION
DEN:  87-233-006-02
                           ANALYTICAL RESULTS FOR BOAT
                    INCINERATION TESTS OF CERCLA SARM WASTES
                     AT  THE JOHN ZINK COMPANY TEST FACILITY
                                  Prepared For:
                                   Pat Espisto
                              PEI Associates, Inc.
                               11499 Chester Road
                             Cincinnati, Ohio  45246
                                  Prepared By:
                               Radian Corporation
                              8501 MoPac Boulevard
                                 P.O. Box 201088
                            Austin, Texas  78720-1088
                                November 17,  1987
Progress Center/3200 E Chapel Hill Rd./Nelson Hwy iP O Box 13000/Research Triangle Park  NC 27709/1919)541-9100

-------
                                LIST OF TABLES
                                                                       Pace
 2-1  SAMPLE CODING AND STATUS REPORT (Volatile*)  	  2
 2-2  SAMPLE CODING AND STATUS REPORT (VOST)  	  3
 2-3  SAMPLE CODING AND STATUS REPORT
     (SEMIVOLATILES/PARTICULATE/MM5/CL")  	 4
 2-4  SAMPLE CODING AND STATUS REPORT (DIOXINS/FURANS)  	  5
 2-5  SAMPLE CODING AND STATUS REPORT (METALS/METHOD 12)  	  6
 3-1  FINN ICAN-MAT 4000 AND FINNIGAN MAT 5100
     OPERATING CONDITIONS 	  8
 3-2  OPERATING INSTRUCTIONS FOR VOST ANALYSIS
     USING THE FINNIGAN OWA 	  10
 3-3  OPERATING CONDITIONS, FINNIGAN-MAT 4500 	  12
 3-4  HEWLETT-PACKARD 5985 OPERATING INSTRUCTIONS  	  15
 4-1  VOLATILE RESULTS FOR SCRUBBER WATER  	  18
 4-2  VOLATILE RESULTS FOR BOTTOM ASH 	  19
 4-3  VOLATILE RESULTS FOR WASTE FEED 	  20
 4-4  VOST RESULTS FOR STACK EMISSIONS 	  22
 4-5  SEMIVOLATILE RESULTS FOR SCRUBBER WATER,
     ASH, FEED  AND MM5 	  25-26
 4-6  PARTICULATE RESULTS 	  27
 4-7  CHLORIDE RESULTS 	  29
 4-8  DIOXIN/FURAN RESULTS FOR FEED 	  30
 4-9  DIOXIiyFURAN RESULTS FOR ASH 	;...  31
 4-10 DIOXIN/FURAN RESULTS FOR SCRUBBER WATER 	  32
4-11 METALS RESULTS FOR FEED 	  33
4-12 METALS RESULTS FOR ASH 	  34

-------
                          LIST OF TABLES (CONTINUED)
                                                                       Pace
4-13 METALS RESULTS FOR SCRUBBER WATER 	   35
4-14 METALS ANALYSIS FOR METHOD 12 	   36
5-1  VOLATILE SURROGATE RECOVERIES SCRUBBER WATER,
     ASH AND FEED 	   39
5-2  VOLATILE SYSTEM BLANK ANALYSIS RESULTS 	   40
5-3  VOLATILES SPIKE RECOVERY (ACCURACY) AND
     RELATIVE PERCENT DIFFERENCE (PRECISION) FOR BOTTOM ASH 	   42
5-4  VOLATILES SPIKE RECOVERY (ACCURACY) AND
     RELATIVE PERCENT DIFFERENCE (PRECISION) FOR SCRUBBER WATER 	   43
5-5  VOLATILES SPIKE RECOVERY (ACCURACY) AND
     RELATIVE PERCENT DIFFERENCE (PRECISION) FOR FEED 	   44
5-6  VOST SURROGATE PERCENT RECOVERIES 	   46-47
5-7  SYSTEM BLANK DATA FOR VOST ANALYSES 	   49
5-8  SEMIVOLATILE SURROGATE RECOVERIES 	   51-53
5-9  SYSTEM BLANK DATA FOR SEMIVOLATILE ANALYSES 	   55
5-10 SEMIVOLATILE MATRIX SPIKE RECOVERY (ACCURACY) AND
     RELATIVE PERCENT DIFFERENCE (PRECISION) FOR ASH 	   56
5-11 SEMIVOLATILE MATRIX SPIKE RECOVERY (ACCURACY) AND
     RELATIVE PERCENT DIFFERENCE (PRECISION) FOR FEED 	   57
5-12 SEMIVOLATILES MATRIX SPIKE RECOVERY (ACCURACY)
     AND RELATIVE PERCENT DIFFERENCE (PRECISION)
     FOR SCRUBBER WATER 	   58
5-13 CHLORIDE CONTROL CHECK AND MATRIX SPIKE RECOVERY DATA 	   61
5-14 DIOXIN/FURAN EXTRACT SURROGATE RECOVERIES FOR ASH ..-.	   65
5-15 DIOXIN/FURAN EXTRACT SURROGATE RECOVERIES FOR FEED 	   66
5-16 DIOXIN/FURAN EXTRACT SURROGATE RECOVERIES FOR SCRUBBER WATER ...   67
5-17 MINIMUM DETECTION LIMITS FOR METALS BY ICPES/GRAPHITE AA 	   69-70
5-18 DUPLICATE MATRIX SPIKE RECOVERIES FOR METALS IN FEED 	   71
5-19 DUPLICATE MATRIX SPIKE RECOVERIES FOR METALS IN ASH 	   72
5-20 DUPLICATE MATRIX SPIKE RECOVERIES FOR METALS
     IN SCRUBBER WATER 	   73
5-21 DUPLICATE MATRIX SPIKE RECOVERIES FOR METHOD 12 METALS 	   75

-------
                              TABLE OF CONTENTS

                                                                   Page

1.0  Overview	    1

2.0  Sample Description 	    1

3.0  Analytical Methodology 	    7

     3.1  Volatiles 	    7
     3.2  VOST 	    9
     3.3  Semivol ati 1 es 	   11
     3.4  Particulate/Modified Method 5/Chloride	   13
     3.5  Dioxins/Furans 	   14
     3.6  Metals/Method 12 	   16

4.0  Results and Discussion 	   17

     4.1  Volatiles 	   17
     4.2  VOST 	   21
     4.3  Semivolatiles 	   23
     4.4  Particulate/Modified Method 5/Chloride 	   24
     4.5  Dioxins/Furans 	   28
     4.6  Metals/Method 12 	   28

5.0  QA/QC 	   28

     5.1  Volatiles Analyses	   37

          5.1.1  Instrument Calibration and Tuning 	   37
          5.1.2  System Performance  	   37
          5.1.3  Analyte Calibration	   37
          5.1.4  Surrogate Recovery  	   38
          5.1.5  Blanks 	   38
          5.1.6  Duplicate Matrix Spike Analyses 	   38

     5.2  VOST  Analyses 	   41

          5.2.1  Instrument Calibration and Tuning 	   41
          5.2.2  System Performance 	   41
          5.2.3  Analyte CalIbration 	   41
          5.2.4  Surrogate Recovery 	   45
          5.2.5  Blanks 	   48
          5.2.6  Duplicate Matrix Spike Analyses	   48

     5.3  Semivolatiles Analyses  	   48

          5.3.1  Instrument Calibration and Tuning 	   48
          5.3.2  System Performance 	   48
          5.3.3  Continuing Analyte Calibration	   50
          5.3.4  Surrogate Recoveries  	   50
          5.3.5  Blanks 	   54
          5.3.6  Duplicate Matrix Spike Analysis	   54

-------
                         TABLE OF CONTENTS (CONTINUED)

                                                                      Page

     5.4  Particulate/Modified Method 5/Chloride Analyses	   54

          5.4.1  Instrument Calibration and Tuning 	   54
          5.4.2  System Performance 	   59
          5.4.3  Continuing Analyte Calibration 	   59
          5.4.4  Surrogate Recoveries 	   60
          5.4.5  Blanks 	   60
          5.4.6  Duplicate Matrix Spike Analyses	   62

     5.5  Dioxins/Furans Analyses 	   62

          5.5.1  Instrument Calibration and Tuning 	   62
          5.5.2  System Performance 	   63
          5.5.3  Continuing Analyte Calibration 	   64
          5.5.4  Blanks 	   64
          5.5.5  Duplicate Matrix Spike Analysis 	   64

     5.6  Metals/Method 12 Analyses	   64

          5.6.1  Instrument Calibration and System Performance 	   64
          5.6.2  Blanks 	   68
          5.6.3  Interference Check/Control Samples 	   68
          5.6.4  Duplicate Matrix Analysis 	   74

Attachment I - Chain-of-Custody Documentation 	   76-85

-------
 1.0       OVERVIEW

           This  report  contains  the  results  of  the  analyses  for  volatiles,
 VOST,  semivolatiles, particulates,  modified method five  (MM5),  dioxins/furans,
 metals,  Method  12,  and chloride performed on samples  collected  by  PEI  at  the
 John  Zink  pilot  plant  facility  in Tulsa, Oklahoma  using  a rotary kiln
 incineration  system capable  of  handling  1000 Ib/h  of  low-Btu  solids.   Under
 this  work  assignment,  incineration  was evaluated as a "Best Demonstrated
 Available  Technology"  (BOAT)  treatment technology  for CERCLA  wastes  prior to
 land  disposal.   Because Superfund wastes differ markedly from site to  site,
 EPA prepared  two  synthetic soil  samples  containing a  prescribed list of
 contaminants  for  BOAT  testing.   The soil samples were referred  to  as Standard
 Analytical Reference Matrices,  or SARMS.  This sampling  and analysis program
 was accomplished  under a  subcontract  from EPA/HWERL Cincinnati, Ohio
 subcontract No.  750-87,  EPA  contract  No. 68-03-3389.   The volatile organic
 compounds  were analyzed according to  EPA Method 8240,  SW-846, 3rd  ed.  The
 VOST  (<100C) emission samples  were analyzed according to Method 5040, SW-846,
 semivolatiles by  EPA Method  8270, dioxins/furans by EPA  Method  8280, and
 semivolatile  compound  (  > 100C  ) stack emissions  by  Modified Method Five
 method.  The  metals were  analyzed according  to EPA Method 6010  (ICP) and
 Method 7060 ( GF  AAS).  All  metal samples were prepared  by Method  3050,
 SW-846.  Metal stack emission samples were  analyzed according to EPA Method
 12. Particulate samples were  analyzed according to EPA Method 5.   Chloride
 emission samples were  analyzed  by EPA method 300 (1C).
2.0       SAMPLE DESCRIPTION

          The sample coding and status report can be found in Tables 2-1, 2-2,
2-3, 2-4, and 2-5.  The samples were accompanied by a chain of custody record
which was signed by the Radian sample custodian upon inspection of the
samples.  The samples were logged in to the Radian computerized Sample and
Analysis Management system and transferred to a secured facility for storage.
Copies of the chain of custody forms are provided as Attachment 1.

-------
TABLE 2-1.  VOA SAMPLE CODING AND STATUS SUMMARY
Client ID
Scrubber Water
ZSARM-I-l-INF
ZSARM-I-l-S
ZSARM-I-l-S-MS
ZSARM-I-l-S-MSD
ZSARM-I-3-S
ZSARM-I-2-S
ZSARM-II-4-S
ZSARM-II-5-S
ZSARM-II-6-S
Feed Extract
ZSARM-I-l-F
ZSARM-I-l-F-MS
ZSARM-I-l-F-MSD
ZSARM-I-3-F
ZSARM-I-2-F
ZSARM-II-4-F
ZSARM-II-5-F
ZSARM-II-6-F
Bottom Ash
ZSARM-I-l-A
ZSARM-I-l-A-MS
ZSARM-I-l-A-MSD
ZSARM-I-3-A
ZSARM-I-2-A
ZSARM-II-4-A
ZSARM-II-5-A
ZSARM-II-6-A
Reagent Blank
Reagent Blank
Radian
Number

S7-09-061-01B
S7-09-061-03B
S7-09-061-03C
S7-09-061-03D
S7-09-061-05B
S7-09-061-08B
S7-09-061-11B
S7-09-062-02B
S7-09-062-05A

S7-09-061-02B
S7-09-061-02C
S7-09-061-02D
S7-09-061-06B
S7-09-061-09B
S7-09-061-12B
S7-09-062-03B
S7-09-062-06B

S7-09-061-04B
S7-09-061-04C
S7-09-061-04D
S7-09-061-07B
S7-09-061-10B
S7-09-062-01B
S7-09-062-04B
S7-09-062-07B
S7-09-061-13B
S7-09-062-08B
Radian
FRN

0906101B
0906103B
0906103CR
0906103D
0906105B
0906108B
090611 IB
0906202B
0906205B

0906102B
0906102C
0906102D
0906106B
0906109B
0906 112B
0906203B
0906206B

0906104B
0906104C
0906104D
0906107B
0906 11 OB
0906201B
0906204B
0906207B
09061 13A
0906208B
Date
Received

9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87

9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87

9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
Date
Analyzed

9-24-87
9-24-87
9-25-87
9-25-87
9-24-87
9-25-87
9-24-87
9-24-87
9-25-87

9-27-87
9-27-87
9-27-87
9-27-87
9-27-87
9-27-87
9-27-87
9-27-87

9-25-87
9-26-87
9-26-87
9-25-87
9-26-87
9-26-87
9-26-87
9-26-87
9-24-87
9-25-87

-------
TABLE 2-2.   VOST SAMPLE CODING AND STATUS SUMMARY
Client ID
SAI-V-1-A
SAI-V-1-B
SAI-V-1-C
SAI-V-2-A
SAI-V-2-B
SAI-V-2-C
SAI-V-3-A
SAI-V-3-B
SAI-V-3-C
SAII-V-1-A
SAII-V-1-B
SAII-V-1-C
SAII-V-2-A
SAII-V-2-B
SAII-V-2-C
SAII-V-3-A
SAII-V-3-B
SAII-V-3-C
SAI-V-1-Condensate
SAI-V-2-Condensate
SAI-V-3-Condensate
SAII-V-1-Condensate
SAII-V-2-Condensate
SAII-V-3-Condensate
SAI-V-l-2-Field Blank
SAII-V-1-Field Blank
SAII-V-3-Field Blank
Method Blank #1
Method Blank #2
Radian
Number
S7-09-025-01A
S7-09-025-02A
S7-09-025-03A
S7-09-025-04A
S7-09-025-05A
S7-09-025-06A
S7-09-025-07A
S7-09-025-08A
S7-09-025-09A
S7-09-025-10A
S7-09-025-11A
S7-09-025-12A
S7-09-025-13A
S7-09-025-14A
S7-09-025-15A
S7-09-025-16A
S7-09-025-17A
S7-09-025-18A
S7-09-025-19A
S7-09-025-20A
S7-09-025-21A
S7-09-025-22A
S7-09-025-23A
S7-09-025-24A
S7-09-025-25A
S7-09-025-26A
S7-09-025-27A
S7-09-025-28A
S7-09-025-29A
Radian
FRN
OWA870271
OWA870272
OWA870273
OWA870274
OWA870275
Sample Lost
OWA870299
OWA870300
OWA870301
OWA870302
OWA870303
OWA870304
OWA870316
OWA870317
OWA870318
OWA870319
OWA870320
OWA870321
OWA870276
OWA870277
OWA870305
OWA870322
OWA870323
OWA870324
OWA870325
OWA870326
OWA870327
OWA870270
OWA870298
Date
Received
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87

9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
Date
Analyzed
9-25-87
9-25-87
9-25-87
9-25-87
9-25-87

9-29-87
9-29-87
9-29-87
9-29-87
9-29-87
9-29-87
9-29-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
9-25-87
9-25-87
9-29-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
9-25-87
9-29-87

-------
         TABLE 2-3.  SEM1-VOLAT11E/NMS SAMPLE COOING AND STATUS SUMMARY
Client ID
(Scrubber Water)

ZSARM-I-1-S
ZSARM-I-2-S
ZSARM-I-3-S
ZSARM-II-4-S
ZSARM-II-5-S
ZSARM-I1-6-S
ZSARM-I-1-S-MS
ZSARM-i-1-S-MSD
Method Blank
ZSARM-1-1-INF

(Ash)

ZSARM-I-1-A
ZSARM-I-2-A
ZSARM-I-3-A
ZSARM-II-4-A
ZSARM-II-S-A
ZSARM-II-6-A
ZSARM-I-1-A-MS
ZSARM-I-1-A-MSO
Method Blank

(Feed)

ZSARM-I-1-F
ZSARM-I-2-F
ZSARM-1-3-F
ZSARM-II-4-F
ZSARM-II-5-F
ZSARM-1I-6-F
ZSARM-I-1-F-MS
ZSARM-I-1-F-MSO
Method Blank

SAI-V-1
SAI-SV-2
SAI-SV-3
SAII-SV-1
SAM-SV-2
SAI1-SV-3
Method Blank

Reagent Blank MeCl2
Reagent Blank MaOH
Reagent Blank Filter
Reagent Blank XAD-2
Field Train Blank
Radian
Nuater
P7-09-024-01A
P7-09-024-02A
P7-09-024-03A
P7-09-024-04A
P7-09-024-05A
P7-09-024-06A
P7-09-024-07A
P7-09-024-08A
P7-09-024-09A
P7-09-024-40A
P7-09-024-10A
P7-09-024-11A
P7-09-024-12A
P7-09-024-13A
P7-09-024-14A
P7-09-024-15A
P7-09-024-16A
P7-09-024-17A
P7-09-024-18A
P7-09-024-19A
P7-09-024-20A
P7-09-024-21A
P7-09-024-22A
P7-09-024-23A
P7-09-024-24A
P7-09-024-25A
P7-09-024-26A
P7-09-024-27A
P7-09-024-2BA
P7-09-024-29A
P7-09-024-30A
P7-09-024-31A
P7-09-024-32A
P7-09-024-33A
P7-09-024-39A
P7-09-024-34A
P7-09-024-35A
P7-09-024-36A
P7-09-024-37A
P7-09-024-38A
Radian
FRN
F872139
F872142
F872143
F8721U
F872145
F872146
F872U7
F872148
F872138
F872149
F872151
F872154
F872155
F872156
F872157
F872158
F872159
F872160
F872150
F872167
F872168
F872169
F872164
F872165
F872166
F872170
F872171
F872163
F872183
F872186
F872187
F872190
F872191
F872192
F872185
F872178
Sample Lost
F872179
F872182
F872193
Date
Received
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
9-19-87
N/A

M/A
N/A
I/A
Date
Extracted
9-24-87
9-24-87
9-24-87
9-24-87
9-24-87
9-24-87
9-24-87
9-24-87
9-24-87
9-24-87
9-25-87
9-25-87
9-25-87
9-25-87
9-25-87
9-25-87
9-25-87
9-25-87
9-25-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
10-1-87
10-6-87
10-6-87
10- -87
10- -87
10- -87
10- -87
10- -87
10-12-87

10-8-87
10-7-87
10-6-87
Date
Analyze
10-5-87
10- -87
10- -87
10- -87
10- -87
10- -87
10- -87
10-6-87
10-5-87
10-6-87
10-6-87
10-7-87
10-7-87
10-7-87
10-7-87
10-7-87
10-7-87
10-7-87
10-6-87
10-8-87
10-8-87
10-8-87
10-8-87
10-8-87
10-8-87
10-8-87
10-8-87
10-8-87
10-13-87
10-13-87
10-13-87
10-14-87
10-14-87
10-14-87
10-13-87
10-12-87

10-12-87
10-13-87
10-14-87

-------
                  TABLE 2-4.  SAMPLE CODING AND STATUS REPORT (DIOXINS/FURANS)
Sample
 Type
Client
  ID
Radian
Number
  Date
Received
   Date
 Analyzed
Feed
Ash
Scrubber Water
ZSARM-I-2-F


ZSARM-II-5-F


ZSARM-I-2-A


ZSARM-II-5-A


ZSARM-I-2-S


ZSARM-II-5-S
A710003-07-A
   37034

A710003-08-A
   37035

A710003-04-A
   37020

A710003-05-A
   37021

A710003-01-A
   37018

A710003-02-A
   37019
9-29-87


9-29-87


9-29-87


9-29-87


9-29-87


9-29-87
 10-26-87


 10-26-87


 10-26-87


 10-26-87


, 10-26-87


 10-26-87

-------
       TABLE 2-5.   METALS/METHOD 12 CODING AND STATUS SUMMARY

Scrubber Water Samples      Radian Number   Date Received   Date Analyzed
    Client Number
ZARM I 1-S
ZARM I 2-S
ZARM I 3-S
ZARM II 4-S
ZARM II 5-S
ZARM II 6-S
ZARM I 1-S MS
ZARM I 1-S MS dup.
Scrubber Water Method 81 c
ZSARM-I-l-INF
Ash Samples
Client Number
ZARM I 1-A
ZARM I 2-A
ZARM I 3-A
ZARM II 4- A
ZARM II 5-A
ZARM II 6-A
ZARM I 1-A MS
ZARM I 1-A MS dup.
Ash Method Blank
Waste Feed Samples
Client Number
ZARM I 1-F
ZARM I 2-F
ZARM I 3-F
ZARM II 4-F
ZARM II 5-F
ZARM II 6- F
ZARM I 1-F MS
ZARM I 1-F MS dup.
Waste Feed Method Blanl
Method 12 Train Sample;
Client Number
SAI-M-1 3 components
SAI-M-2 3 components
SAI-M-3 (3 components
SAII-M-1 (3 components
SAII-M-2 (3 components
SAII-M-3 (3 components
Container # 6750-A
P7-09-023-la
P7-09-023-2a
P7-09-023-3a
P7-09-023-4a
P7-09-023-5a
P7-09-023-6a
P7-09-023-7a
P7-09-023-8a
ink P7-09-023-9a
P7-09-023-37a
Radian Number
P7-09-023-10a
P7-09-023-lla
P7-09-023-12a
P7-09-023-13a
P7-09-023-14a
P7-09-023-15a
P7-09-023-16a
P7-09-023-17a
P7-09-023-18a
Radian Number
P7-09-023-19a
P7-09-023-20a
P7-09-023-213
P7-09-023-223
P7-09-023-23a
P7-09-023-24a
P7-09-023-253
P7-09-023-26a
c P7-09-023-27a
> Radian Number
P7-09-023-28a
P7-09-023-293
P7-09-023-30a
P7-09-023-31a
P7-09-023-32a
P7-09-023-333
P7-09-023-343
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
Date Received
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
Date Received
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
Date Received
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
9/21/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
Date Analyzed
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
Date Analyzed
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
Date Analyzed
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87
10/13/87

-------
 3.0        ANALYTICAL METHODOLOGY

 3.1        Volatiles

           All  samples analyzed  for  volatile  organics were  analyzed  by gas
 chromatography/mass  spectrometry  (GC/MS)  in  the  full scan  mode,  following  the
 methodology  of Method 8240,  SW-846,  Third  Edition.  The  instrumental
 conditions shown  in  Table  3-1 were  used on a Finnigan-MAT  5100  or a
 Finnigan-MAT 4000 for analysis  of samples  by Method 8240.  Analyte
 identification was performed using  retention times and reference mass spectra
 from  the  analysis of standards; quantitative analysis was  performed by the
 method  of response factors relative  to the closest-eluting of three internal
 standards.   The response factors were generated  from a five-point calibration
 curve.  The  three quantitation  standards were:
                bromochloromethane
                1,4-difluorobenzene
                dj.-chlorobenzene.

           Surrogate  compounds added  to each  sample prior to  analysis  which
 were  used  to  assess  purging  and trapping efficiency were:

               d.-dichloroethane
               dp-toluene bromofluorobenzene.

           The  calibration standard mixtures  contained the  following compounds:

               ethyl benzene
               xylenes (total)
               tetrachloroethylene
               chlorobenzene
               acetone
               1,2-dichloroethane
               styrene.

          Scrubber water samples were purged per Method 8240.  Ash  samples
were purged as an aqueous slurry.   Sludge feed samples were  prepared  by
methanol extraction,  according to Method 8240 (SW-846,  Third Edition), and a
dilution of the methanol  extract was purged.   System blanks  were  prepared  and

-------
            TABLE 3-1.  OPERATING CONDITIONS, FINNIGAN-MAT 4000 AND
                               FINNIGAN-MAT 5100
lonization Mode
Electron Energy
Resolution Unit
Mass Range
Scan Mode
Manifold Temperature
Ion Source Temperature
Interface Temperature
Electron ionization
70 eV, nominal

40 to 300 amu
Linear, 3 sec/cycle
80C
200C
220C
Gas Chromatograph Column

Carrier Gas
Carrier Flow Rate
GC Program
6 ft x 1/8 in, 1% SP-1000 on
 Carbopak B, 60/80 mesh
Helium
30 mL/min
Initial hold of 3 min at 45C;
 45C to 220C at 10/min; hold at
 220C for 18 min
Injector:
 Tekmar LSC 2 Purge and Trap Unit
Purge Time
Desorption Time
Desorption Temperature
Bakeout Time
Bakeout Temperature
 11 min
 4 min
 180C
 12 min
 220C
                                         8

-------
analyzed with these samples.  At least one blank was analyzed per day of
analysis.  In addition, a set of matrix spikes and matrix spike duplicates was
prepared and analyzed for each matrix type as part of the QA/QC for this part
of the program.  A detailed description of all QA/QC performed is presented in
Section 5.1.

3.2       VOST

          All emissions samples for Volatile Organic Sampling Train (VOST)
analysis were analyzed by gas chromatography/mass spectrometry according to
EPA Method 5040, SW-846,. Third Edition.  The instrumental conditions shown in
Table 3-2 were used on a Finnigan OWA for these analyses.  Analyte identifi-
cation and quantification were performed using response factors and retention
times relative to standard compounds.  A five-point calibration curve was
generated initially.  The internal  standard used in Method 5040 is dg-benzene;
hexafluorobenzene was also added for possible use as an internal standard in
the event matrix interferences precluded the use of dg-benzene.

          Blanks that were prepared and analyzed with the field samples
included laboratory blanks and field blanks.  Laboratory blanks consisted of
TenaryTenax charcoal tubes which were cleaned and prepared for use in the
field.  However, the laboratory blanks are sealed and stored in a special
refrigerator, and analyzed in conjunction with the field samples.  A field
blank consists of a set of sampling tubes which have been prepared and shipped
to the field.  These sampling tubes are opened and placed into a sampling
train which does not then draw gas.  The sampling tubes are removed from the
train and returned to the laboratory to be analyzed with the other samples.
Both types of blanks are required to document the nature of any contamination
problems with field samples.  Matrix spikes and matrix spike duplicates are
not part of EPA Method 5040 (SW-846, Third Edition), so none of these
determinations were performed with the VOST samples. Three surrogate compounds
were added to each set of sampling tubes prior to analysis to assess
efficiency of the combined process of desorption and purge and trap.  These
compounds were:

              d4-l,2-dichloroethane
              dg-toluene
              bromofl uorobenzene

-------
TABLE 3-2.  OPERATING CONDITIONS FOR VOST ANALYSIS USING THE FINNIGAN OWA
GC Column
Carrier Gas
Carrier Gas Flow Rate
30 m DB-624 megabore fused silica capillary
Helium
15 mL/min with 15 mL/min makeup
GC Program

Electron Energy
Resolution
Mass Range
5C for 2 min, then 6C/min to 200C,
hold at 200C for 10 min
70 eV, nominal
Unit
35 -250 amu
Scan Cycle
Interface Oven Temperature
Injector Temperature
Manifold Temperature
1 sec/cycle
200C
100C
100C
Tekmar LSC-2
Analytical Trap
Purge Time
Purge Flow
Desorb Time
Desorb Temperature
Bakeout Time
Bakeout Temperature
EPA Method 601
10.0 min
40 mL/min, helium
4.0 min
180C
15.0 min
200C
                                     10

-------
          A  complete description of all QA/QC performed with the VOST analyses
 is  presented  in  Section  5.2.

 3.3       Semi-Volatiles

          All PEI semi-volatile extracts were analyzed by gas chromatography/-
 mass spectrometry following Method 8270 (SW-846, Third Edition).  A Finnigan-
 MAT 4500 using the conditions shown in Table 3-3 was used to perform these
 analyses.  Quantitative  analysis was performed using retention time standards
 and response  factors generated from the mean of a five-point calibration. The
 six internal  standards used for determination of retention times and
 quantitative  analysis were:

               d.-dichlorobenzene
               dg-naphthalene
               d?0-acenaphthene
               djg-phenanthrene
               d17-chrysene
          Target analyte identification was determined from both retention
times and by the match of three major ions from the mass spectrum of the
analyte with the ions in the mass spectral library.  The compounds of interest
for the analysis were:

          t    anthracene
              bis (2-ethylhexyl) phthalate
              pentachlorophenol.

          All semi-volatile extracts were prepared following the extraction
procedures outlined in EPA SW-846, Third Edition.  With the extraction
procedures, a mixture of six surrogate compounds was added to each sample
prior to extraction to assess extraction efficiency.  These surrogate
compounds were:

               d5-phenol
               2-fluorophenol
               d~-nitrobenzene
               2?fluorobiphenyl
               2,4,6-tri bromopheno 1
               d.4-terphenyl.
                14                       11

-------
             TABLE 3-3.  OPERATING CONDITIONS, FINNIGAN-MAT 4500
Ionizer Temperature
Injection Port Temperature
Manifold Temperature
Transfer Line Oven Temperature
Electron Energy
lonization Mode
Resolution
Mass Range
Scan Time
150C
280C
95C
270C
70 eV, nominal I
Electron lonization
Unit
35-450 amu
1 sec/cycle
Column

Column Head Pressure
Carrier Gas
30 m 06-5 fused silica capillary, 0.32 mm
ID, 1.0 u film thickness
8 psi
Helium
Injection Mode
Interface to MS
      i
Injection Volume
GC Program
Splitless 0.6 min, then 10:1 split
Direct Coupling
1 uL of sample extract
Hold at 35C for 4 min, then program at
 10/min to 270C;  hold until elution of
 peaks ceases
                                        12

-------
          A detailed description of all QA/QC performed during the analysis of
 the  semi-volatile extracts is presented in Section 5.3.

 3.4       Particulate/Modified Method 5/Chloride

          Particulates, semivolatile compounds, and chloride collected by the
 Modified Method 5 sampling train were determined by the analytical procedures
 of EPA Method 5 (SW-846, Third Edition), EPA Method 8270 (SW-846, Third
 Edition), and EPA Method 300 (SW-846, Third Edition), respectively.

          Each Modified Method 5 train filter was conditioned in a weighing
 room maintained at less than 50% relative humidity.  Each probe
 residue/solvent rinse was evaporated at room temperature in a fume hood.  The
 samples were protected from air particulate matter in a special designed
 drying shield. All filters and dried probe residues were constant weighed
 using a calibrated analytical balance.

          All  PEI Modified Method 5 train samples were analyzed by gas
 chromatography/mass spectrometry following Method 8270 (SW-846, Third
 Edition).  A Finnigan-MAT 4500 using the conditions shown in Table 3-3 was
 used to perform these analyses.  To prepare the samples, the XAD-z**resin and
 the methylene chloride rinse of the connecting glassware and the first
 impinger were combined in a Soxhlet extractor and extracted for 16 hours.  A
mixture of surrogate compounds was added to each sample during the preparation
process to assess extraction efficiency.  Each XAD-2^ resin sample was spiked
with the following surrogate compounds:

              djQ-anthracene
              2-rluorobiphenyl
              2,4,6-tribromophenol.

          The  condensate and NaOH impinger solutions from each train were
combined and spiked with the following surrogate compounds:

          t    d.Q-anthracene
              dJV-terphenyl
              de-phenol.

                                     13

-------
          Extraction of the condensate/impinger solutions was performed under
both acidic and basic conditions.  After particulate analysis, the residue
from the probe rinse was dissolved in methylene chloride, combined with the
particulate filter in the Soxhlet extractor, and extracted for 16 h.  Each
filter and probe residue was spiked with the following surrogate compounds:

          t    d,Q-anthracene
          t    2-rluorophenol
              dg-nitrobenzene.

          All extracts were combined and concentrated to 1 ml final volume in
a Kuderna-Danish concentrator for GC/MS analysis.  Quantitative analysis was
performed using retention time standards and response factors generated from
the mean of a five-point calibration.  The six internal standards used for
determination of retention times and quantitative analysis were:
               d.-dichlorobenzene
               dp-naphthalene
               d,g-acenaphthene
               dJQ-phenanthrene
               df-'Chrysene
                  -
          Target analyte identification was determined from both retention
times and by the match of the three major ions from the mass spectrum of the
analyte with the ions in the mass spectral library.  The compounds of interest
for the analysis were:

          t    anthracene
              bis (2-ethyl hexyl)phthai ate
              pentachlorophenol.

     A detailed description of all QA/QC performed during the analysis of the
semi-volatile Modified Method 5 train components is presented in Section 5.4.
A small aliquot was obtained from both the train condensates and NaOH impinger
solutions and analyzed for chloride by ion chromatography according to EPA
Method 300 (SW-846, Third Edition).
                                      14

-------
 3.5        Dioxins/Furans

           The  determination of tetra-, penta-, hexa-, and octachlorodibenzo-
 dioxins  (PCDDs)  and  dibenzofurans  (PCDFs) was performed following the
 analytical  methodology  of  EPA Method 8280 (SW-846, Third Edition).  A
 Hewlett-Packard  5985/87 using the  conditions shown in Table 3-4 was used to
 perform  these  analyses.  The analytical procedure employed high resolution
 capillary  gas  chromatography/low resolution mass spectrometry using the
 Selected Ion Monitoring technique.  Quantitative analysis was performed using
 a  recovery  standard,    C-l,2,3,4-tetrach1orodibenzodioxin.  The following
 internal standards are  added at the start of the sample preparation process to
 assess extraction efficiency:

                 C-2,3,7,8-tetrachlorodibenzodioxin
           *      C-2,3,7,8-tetrachlorodibenzofuran
           *      C-l,2,3,7,8-pentachlorodibenzodioxin
           *      C-l,2,3,7,8-pentachlorodibenzofuran
           *      C-l,2,3,6,7,8-hexachlorodibenzodioxin
          *      C-l,2,3,4,7,8-hexachlorodibenzofuran
          *      C-l,2,3,4,6,7,8-heptachlorodibenzodioxin
          *      C-l,2,3,4,6,7,8-heptachlorodibenzofuran
          *      C-pctachlorodibenzodioxin
          *      C-octachlorodibenzofuran.

          Target analyte identification relies upon establishing retention
time windows for the analytes at each level  of chlorination using a specific
retention tine standard, as well  as the presence of all  of the characteristic
ions listed 1n Table 2  of Method 8280 (SW-846,  Third Edition) for each class
of PCDO  and PCDF and the fragment ion (M-COC1)  for confirmation of the
identification.  The maximum intensity of each of the specified characteristic
ions must coincide within 2 scans or 2 sec.   The relative intensities of the
selected isotopic ions within the molecular ion cluster of a homologous series
of PCODs or PCOFs must  lie within the range specified in Table 3 of Method
8280 (SW-846,  Third Edition).   A single response factor is used for the
compounds at each level  of chlorination,  so a single standard 1s used at each

                                    15

-------
           TABLE 3-4.   HEWLETT-PACKARD 5985 OPERATING CONDITIONS
Source Temperature

lonlzation Mode

Electron Energy

Resolution

Interface Temperature

Scan Mode

GC Column
Carrier Gas

Injector

Interface

GC Temperature Program
200C
Electron lonization

70 eV, nominal

Unit
275C
Selected Ion Monitoring

60 m x 0.32 mm ID
J&W DB-5 fused silica
capillary 1.0 u-film
thickness

He 8 15 psi

Cool on-column (35C)

Direct source coupling

Initial hold of 0.5 min,
then 35-200C at 3C/min,
then 200-310C at 4C/min
Injection Volume
1 uL
                                 16

-------
 level of chlorination to determine the response factors.

 compounds are components of the calibration standard:
                                                The following
               2,3,7,8-tetrachlorodibenzodioxin
               2,3,7,8-tetrachlorodibenzofuran
               1,2,3,7,8-pentachlorodi benzodi oxi n
               1,2,3,4,7-pentachlorodibenzodioxin
               1,2,3,7,8-pentachlorodi benzodi oxi n
               2,3,4,7,8-pentachlorodi benzofuran
                 ,2,3,4,7,8-hexachlorodi benzodi oxi n
                 2,3,6,7,8-hexachlorodibenzodioxin
                 2,3,7,8,9-hexachlorodibenzodioxin
                 ,2,3,4,7,8-hexachlorod i benzofuran
                 ,2,3,6,7,8-hexachlorodi benzofuran
                 ,2,3,7,8,9-hexachlorodi benzofuran
                 ,2,3,4,6,7,8-heptachlorodibenzodioxin
                 ,2,3,4,6,7,8-heptachlorod i benzofuran
               1,2,3,4,7,8,9-heptachlorodibenzofuran
               octachlorodi benzodi oxi n
               octachlorodi benzofuran.
          All dioxin/furan extracts were prepared following the extraction/-

purification procedures of Method 8280 (SW-846, Third Edition).  A detailed

description of all QA/QC performed during the analysis of the dioxin/furan

extracts is presented in Section 5.5.
3.6
Metals/Method 12
          The feed, ash, scrubber water, and Method 12 samples were analyzed
for metals using ICPES and graphite furnace atomic absorption techniques.
Prior to analysis, samples were subjected to the acid digestion procedures as
described in Method 3050 (SW-846, Third Edition) and EPA Method 12.
Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) was used for
the analysis of chromium, zinc, lead, cadmium, nickel, and copper.  The basis
of chemical  analysis by ICP-AES is the measurement of the atomic emission by

an optical spectroscopic technique.  Samples are nebulized and the aerosol
that is produced is transported to the plasma torch where excitation occurs.
                                  17

-------
Characteristic atom-line emission spectra are produced by a radio frequency
spectrometer.  These samples were analyzed using a sequential  type ICP-PES (a
computer-controlled slow scan monochromator). The monochromator isolates the
atomic lines of interest and the intensities  are multiplied by the photo-
multiplier.

          Furnace atomic absorption spectrophotometry was used to analyze
samples for arsenic by the procedure outlined in Method 7060,  SW-846 .   An
aliquot of each sample was dried, charred and atomized in a graphite furnace.
Light from a metal-specific hollow cathode tube is passed through the
resulting vapor containing ground-state atoms.  The decrease in the spectral
intensity across the vapor is proportional to the concentration of the metal
being determined.  A detailed description of  the QA/QC performed during the
analysis is presented in Section 5.6.

4.0       RESULTS AND DISCUSSION

4.1       Volatiles

          The results of the analyses of the  volatile samples  for the selected
organic compounds are shown in Tables 4-1 through 4-3.  Scrubber water showed
only the presence of small quantities of acetone in two of the samples.  No
analyte was detected at a level of five times greater than the detection
limit.  Bottom ash (Table 4-2), which was purged as a water slurry, showed the
presence of acetone, 1,2-dichloroethane, ethylbenzene, and xylenes.  Only
acetone was present at a level five times greater than the detection limit in
all of the samples.  Total xylenes were observed at a level greater than five
times the detection limit in only one sample.  All other compounds observed
were present at significantly lower levels in the bottom ash.   The sludge
feeds (analyzed as methanol extracts) showed  very high levels  of all of the
target compounds  (Table 4-3), and required extensive dilution  to avoid
saturation of peaks in the chromatogram and in the mass spectrum.
                                   18

-------
                     TABLE 4-1.   VOLATILE RESULTS FOR PEI  ASSOCIATES  -  SCRUBBER  WATER  (ug/L)
Analyte
icetone
I , 2-dicMoroethane
tetrachloroethene
chlorobenzene
ethyt benzene
styrene
total xylenes
Method
Detection
Limit
8.0
3.0
4.0
6.0
7.0
3.0
5.0
02
ZSARM-
II-5-S
ND
NO
ND
ND
ND
ND
NO
05
ZSARM-
II-6-S
ND
ND
ND
ND
UD
ND
ND
01
ZSARM -
I-1-INF
ND
ND
ND
ND
ND
ND
ND
03
ZSARM-
I-1-S
NO
ND
ND
NO
ND
NO
ND
05
ZSARM
1-3-S
12
NO
ND
NO
ND
ND
ND
08
ZSARM-
I-2-S
17
ND
ND
NO
ND
ND
ND
11
ZSARM-
II-4-5
NO
ND
ND
ND
ND
ND
ND
NO = not detected at  specified detection limit
                                                        19

-------
                  TABLE 4-2.   VOLATILE RESULTS FOR PE!  ASSOCIATES -  BOTTOM ASH  (ug/kg)
Method
Detection
Limit
8.0
oroethane 3.0
roethene 4.0
zene 6.0
ene 7.0
3.0
enes 5.0
01
ZSARM-
1I-4-A
190
ND
ND
ND
8
ND
11
04
ZSARM-
1I-5-A
210
5
ND
ND
NO
ND
6
07
ZSARM-
II -6- A
790
10
ND
ND
13
ND
20
04
ZSARM-
1-1-A
440
ND
NO
ND
ND
ND
ND
07
ZSARM-
I-3-A
630
ND
ND
ND
ND
NO
ND
10
ZSARM-
I-2-A
420
ND
ND
ND
19
ND
34
Analyte

acetone
ethyl benzene
styrene
ND = not detected at specified detection limit
                                                      20

-------
                      TABLE 4-3.    VOLATILE RESULTS FOR  PE1  ASSOCIATES  -  FEED  EXTRACTS  (ug/kg)





acetone
1 ,2-dichloroethane
tetrachloroethene
chtorooenzene
ethylbenzene
styrene
total xylenes


Method
Detection
Limit
8.0
3.0
4.0
6.0
7.0
3.0
5.0
02
ZSARM-
I-1-F
(1:12500dil)
(0.82g)
3300000
450000
NO
340000
3600000
770000
5800000
03
ZSARM-
II-5-F
(1:625dil)
(4.0g)
570000
3500
8500
6900
84000
16000
150000
06
ZSARM -
II -6- F
(1:1250dil)
(0.83g)
270000
28000
36000
30000
330000
67000
520000
09
ZSARM -
I-2-F
(1:12500dil)
<4.0g)
6000000
140000
260000
240000
2400000
580000
4000000
06
ZSARM -
I-3-F
(1:12500dil)
(0.859)
2700000
340000
350000
360000
4000000
810000
6000000
12
ZSARM
11-4-
(1:125
(4.0s
6800C
130C
290C
220C
2400C
510C
12001
NO = not detected at  specified detection limit
                                                          21

-------
          All samples were analyzed within the holding times required by
Method 8240 (SW-845, Third Edition).  GC/MS analysis was performed the same
day as the methanol extraction.
4.2  VOST

          The results for the VOST analysis of incinerator stack emissions are
shown in Table 4-4.  One sample could not be analyzed because the sampling
tube arrived broken.  Only one sample did not show the presence of any
analytes at a detectable level.  All of the other samples contained at least
one analyte at a level five times the detection limit.  Levels of analyte
observed ranged from the detection limit to more than one hundred times the
detection limit.  In view of the extremely high surrogate recoveries
encountered for bromofluorobenzene, values for the late-eluting compounds
(most especially ethyl benzene, styrene, and the xylenes) may be high by the
factor above 100% exhibited by the bromofluorobenzene.  Since response factors
remain stable (as demonstrated by the initial calibration check at the
beginning of the day and an additional calibration check at the end of the
day) and, in general, the blanks do not exhibit these inflated surrogate
compound recoveries, the occurrence of elevated surrogate compound recoveries
in the course of the performance of VOST analyses must be considered a matrix
effect.   The classic means of demonstrating the operation of a matrix effect,
namely,  repeated analysis of the same sample, repeated preparation and
analysis of the same sample, and occurrence of the matrix effect throughout
all analyses of the sample, cannot be performed in the VOST assay, since the
VOST sample consists only of a single set of sampling tubes and the compounds
which are desorbed from the sampling tubes are analyzed in the initial
analysis.  No VOST sample can be re-analyzed.  VOST samples are known to
contain  high levels of water, since stack emissions contain high levels of
water.  Large quantities of water introduced into a chromatographic analysis
and/or into a mass spectrometer will distort the chromatography and will cause
relative signal  levels for the compounds to be distorted.  Additional
components of the stack gases such as various acids can also have the effect
of perturbing the chromatography, and stack emissions are often highly acidic.
                                      22

-------
                                   TABLE 4-4.  VOST RESULTS OF  INCINERATOR  STACK  EMISSIONS  (nanograms)


Compound Compound
acetone acetone
1 , 2-dichl 1 ,2-dichloroethane
perch I oroperch I oroethy lene
ch I orobench I orobenzene
ethylbenzethylbenzene
styrene styrene
total xyltotal xylenes


Compound Compound
acetone acetone
1,2-dichl1,2-dichtoroethane
perch loroperchloroethylene
ch I orobench I orobenzene
ethylbenzethylbenzene
styrene styrene
total xyltotal xylenes
Method
Detection
Limit (ng)
5.0
1.0
1.0
0.7
2.0
2.0
4.0
Method
Detection
Limit (ng)
5.0
1.0
1.0
0.7
2.0
2.0
4.0
01
SA1-
V-1-A
ND
ND
ND
28
230
130
230
10
SAII-
V-1-A
ND
NO
2
ND
12
ND
17
02
SAI-
V-1-B
120
ND
ND
13
74
53
83
11
SAII-
V-1-B
ND
ND
3
10
47
240
82
03
SAI-
V-1-C
210
ND
2
7
29
22
71
12
SAII-
V-1-C
ND
NO
ND
ND
ND
NO
ND
04
SA1-
V-2-A
76
10
9
9
97
40
190
13
SAI1-
V-2-A
ND
1
7
4
14
7
47
05
SA1-
V-2-B
75
ND
ND
2
7
24
37
14
SAII-
V-2-B
ND
ND
5
9
20
1
78
06
SA1-
V-2-C
.






15
SAII-
V-2-C
NO
NO
3
2
6
3
30
07
SAI-
V-3-A
67
16
24
60
120
340
180
16
SAM-
V-3-A
13
NO
21
5
16
7
49
08 (
SAI- S^
V-3-B V'
110
17
29
130
170 :
760
180 !
17
SAI I- SJ
V-3-B V
ND
2
6
2
7
3
18


Compound Compound
acetone acetone
1, 2-dich 1 1,2-dichlorocthan*
perch I oroperch I oroethy t ene
ch I orobench I orobenzene
ethylbenzethylbenzene
styrene styrene
total xyltotal xylenes
Method
Detection
Limit
5.0
1.0
1.0
0.7
2.0
2.0
4.0
25
SAI-V-1-2
FIELD BLANK
NO
ND
1
NO
ND
ND
4
26
SAII-V-1
FIELD BLANK
NO
ND
1
ND
NO
NO
ND
27
SAII-\
FIELD
NO
ND
NO
ND
ND
NO
ND

/-3
BLANK







tube bro'tube broken
                                                          23

-------
The Method 5040 QC measures were executed with acceptable results, but sample
surrogate recoveries are often seen to be above the 50-150% criterion for
acceptability of the method.

4.3       Semi-Volatiles

          The results for the analysis of semi-volatile sample extracts are
shown in Table 4-5.  In analogy to the Volatiles assays, only low levels of
analytes (many of them not more than five times the method detection limit)
are observed in scrubber water and bottom ash.  Relatively low levels of
analytes are also observed in Condensate/Back Methylene Chloride samples. High
levels of analytes, ranging in the millions of ug/kg for some of the analytes,
are observed in the feed extracts.  Results for bis (2-ethylhexyl) phthalate
must be interpreted with caution, however.  Blanks which were analyzed (Table
5-9) show the presence of this compound, with the filter blank, XAD-Z^blank,
and train blanks showing the presence of bis (2- ethylhexyl) phthalate at
levels which range from a factor of approximately 30 times the detection limit
to 65 times the detection limit.  Obviously significant quantities of bis
(2-ethylhexyl) phthalate are detected upon analysis of any of the blanks which
incorporate train components. Contamination by this compound thus is observed
to occur readily, and perhaps a higher criterion for credibility for the
concentration of this compound than a factor of five times the method
detection limit should be considered. If blanks exhibit the presence of the
compound at a level of sixty times the detection limit, then perhaps a
criterion of one hundred times would be more credible than five times the
method detection limit.

4.4       Particulate/Modified Method 5/Chloride

          The results for the analysis of particulate are shown in Table 4-6.
Particulate weights in grams are reported for the filter and the condensate.
As expected,  the weight of particulate is far higher on the filter than in the
condensate.  The results for the Modified Method 5 samples are shown in Table
4-5, with the other semivolatile data.  Pentachlorophenol is observed in one
                                     24

-------
                  TABLE 4-5.  SEMIVOLATILE RESULTS FOR PEI ASSOCIATES   SCRUBBER WATER,  ASH AND FEED EXTRACTS/MM5
Scrubber Water (ug/L)


Analyte
pentachlorophenol
anthracene
bis(2-ethylhexyl)phthalate
Estimated
Instrument
Det Limit
0.4
ND
3
01
2SARM-
1-1-S
8
ND
ND
02
2SARM-
I-2-S
4
ND
5
03
ZSARM-
I-3-S
NO
ND
2.3
04
ZSARM-
II-4-S
ND
NO
5
05
2SARM-
II-5-S
NO
ND
ND
06
2SARM- ZS
II-6-S 1-1
ND
ND
9
Bottom Ash (ug/kg)


Analyte
pentachlorophenol
anthracene
bis(2-ethylhexyl)phthalate
Estimated
Instrument
Det Limit
370
37
63
10
2SARM-
I-1-A
ND
NO
1600
11
ZSARM-
I-2-A
NO
ND
540
12
ZSARM -
I-3-A
ND
ND
740
13
ZSARM-
I1-4-A
:JEfltXXK3XX3tSXX
NO
ND
950
14
ZSARM-
II-5-A
NO
ND
710
15
ZSARM -
II-6-A
ND
ND
1300
Feed Extracts (ug/kg)
         Analyte
Estimated
Instrument
Dt Limit
2SARM-      2SARM-
I-1-F       I-2-F
(1:10 dil)  (1:10 dil)
  21          22
ZSARM-      2SARM-
I-3-F       II-4-F
(1:10 dil)
                                                                                               ZSARM-
                                                                                               II-5-F
ZSARM-
II-6-F
pentachlorophenol                   3300
anthracene                         6000
bis<2-ethylhexyl)phthalate       44,000
               NO            630,000   NO           NO          ND              ND
               6,200,000   8,500,000   5,300,000    480,000     420,000    440,000
               2,800,000   3,300,000   2,200,000    290,000     270,000         NO
                                                         25

-------
                           TABLE 4-5.  CONCLUDED
MMS
XAD-2, Condcnsate/Back MeCl2 (total ug)
zzzzzzzzzxzxzxxzKzzzzszzzza
         Analyte
sssszszzzxzxzzzxsszxzxzzzxzzzzxxx:
pentachIorophenoI
anthracene
bis(2-ethylhexyl)phthalate
                       28       29       31
         Target        SAI-     SAI-      SAM-
       Det  Limit      SV-1     SV-2      SV-1
:XZZZZZZZZZXZZZZZZZ==ZZZZXXXXZXZZXXXXZXZZZZZZZ
            .2           ND      ND         5
          2.9           ND      ND       ND
            .3          230      54       59
MM5
XAD-2 Condensate/Back MeCl2 (total ug)
zzzsxszzzzzzzzzxxsxxxxxxxsz
         Analyte
                                          Target
                                         Det Limit
                        30
                       SAI-
                       SV-3
 32
SAII-
SV-2
                   33
                  SAII-
                  SV-3
pentachlorophenol
anthracene
bis(2-ethylhexyl)phthalate
            .5
            .4
            .4
 ND
 ND
480
 ND
 ND
700
ND
ND
38
                                          26

-------
                    TABLE 4-6.  PARTICIPATE RESULTS
                                         Particulate Weights (grams)
Client ID        Radian Number            Filter        Condensate
SAI-SV-1         P7-09-024-SP-28A         0.1327         0.0101
SAI-SV-2         P7-09-024-SP-29A         0.1081         0.0075
SAI-SV-3         P7-09-024-SP-30A         0.0843         0.0066
SAII-SV-1        P7-09-024-SP-31A         0.0501         0.0045
SAII-SV-2        P7-09-024-SP-32A         0.0367         0.0067
SAII-SV-3        P7-09-024-SP-33A         0.0389         0.0024
                                      27

-------
sample at a level  greater than five times the detection limit,  but no
anthracene is found in any of the train samples.   Bis(2-ethyl  hexyl)phthalate
is observed at very high levels in all  of the samples,  occurring at factors of
several  hundred times the detection limit.   The peak has been  identified
accurately by both retention time and mass  spectrum, but the results should be
interpreted with caution and a knowledge of the field history  and treatment of
the samples, since this compound is a very  common contaminant.  Levels observed
in field blanks were far lower than the values obtained for the field samples,
but the field samples could still be dealing with some contamination which
occurred in the field.

         The results for the analysis of the aliquots from the Modified Method
5 samples are presented in Table 4-7.  The  chloride values ranged from 1.7 to
20 mg for the condensates and impingers.  The measured chloride per train
ranged from 6.9 (SAII-SV-3) to 36.6 (SAI-SV-I) total milligrams.

4.5       Dioxins/Furans

          The results for the analysis of the dioxin/furan samples are shown
in Tables 4-8 to 4-10.  No levels of dioxins or furans above the Method
detection limit were observed in any of the samples, while all  surrogate
compound recoveries were within the limits  specified by Method 8280 (SW-846,
Third Edition).

4.6       Metals/Method 12

          The results for the analysis of the metals in waste feed, ash, and
scrubber water are shown in Tables 4-11 to 4-13,  respectively.   The metal
results of the analysis by Method 12 of the stack emissions are given in Table
4-14.
5.0       QA/QC
                                     28

-------
TABLE 4-7.   PE1  CHLORIDE ANALYSIS
            SAMPLE RESULTS
Date
10/8/87
10/8/87
10/7/87
10/7/87
10/7/87
10/7/87
10/7/87
10/7/87
10/7/87
10/7/87
10/8/87
10/8/87
Field 
SAI-SV-1
SAI-SV-1
SAI-SV-2
SAI-SV-2
SAI-SV-3
SAI-SV-3
SAII-SV-1
SAII-SV-1
SAII-SV-2
SAII-SV-2
SAII-SV-3
SAII-SV-3
Work Order
P709026
P709026
P 709026
P709026
P709026
P 709026
P 709026
P 709026
P 709026
P709026
P709026
P709026
Sample *
01A
02A
03A
04A
OSA
06A
07A
OSA
09A
10A
11A
12A
Description
condensate
impinger
condensate
impinger
condensate
impinger
condensate
impinger
condensate
impinger
condensate
impinger
ppm
14.6
8.9
14.3
11.3
8.4
5.1
4.2
4.4
2.1
1.0
2.3
2.5
Total Vol.
1410
1800
1370
1020
2200
560
1555
1005
2380
520
2270
670
mg
20.59
16.02
19.59
11.53
18.48
2.86
6.53
4.42
5.00
5.20
5.22
1.68
snvsx3
             29

-------
            TABLE 4-8.  DIOXIN/FURAN RESULTS ng/g
                              FEED
                  Reagent blank     ZSARM 1-2-F       ZSARM-II-5-F
Analyte           A7l6oi8-Blank     A710003-07-A      A710003-08-A
                     37031             37034             37035
Total TCDD
Total TCDF
Total PCDD
Total PCDF
Total HxCDD
Total HxCDF
Total HpCDD
Total HpCDF
Total OCDD
Total OCDF
<0.2
<0.2
<0.2
<0.2
<0.5
<0.4
<0.6
<0.4
<1.6
<0.7
<0.6
<0.5
<0.4
<0.4
<1.0
<0.9
<0.6
<0.8
<1.6
<1.6
<0.6
<0.5
<0.5
<0.4
<1.1
<0.8
<0.6
<1.1
<2.2
<1.7
NOTE: All Surrogate recoveries are within method prescribed limits,
                          30

-------
                  TABLE 4-9.  OIOXIN/FURAN RESULTS ng/g
                                  ASH
                  Reagent blank           ZSARM 1-2-A       ZSARM-II-5-A
Analyte           A710003-3540 blank      A710003-04-A      A710003-05A
                     37022                   37020             37021
Total TCDD
Total TCDF
Total PCDD
Total PCDF
Total HxCDD
Total HxCDF
Total HpCDD
Total HpCDF
Total OCDD
Total OCDF
<0.2
<0.1
<0.2
<0.2
<0.4
<0.3
<0.5
<0.3
<0.6
<0.5
<0.2
<0.1
<0.2
<0.1
<0.3
<0.2
<0.4
<0.3
<0.5
<0.4
<0.2
<0.1
<0.2
. <0.1
<0.3
<0.2
<0.4
<0.3
<0.6
<0.5
NOTE:  All  Surrogate recoveries are within method  prescribed  limits.
                                     31

-------
                  TABLE 4-10.
DIOXIN/FURAN RESULTS ng/L
  SCRUBBER

Analyte

Total TCDD
Total TCDF
Total PCDD
Total PCDF
Total HxCLD
Total HxCDF
Total HpCDD
Total HpCDF
13C-OCDD
13C-OCDF
Reagent blank
A7l6003-blank
37017
<2
<}
<2
<1
<3
<2
<4
<2
<5
<4
ZSARM 1-2-S
A710003-01A
37018
<2
<1
<2
<1
<3
<2
<4
<2
<4
<4
ZSARM-II-5-S
A710003-02A
37019
<1
<1
<1
<1
<3
<2
<4
<2
<4
<4
NOTE:  All  Surrogate recoveries are within method prescribed limits.
                                     32

-------
           TABLE  4-11.   PEI  WASTE  FEED  SAMPLE RESULTS
jAnalyte |Analysis| Method MOL Sample
I


I
i

t
(Arsenic
:hromium
I
| Zinc
Lead
)
I
'Cadmium
, Nickel
I
I
Copper
Type [Detection {assuming 5 \ 2ARM I





GF AAS
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
Limit |gram sample | 1-F



(total ug)
0.200
1.50
0.600
21.0
0.600
1.50
2.10

-Myte |Analysis| Method
Type (Detection
I

I
trsenic GF AAS
i
'"hromium| ICAP

I 2 1 nc 1 CAP
1
Lead ICAP

| Cadmium ICAP
i
Nickel ICAP
i
| Copper | ICAP
Limit
(ug/mL)
0.002

|P7-09-023

(ug/g)
0.040
0.300
0.120
4.20
0.120
0.300
0.420
-19a
(ug/g)
16.9
24.2
451
261
26.3
27.5
244

Comments
Sample
JP7-09-023
| -19a

All samples
(ug/mL)
0.886
| brought to j
0.015 J100 mL finaj 1.270
| volume.
0.006 |AU samplesj 23.620
((except the)
0.210 j blank) used) 13.680
1 5 grams of |
0.006 (dry solid, j 1.380
((Reported j
0.015 jus/g per j 1.440
(dry wight.)
0.021 | j 12.790
I
Sample
ZARM I
2-F

P7-09-023
-20a
(ug/g)
17.2
32.8
551
296
25.4
29.8
267
Sample
ZARM I
3-F

P7-09-023
-21a
(ug/g)
19.7
30.6
526
292
26.0
26.8
261

Sample
Sample
P7-09-023|P7-09-023
20a
(ug/mL)
0.858

1.640

27.520

14.810

1.270

1.490

13.370
-21a
(ug/fflL)
0.992

1.540

26.490

14.690

1.310

1.350

13.120
Sample
ZARM II
4-F

P7-09-023
-22a
(ug/g)
19.1
30.1
548
328
26.5
29.5
282

Sample
P7-09-023
-22a
(ug/mL)
0.959

1.510

27.530

16.470

1.330

1.480

14.160
Sample
ZARM II
5-F

P7-09-023
-23a
(ug/g)
19.3
27.3
508
301
25.6
27.6
250
Sample Sample
ZARM II
6-F

P7-09-023
-24a
(ug/g)
17.8
26.6
158
302
25.8
28.1
255
ZARM I
1-F MS

P7-09-023
-25a
(ug/g)
28.8
115
1200
543
118
117
804
Sample Sampl
ZARM I
Metho
1-F MS | Blank
Duplicate!
P7-09-023JP7-09-0
-26a -27a
(ug/g)
30.3
121
1280
587
121
120
836
(total
0.3
< 1.5
3.
< 21.
< 0.6C
< 1.5
< 2.1

Sample
Sample Sample Sample Sampl
P7-09-023|P7-09-023|P7-09-023|P7-09-023|P7-C9-t
-23a
(ug/mU
1.040

1.470

27.380

16.210

1.380

1.490

13.450
-24a
(ug/mL)
0.904

1.350

8.030

15.320

1.310

1.430

12.950
-25a
(ug/mL)
1.450

5.810

60.690

27.370

5.940

5.900

40.540
26s
(ug/mL)
1.520

6.060

64.370

29.420

6.080

6.020

41.930
-27;
(ug/ml
O.t

< MDI

O.I

< MDI

< MDI

< MOI

< MDI
                                                                            XZZZZ>ZZZXX=XXZZZZXXXZXZX=ZZXXXZXZXXZXZZZX=;:===.
MDL  Method Detection Limit
                                                                  33

-------
                TABLE 4-12.  PEI ASH SAMPLE RESULTS
Analyte | Analysis) Method






Arsenic
Chromium
Zinc
Lead
Cadmium
Nickel
Copper
Type (Detection





GF AAS
I CAP
I CAP
I CAP
1CAP
I CAP
I CAP
Limit



(total ug)
0.200
1.500
0.600
21.000
0.600
1.500
2.100

|Analyte
|
I
I ========
Arsenic
|
|Chromium
|
j Zinc
|
| Lead
|
Cadmium
|
I Nickel
|
I Copper

Analysis! Method
Type j Detect ion


GF AAS

I CAP

ICAP

1CAP

ICAP

ICAP

ICAP

Limit
(ug/Rl)
0.002
MDL
assuming 5
gram sample



(ug/)
0.040
0.300
0.120
4.20
0.120
0.300
0.420
Sample
ZARM I
1-A

P7-09-023
10a
(ug/g)
SMBXSBSS
37.7
(a) 9.80
217
56.2
< 1.48
11.8
111
Sample
ZARM I
2-A

P7-09-023
11a
(ug/g)
XX3XWWZ
36.1
13.5
227
97.8
< 1.50
14.8
132

Comments Sample | Sample
JP7-09-023JP7-09-OZ3


| All samples
(brought to
0.015 | 100 m final
| volume.
0.006 j All samples
((except the
0.210 (blank) used
| 5 grams of
0.006 (dry solid.
{(Reported
0.015 jug/g per
(dry weight.)
0.021 j
I
-10a
(ug/mL)
1.920

(a)0.500

11.075

2.863

< MDL

0.600

5.638

-11a
(ug/mL)
1.800

0.675

11.338

4.875

< MDL

0.738

6.600
9**MM
Sample
ZARM I
3-A

P7-09-023
12a
(ug/g)
43.8
(a) 11.9
250
(a) 107
< 1.49
11.4
159

Sample
P7-09-023
-12a
(ug/mL)
2.200

(a)0.600

12.550

(a)5.388

< MDL

0.575

Sample
ZARM II
4-A

P7-09-023
13a
(ug/g)
45.5
11.8
252
146
(a) 3.20
12.0
125
Sample
ZARM II
5-A

P7-09-023
-14a
(ug/g)
38.6
6.90
199
75.1
< 1.48
9.12
106
Sample
ZARM II
6-A

P7-09-023
-15a
(ug/g)
37.4
(a) 9.60
237
(a) 88.3
< 1.45
12.3
162
Sample Sample
ZARM I ZARM I |
1-A MS 1-A MS j
(duplicate!
P7-09-023|P7-09-023|
-16a
(ug/g)
55.9
101
1130
610
87.7
102
604
-17a
(ug/g)
61.5
101
1170
604
87.6
103
585

Sample Sample Sample | Sample Samp I
P7-09-023|P7-09-023|P7-09-023|P7-09-023|P7-09-l,.
-13a
(ug/mL)
2.320

0.600

12.863

7.438

(a)0.163

0.613

7.998 6.350
I
**xcx*xxssaesKSXXXBBX
-Ha
(ug/mL)
1.960

0.350

10.100

3.813

< MDL

0.463

5.400

-15a
(ug/mL)
1.940

(8)0.500

12.263

(a)4.575

< MDL

0.638

8.375

-16a
(ug/mL)
2.810

5.063

56.588

30.688

4.413

5.113

30.388

-178
(ug/n>L)
3.110

5.100

59.250

30.513

4.425

5.212

29.563

MDL = Method Detection Limit
(a) amount shown is a default value,  but agrees with  the amount
                                                       34

-------
        TABLE 4-13.  PE1 SCRUBBER WATER SAMPLE RESULTS
lAnalyte |Analysis| Method
] | Type JDeteetion
1
1
I 1
i i
1
|
jArsenic | GF AAS
1
1
iromium| ICAP
i
! 1
| Zinc | ICAP
t
i
Lead | ICAP
i i
1 !
Cadmium | ICAP
1
1
, Nickel | ICAP
i i
! 1
Copper | ICAP
1
Limit



(ug/mL)*
0.001
0.008
0.003
0.105
0.003
0.008

Sample
ZARM I
1-S

P7-09-023
01e
(ug/mD
0.150
0.530
2.U
(a) 1.75
2.35
0.320

0.011 |(a) 0.595
I
Sample
ZARM I
2-S

P 7- 09- 023
02a
(ug/mL)
0.260
0.363
4.40
1.52
4.13
0.76

(a) 0.530
Sample
ZARM I
3-S

P7-09-023
03a
(ug/mL)
0.150
0.505
1.81
2.25
1.89
0.265

(a) 0.475
Sample
ZARM II
4-S

P7- 09-023
-04a
(ug/mL)
0.270
0.610
2.92
2.23
3.57
0.360

(a) 0.550
Sample
ZARM II
5-S

P7-09-023
-05a
(ug/mL)
0.180
0.535
1.66
2.02
2.03
< 0.075

(a) 0.585
Sample
ZARM II
6-S

P7-09-023
-06a
(ug/nl)
0.405
0.835
3.34
4.82
5.77
0.265

1.14
Sample
ZARM 1
1-S MS

P7-09-023
-07a
(ug/mL)
0.700
3.60
10.9
9.51
19.3
2.96

4.32
Sample
ZARM 1
1-S MS
Duplicate
P7-09-023
-08a
(ug/mL)
0.760
3.39
11.1
9.83
18.6
2.93
i
4.26
Sample
Method
Blank

P7-09-023
-09a
(ug/mL)
0.004
0.020
< 0.003
< 0.105
< 0.003
7.49

0.540

MOL = Method Detection Limit
  11 Amount shown is a default value,  but agrees with the amount
    found in the undiluted sample.
  ror samples concentrated from 200 to 100 ml.
                                                                   35

-------
 Table 4-U,  PEI  METHOD  12  TRAIN  SAMPLE  RESULTS
rrrrsssrs
|Analyte
I
I
I
I
I
I
-"="
(Arsenic
jChromiutn
(
| Zinc
I
| Lead
| Cadmium
Analysis
Type
GF A AS
ICAP
ICAP
ICAP
ICAP
I
| Nickel | ICAP
I
| Copper ICAP
1 1
Method
Detection
Limit
(total ug)
0.200
1.50
0.600
21.0
0.600
1.50
2.10
Sample
ZARM I
M-1
P7-09-023
28a
(total ug)
40.3
167
940
1740
4250
750
447
Sample
ZARM I
M-2
P7-09-023
-29a
(total ug)
44.7
135
602
1970
2730
103
525

lAnalyte
i
i
1
1
1
[Arsenic
1
(Chromium
| Zinc
i
| Lead
i
1
[Cadmium
| Nickel
i
| Copper
1
Analysis
Type
GF AAS
ICAP
ICAP
ICAP
ICAP
ICAP
tCAP
Method
Detection
Limit
(ug/mL)
0.002
0.015
0.006
0.210
0.006
0.015
0.021
Sample
P7-09-023
28a
(ug/mt)
0.403
1.670
9.400
17.380
42.510
7.500
4.470
Sample
P7-09-023
29a
(ug/ml)

0.447
1.350
6.020
19.700
27.320
1.030
5.250
Sample
ZARM I
M-3
P7-09-023
30a
(total ug)
27.2
141
1150
2520
6090
89.0
708

Sample
P7-09-023
-30a
(ug/ml)
0.272
1.410
11.530
25.180
60.850
0.890
7.080
Sample
ZARM II
M-1
P7-09-023
-31*
(total ug)
13.7
78.0
411
923
3000
101
(a) 225

Sample
P7-09-023
-31a
(ug/ml)
0.137
0.780
4.110
9.234
29.970
1.008
|(a) 2.247
Sample
ZARM II
M-2
P7-09-023
-32a
(total ug)
13.3
43.8
284
811
2920
70.6
108
Sample
ZARM II
M-3
P7-09-023
-33a
(total ug)
21.3
32.8
148
750
2170
57.1
83.0

Sample
P7-09-023
-32a
(ug/nu.)
0.133
0.438
2.838
8.110
29.204
0.706
1.084
Sample
P7-09-023
-33a
(ug/mL)
0.213
0.328
1.484
7.500
21.677
0.571
0.830
Sample
6750-A
Nitric
Blank
P7-09-023
-34a
(total ug)
0.300
< 1.50
5.50
< 21.0
< 0.600
< 1.50
< 2.10

Sample
P7-09-023
34a
(ug/ml)
0.003
< MDL
0.055
< MDL
< MDL
< MDL
< MDL
Sample
6750-B
Filter
Blank
P7-09-023
-35a
(total ug)
NA
NA
NA
NA
NA
NA
NA
Sample
Method
Blank
P7-09-023
-36a
(total ug)
< 0.200
< 1.50
3.00
< 21.0
< 0.600
3.20
< 2.10

Sample
P7-09-023
-35a
(ug/n>L>(c)
0.439
< MDL
0.141
< MDL
< MDL
< MDL
< MDL
Sample
P7-09-023
-36a
(ug/mD
< MDL
< MDL
0.030
< MDL
< MDL
0.032
< MDL
 MDL : Method Detection Limit
 NA = Not Available
                                  txxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
                                                                           xxxxxxxxxxx
                                                                      36

-------
5.1       Volatiles

5.1.1     Instrument Calibration and Tuning

          The volatile samples were analyzed according to the QA/QC procedures
outlined in Method 8240, SW-846, Third Edition.  The mass calibration and the
instrument tune were verified daily by using perfluorotributyl amine.  The
acceptability of a tune to meet QC criteria for bromofluorobenzene (Method
8240) was demonstrated daily prior to the initiation of any analyses.

5.1.2     System Performance

          System performance was demonstrated initially with a five-point
calibration.  A minimum average response factor of 0.3 (0.25 for bromoform)
was obtained for the System Performance Check Compounds (SPCCs) specified in
Method 8240:

               chloromethane
               1,1-dichloroethane
               bromoform
               1,1,2,2-tetrachloroethane
               chlorobenzene.

          The minimum response factor criterion was demonstrated every 12
hours for the duration of the volatiles analyses.

5.1.3     Analvte Calibration

          The initial five-point calibration of 5, 10, 50, 100, and 200 ug/L
standards,  used for generating response factors, demonstrated a percent
relative standard deviation (% RSO) of less than 30 for all of the calibration
check compounds (CCCs)  shown below:

               1,1-dichloroethene
               chloroform
               1,2-dichloropropane
               toluene
               ethyl benzene
               vinyl  chloride.
                                       37

-------
          This criterion for correspondence of values within 30% RSD was
demonstrated every twelve hours for the duration of the volatiles analyses for
this program.

5.1.4     Surrogate Recovery

          To monitor the efficiency of the purge and trap operation, each
sample was spiked with three surrogate compounds before analysis, as specified
in Method 8240, SW-846, Third Edition.  These compounds are:

              d.-l,2-dichloroethane
              dp-toluene
          t    bromofluorobenzene.

          Actual surrogate recoveries are listed in Tables 5-1.  All
recoveries were between 90-122%, within acceptable QA/QC limits.

5.1.5     Blanks

          At least one daily system/reagent blank was analyzed to check for
background contamination or contamination of the analytical  system.  All of
the method blank data can be found in Table 5-2.  No contamination was found
in any of the blanks;  no corrections were made for contamination in the
blanks.

5.1.6     Duplicate Matrix Spike Analyses

          A sample from each matrix was used to perform duplicate matrix spike
analyses.  Each sample was spiked with 100 ng of each of the following matrix
spike compounds according to Method 8240, SW-846, Third Edition:

               acetone
               1,2-dichloroethane
               tetrachloroethene
               chlorobenzene
               ethyl benzene
               styrene
               total xylenes

                                      38

-------
TABLE 5-1.  VOLATILE SURROGATES PERCENT  RECOVERIES:  SCRUBBER WATER, ASH, AND FEED

Scrubber Water
Surrogates
d4-1,2-dichloroethane
d8- toluene
Bromof I uorobenzene
Bottom Ash



Surrogates
d4-1 ,2-dichloroethane
d8- toluene
3 romof I uorobenzene
02
ZSARM-
II-5-S
92
98
106

01
ZSARM-

I I-4-A
101
108
100
05
ZSARM-
II-6-S
96
94
107

04
ZSARM-
Me *
5-A
122
101
96
01
ZSARM-
I-1-INF
96
102
105

07
ZSARM-
M^ 
O-A
121
102
100
03
ZSARM-
I-1-S
108
105
105

04
ZSARM-


91
101 .
99
03
ZSARM-
I-1-S-MS
109
97
104

04
ZSARM -


111
105
102
03
ZSARM-
I-1-S-MSO
113
94
102

04
ZSARM-
t . 1 -A-ucrt
i i  nau
106
103
100
05
ZSARM
I-3-S
94
103
107

07
ZSARM-
. _ A

90
105
89
08
ZSARM -
I-2-S
100
96
106

10
ZSARH-
1 -2-A
ten
SSMMSMS
95
105
100
                                                                                                             11
                                                                                                            ZSARM-
                                                                                                            n-4-5

                                                                                                             103
                                                                                                             98
                                                                                                             108
Feed Extract
Surrogates
64-1,2-diehtoroethane
d8- toluene
Bromof tuorobenzene
Blanks


Surrogates
d4  1 , 2  d i ch I oroethane
'8- toluene
6 romof I uorobenzene
03
ZSARM -
II-5-F
95
96
100

08
REAGENT
06 02 02 02 06 09 12
ZSARM- ZSARM- ZSARM- ZSARM- ZSARM- ZSARM- ZSARM-
II-6-F 1-1-F I-1-F-MS I-1-F-MSD I-3-F I-2-F II-4-F
106 106 107 108 110 96 97
102 103 102 103 101 96 96
104 106 106 104 103 103 102

13
REAGENT
BUNK BLANK
93 91
102
99
107
106
                                                    39

-------
         TABLE 5-2.   VOLATILE SYSTEM BLANK ANALYSIS RESULTS
                      FOR PEI ASSOCIATES (ug/L)
Analyte
acetone
1,2-dichloroethane
tetrachloroethene
chlorobenzene
ethyl benzene
styrene
total xylenes
Method
Detection
Limit
8.0
3.0
4.0
7.0
7.0
3.0
5.0
8
REAGENT
BLANK
ND
ND
ND
ND
ND
ND
ND
13
REAGENT
BLANK
ND
ND
ND
NO
ND
ND
ND
ND = not detected at specified detection limit
                                       40

-------
          Tables  5-3  -  5-5  show the accuracy and precision of these analyses.

 5.2       VOST Analyses

 5.2.1     Instrument  Calibration and Tuning

          The VOST samples  were analyzed according to the QA/QC procedures
 outlined in Method 5040, SW-846, Third Edition.  Acceptability of the
 instrument tune was verified daily by the analysis of 50 ng of
 bromofluorobenzene.   No analyses were initiated until an acceptable tune
 according to the  criteria of Method 8240 (SW-846, Third Edition) had been
 demonstrated.

 5.2.2     System  Performance

          System  performance was established initially using a five-point
 calibration to ensure a minimum average response factor of 0.3 (0.15 for
 acetone) for the  System Performance Check Compounds  (SPCCs):

               acetone
               1,2-dichloroethane
               tetrachloroethylene
               chlorobenzene
               ethyl benzene
               styrene
               xylene (total).

          Since Method 5040 does not specify SPCCs, the analytical target
 compounds were selected as SPCCs.   The minimum response factor of 0.3 (0.15
 for acetone)  was demonstrated daily.

 5.2.3     Analvte Calibration

          The initial  five-point calibration of 20, 50, 100, 250, and 500 ng,
used for generating response factors,  also demonstrated a percent relative
standard deviation (% RSO) of less than 30 for all  of the target compounds:
                                       41

-------
TABLE 5-3.   VOLATILE;  SPIKE RECOVERY  (ACCURACY) AND RELATIVE.PERCENT DIFFERENCE (PRECISION) FOR BOTTOM ASH
Matrix Spike = 100 ug/kg
acetone
1 ,2-dichloroethane
tetrachloroethene
chlorobenzene
ethylbenzene
Determined
ZSARM-I-1-A
0906104B
440
ND
NO
ND
ND
Concentration
ZSARM-I-1-A
0906104C
1600
160
110
110
HO
(ug/kg)
MS ZSARM-I-1-A USD
09061040
1100
130
120
110
HO
SPIKE
RECOVERY
1160
160
110
110
HO
SPIKE
RECOVERY
DUPLICATE
660
130
120
110
HO
RELATIVE
PERCENT
DIFFERENCE
55
21
9
0
0
                                                       42

-------
TABLE 5-4.   VOLATILES  SPIKE  RECOVERY  (ACCURACY) AND RELATIVE PERCENT DIFFERENCE (PRECISION) FOR SCRUBBER WATER
                             Determined  Concentration  (ug/L)
Matrix Spike = 100 ug/L
acetone
1,2-dichloroethan*
tetrachloroethene
chlorobenzene
ethylbenzene
styrene
total xylenes
ND - not detected.
ZSARM-I-1-S
0906 103B
ND
ND
ND
ND
ND
ND
ND

2SARM-I-1-S MS
0906103CR
50
110
85
92
85
85
49

ZSARM-I-1-S USD
09061 030
54
120
96
100
98
96
56

SPUE
RECOVERY
50
110
85
92
85
85
49

SPIKE
RECOVERY
DUPLICATE
54
120
96
100
98
96
56

RELATIVE
PERCENT
DIFFERENCE
8
9
12
8
14
14
13

                                                     43

-------
    TABLE 5-5.   VOlATILES  SPIKE  RECOVERY  (ACCURACY) AND RELATIVE PERCENT DIFFERENCE (PRECISION) FOR FEED EXTRACT
Matrix Spike = 100 ug/kg
acetone
1,2-dichloroethane
tetrachloroethene
chlorobenzene
ethylbenzene
styrene
total xylenes
Determined
ZSARM-I-1-F
09061028
220
30
36
22
2(0
50
380
Concentration
2SARM-I-1-F
09061 02C
330
160
140
130
390
160
540
(ug/kg)
MS ZSARM-I-1-F MSO
09061020
340
170
140
no
400
170
550
SPIKE
RECOVERY
110
130
104
108
150
110
160
SPIKE
RECOVERY
DUPLICATE
120
140
104
118
160
120
170
RELATIVE
PERCENT
DIFFERENT
9
7
0
9
6
9
6
NO = not detected
                                                          44

-------
               acetone
               1,2-dichloroethane
               tetrachloroethylene
               chlorobenzene
               ethyl benzene
               m-, ji-xylene
               o-xylene
               styrene.

This criterion was demonstrated daily for the duration of the VOST analyses.

5.2.4     Surrogate Recovery

          To monitor desorption/purge and trap efficiency, each sample was
spiked with three surrogate compounds immediately before analysis.  These
compounds are listed below:
                                                                       i
              d.-l,2-dichloroethane
          t    dg-toluene
              bromof1uorobenzene

Actual recoveries are listed in Table 5-6.  The Method Blanks (Laboratory
Blanks of VOST tubes) show surrogate recoveries which range from 45% for
bromof1uorobenzene to 108% for dg-toluene.  Field Blanks show a range of 81%
for dg-toluene to 206% for bromof1uorobenzene.  Most of these recoveries are
within the acceptable range as determined by Method 8240 (SW-846, Third
Edition).  However, actual sample surrogate recoveries show the following
ranges:

          broMfl uorobenzene               141% - 585%
          d.-1,2-dichloroethane             79% - 158%
          dg-toluene                        94% - 393%.

The sample which showed the very high surrogate recoveries also exhibited poor
chromatography on the megabore column: both of the internal standard peaks
were wide and diffuse.  The presence of large quantities of water on the
sampling tubes may be inferred, illustrating a matrix effect on this sample.
                                       45

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               TABLE 5-6.   VOST SURROGATE PERCENT RECOVERIES

Sample 1.0.            p-Bromofluoroberuene    d4-1,2-Dichloroethane    d8-Toluene

SA1-V-1-A
OWA870271                          585                     158             393

SA1-V-I-B
OWA870272                          258                     112             155

SAI-V-I-C
OUA870273                          212                     104             139

SAI-V-1I-A
CJA870274                          223                      93             139

SAI-V-II-B
CUA870275                          219                      94             131

SAI-V-MI-A
CWA870299                          257                     101             141

SAI-V-I II-B
OUA870300                          281                     101             134

SAI-V-III-C
OUA870301                          279                     141             103

SAII-V-I-A
OWA870302                          199                      91             117

SAI1-V-1-B
CWA870303                          220                     108             110

SAII-V-I-C
OUA870304                          203                     103             109

SAIl-V-ll-A
OWA870316                          245                      84             171

SA1I-V-II-B
OUA870317                          267                      79             155

SAII-V-II-C
OUA879318                          197                      85             153
                                                  46

-------
                        IA8LE  5-6.  CONCLUDED

Sample  I.D.             p-Bromof luorobenzene    d4-1 ,2-Dichloroethane    d8-Toluene
SAI1-V-III-A
OUA870319                          264                      94              US

SAII-V-MI-B
OUA870320                          203                      88              U8

SAII-V-IU-C
OUA870321                          260                      89              158

SAI-V-1 CONDENSATE
OUA870276                          220                      92              127

SAI-V-II CONDENSATE
OWA870277                          207                      88              12;

SAI-V-II1 CONDENSATE
OWA870305                          211                     102              94

SAII-V-1 CONDENSATE
OUA870322                          279                      96              158

SAIt-V-2 CONDENSATE
OWA870323                          292                      97              166

SAIl-V-III
OUA870324                          299                      98              169

SAI-V-I-2 FIELD BLANK
OWA870325                          206                      95              154

SAII-V-1 FIELD BLANK
OWA870326                          119                     101              81

SAII-V-3 FIELD BLANK
OWA870327                          101                      94              95

METHOD BLANK 1
OWAS70270                           45                     105              69

METHOD BLANK 2
OWA870298                           87                     108              78
                                                 47

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5.2.5     Blanks

          Daily laboratory blanks,  consisting of clean sampling tubes which
had not been sent to the field,  were analyzed to check for background
contamination.  The results are shown in Table 5-7.   No significant
contamination was observed on the sampling tubes.   Results for the field blank
analyses are reported with the data for the field samples.

5.2.6     Duplicate Matrix Spike Analyses

          Since duplicate matrix spike analyses are not required according to
the protocol of Method 5040 (SW-846, Third Edition) and since the ability to
perform these analyses is dependent upon the supply of a given sample in
triplicate from the field, no duplicate matrix spike analyses could be
performed because the samples were not supplied for spiking.

5.3       Semi-Volatiles

5.3.1     Instrument Calibration and Tuning

          All semi-volatile extracts were analyzed using the QA/QC procedures
outlined in Method 8270, SW-846, Third Edition, without significant
modification.  The tune of the mass spectrometer used for these analyses was
verified  by demonstrating an acceptable mass spectrum of
decafluorotriphenylphosphine every twelve hours.  Acceptable chromatography
was verified daily by examination of the shape of the chromatographic peaks
produced by benzidine and pentachlorophenol.

5.3.2     System Performance

          System performance was verified daily beginning with the initial
five- point calibration by demonstrating that system performance check
compounds (SPCCs) had response factors greater than 0.05 using the 50 ug/mL
calibration standard.  The System Performance Check Compounds are:
                                       48

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   TABLE 5-7.  SYSTEM BLANK DATA FOR VOST ANALYSES (NG)
                       ESTIMATED    28A         29A
                       LIMITS OF    METHOD      METHOD
ANALYTE                DETECTION    BLANK #1    BLANK = 2
Acetone                   5.0          NO          NO
1,2-dichloroethane        1.0          NO          ND
Perchloroethylene         1.1          ND          ND
Chlorobenzene             0.7          ND          ND
Ethylbenzene              1.8          ND          ND
Styrene                   1.6          ND          ND
Total  Xylenes             3.8          ND          ND
                        49

-------
              N-Nitrosodi-n-propylamine
          a    hexachlorocyclopentadiene
              2,4-dichlorophenol
          t    4-nitrophenol.


5.3.3     Continuing Analvte  Calibration


          In the course of generating a five-point calibration for this

program,  response factors for the  calibration check compounds (CCCs) were

verified  to have less than 30% relative standard deviation (RSD) over the
calibration range.  The calibration check compounds (CCCs) were:


               phenol
               1,4-dichlorobenzene
               2-nitrophenol
               2,4-dichlorophenol
               hexachlorobutadiene
               4-chloro-3-methyl phenol
               acenaphthene
               2,4,6-trichlorophenol


               N-nitroso-di-N-phenylamine
               pentachlorophenol
               fluoranthene
               di-n-octyl phthalate
               benro(a)pyrene


The analysis of the Calibration Check Compounds was repeated every twelve
hours to  verify that the response  factors were within 30% of the mean
generated in the five-point calibration curve.


5.3.4     Surrogate Recoveries


          Surrogate recoveries were determined for all of the semi-volatile

samples,  blanks, and matrix spikes.   Surrogate recoveries are shown in Table

5-8.
                                       50

-------
                       TABLE  5-8.    SEMIVOLATILES  SURROGATE  PERCENT  RECOVERIES

                       2-cluoro-      d5-        dS-Nitro-      2-Fluoro-      2,4,6-Tri-        d14-
Sample 1.3             pnenol         Phenol     benzene        biphenyl       bromophenol       Terphenyl
Scrubber Water
ZSARM-I-1-S
F872139
ZSARM-I-2-S
F872H2
ZSARM-1-3-S
'872143
ZSARM-II-4-S
F872144
ZSARM- Ii-5-S
F872U5
ZSARM- I I-6-S
F872146
ZSARM-I-1-S MS
F872K7
ZSARM- I-1-S MSD
372148
METHOD BLANK
F872138
ZSARM- 1-1- INF
F872H9
Bottom Ash
ZSARM- I -1-A
F872151
ZSARM-I-2-A
F872154
2SARM-I-3-A
F872155
ZSARM-II-4-A
F872156
ZSARM- 11-5-A
F872157
ZSARM-1I-6-A
F872158


75 84 72 98 114 101

86 101 69 90 64 94

86 96 94 95 97 109

82 96 67 89 105 92

64 78 91 87 87 95

48 61 92 87 77 90

74 93 77 91 48 95

35 91 69 91 55 91

48 73 79 87 69 102

77 88 103 88 87 88


24 46 84 80 12 91

9 39 65 77 13 89

25 55 79 84 30 93

2 10 82 86 NO 99

4 13 64 75 ND 94

15 40 79 79 ND 91
                                                                51

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TABLE 5-8.   CONTINUED
Sample I .0
ZSARM-I-1-A MS
F872159
2SARM-1-1-A MSD
F872160
METHOD BLANK
F872150
Feed Extract
ZSARM-I-1-F
F872167
ZSARM-I-2-F
F872168
ZSARM-I-3-F
F 872 169
ZSARM-II-4-F
F 872 164
ZSARM-II-5-F
F872165
i
2SARM-II-6-F
F 872 166
ZSARM-I-1-F MS
F872170
ZSARM-1-1-F MSD
F872171
METHOD BLANK
F872163
2-Ftuoro-
phenol
5
7
79

91
88
89
80
85
89
78
84
83
d5-
Phenol
38
25
90

96
91
94
92
91
87
78
85
90
d5-Nitro-
Benzene
69
74
88

93
90
93
94
90
92
73
84
92
2-Fluoro-
biphenyl
73
73
86

115
110
118
105
112
109
107
109
112
2,4,6-Tri-
bromo phenol
ND
ND
84

24
119
122
102
112
121
137
142
114
d14-
Terphenyl
82
85
93

107
103
107
98
101
109
106
101
97
                    52

-------
                                                  TABLE 5-8.  CONCLUDED

                       2-Ftuoro-      a5-         d5-Nitro-     2-Fluoro-     2,4,6-Tri-      d14-           d10-
Sample I.D             phenol         Phenol      benzene       biphenyl      bromophenol     Terphenyl      Anthracene

SAI-SV-1
F872183                   77            85           88            95             91            93              83

SAI-SV-2
F872186                   62            54           66            97            101            88              44

SAI-SV-3
FS72187                   63            57           68            97            104            99              55

SAM -SV- 1
F872190                    64            58           55            90           122            100              84

5AI1-SJ-2
F872191                    65            64           63            93           111            91              79

SAII-SV-3
'872192                    69            52           57            96           113            88              92

         Reagent Blanks

 'agent Blank MeCl2
F872178                    NO            NO           ND            NO            NO            NO              NR

Reagent Blank Filter
?372179                    69            ND           69            NO            ND            ND              84

Reagent Blank XAD-2
F872182                    NO            ND           NO            90            20            ND              100

Field Train Blank
F872193                    64            68           53            95            98            96              102

Method Blank Train
F872185                    50            57           52            35            78            90              71


ND - Not Detected
                                                            53

-------
5.3.5     Blanks

         At least one extraction blank was generated for each sample set.   No
target analytes were detected in any of the blanks.   Results of the analyses
of blanks are shown in Table 5-9.

5.3.6     Duplicate Matrix Spike Analyses

          A sample from each matrix type was used to perform duplicate matrix
spike analyses.  Prior to extraction,  samples were spiked with a mixture
containing the following compounds:

              anthracene
              bis (2-ethylhexyl)  phthalate
              pentachlorophenol.

The accuracy and precision of these analyses is reported in Tables 5-10,
5-11, and 5-12.

5.4       Particulate/Modified Method 5/Chloride

5.4.1     Instrument Tuning and Calibration

          All particulate samples  were weighed on an analytical balance.  The
balance was checked at each use with a set of NBS certified Class S weights.

          All Modified Method 5 extracts were analyzed using the QA/QC
procedures outlined in Method 8270 (SW-846, Third Edition), without
significant modification.  The tune of the mass spectrometer used for these
analyses was verified by demonstrating an acceptable mass spectrum of
decafluorotri- phenylphosphine every twelve hours.  Acceptable chromatography
was verified daily by examination  of the shape of the chromatographic peaks
produced by benzidine and pentachlorophenol.
                                      54

-------
         TABLE 5-9.  SYSTEM BLANK DATA FOR SEMIVOLATILE ANALYSES (ug/L)


                           pentachlorophenol    anthracene    bis(2-ethythexyt)phthalate

Estimated Limits
of Detection                    5                  0.4                     0.7

METHOD BLANK
F872138                         7                   NO                    ND

METHOD BLANK
F872150                        ND                   NO                    13

METHOD BLANK
F872163                        ND                   ND                    ND

REAGENT BLANK MeCl2
F872178                        ND                   NO                    ND

REAGENT BLANK FILTER
F872179                        ND                   ND                    29

REAGENT BLANK XAO-2
F872182                        ND                   ND                    43

FIELD TRAIN BLANK
F872193                        ND                   ND                    45

METHOD BLANK TRAIN
F872185                        ND                   ND                    40


NO = Not Detected
                                                55

-------
TABLE 5-10.   SEMIVOLTILES MATRIX SPIKE RECOVERY (ACCURACY) AND RELATIVE DIFFERENCE (PRECISION) FOR ASH
=r==z==zr=rzzzzzzzzzzzzszs=zzzzzzzssz=zzzzzzz=zzzzzzzzzz=zzzzzzzzzz=zzzzzzs=zz!
Determined Concentration dig/ml)
Matrix Spike = 100 ug/g
ZSARM-I-1-A ZSARM-I-1-A MS ZSARM-1-1-A MSI
F872151 F872159 F872160
Pentachlorophenol NO ND NO
Anthracene ND 90 87
8is(2-ethylhexyi)phthatate 13 200 126
BZZZZZZZZSZZZZZZZZZZZZSZZZZZZZZZZZZZZZZ
SPIKE RELATIVE
) SPIKE RECOVERY PERCENT
RECOVERY DUPLICATE DIFFERENCE
0 00
90 87 3
187 113 49
                                                  56

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TABLE  5-11.   SEMIVOLATILES MATRIX SPIKE  RECOVERY  (ACCURACY)  AND  RELATIVE  DIFFERENCE  (PRECISION)  FOR  FEED
Determined Concentration (ug/g)
3tnx Spike = 100 ug/g


Penrachtorophenol
Anthracene
3; ;(2-etnyihexyl )pntnala'
ZSARM-I-1-F
F 872 167
ND
74
ce 33
ZSARM-I-1-F MS
F872170
116
210
134
ZSARM-I-1-F MSO
F872171
138
215
139
SPIKE
SPIKE RECOVERY
RECOVERY DUPLICATE
116 138
136 141
101 106
RELATIVE
PERCENT
DIFFERENCE
17
4
5
                                                         57

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 TABLE 5-12.   SEMIVOLATILES MATRIX SPIKE RECOVERY (ACCURACY)  AND RELATIVE DIFFERENCE (PRECISION) FOR SCRUBBER WATER
========"
                                Determined Concentration  (ug/ml)
Matrix Spike = 100ug/ml
                                ZSARM-I-1-S
                                F872139
              2SARM-I-1-S MS
              F872147
2SARM-I-1-S MSD
F872148
SPIKE
RECOVERY
SPIKE
RECOVERY
DUPLICATE
RELATIVE
PERCENT
DIFFERENCE
Fen:ocruorophenol

Anthracene
8             74

ND            89

NO            123
80

84

118
66          72

89          84

123         118
                                                                58

-------
          All chloride analyses were performed on a Dionex Model 16 ion
chromatograph.  All standards were prepared from ACS reagent-grade chemicals,
A multipoint calibration curve was prepared and a linear regression analysis
performed to determine the best-fit linear calibration fit for the chloride
ion.


5.4.2     System Performance


          System performance was verified daily beginning with the initial

five-point calibration by demonstrating that System Performance Check

Compounds (SPCCs) had response factors grater than 0.05 using the 50 ug/mL
calibration standard.  The System Performance Check Compounds are:


              N-nitrosodi-n-propylamine
              hexachlorocyclopentadiene
          t    2,4-dichlorophenol
          t    4-nitrophenol.


5.4.3     Continuing Analvte Calibration


          In the course of generating a five-point calibration for this

program, response factors for the Calibration Check Compounds (CCCs) were

verified to have less than 30% relative standard deviation (RSD) over the

calibration range.   The Calibration Check Compounds which were used were:


               phenol
               1,4-dichlorobenzene
               2-nitrophenol
               2,4-dichlorophenol
               hexachlorobutadi ene
               4-ch1oro-3-methylphenol
               acenaphthene
               2,4,6-trichlorophenol
               N-nitroso-di-N-Phenylamine
               pentachlorophenol
               fluoranthene
               di-n-octyl  phthalate
               benro(a)pyrene
                                        59

-------
          The analysis of the Calibration Check Compounds  was repeated every
twelve hours to verify that the response factors were within 30% of the mean
generated in the five-point calibration curve.

          On each analysis day for chloride by  ion chromatography a multipoint
calibration curve was prepared.  A check sample was analyzed each day with the
results shown in Table 5-13.  Check sample values agreed within 99 percent of
the true chloride concentrations.

5.4.4     Surrogate Compound Recoveries

          Surrogate recoveries were determined  for all of the Modified Method
5 samples and blanks.  Surrogate recoveries are shown in Table 5-8.

5.4.5     Blanks

          For the set of Modified Method 5 samples, the following blanks were
generated and analyzed:

               Methylene Chloride Reagent Blank
               Filteg Reagent Blank
               XAD-2* Reagent Blank
               Method Train Blank
               Field Train Blank.

          Results of the analyses of blanks are shown in Table 5-9.   All of
the blanks  associated with components of the sampling train  showed  levels of
bis(2-ethyl  hexyl) phthalate at  a level of at  least 40 times the detection
limit.  The  presence of the phthalate at this  high level suggests  a systematic
contamination  in the train with  plasticizers.  However, the  level  of the
bis(2-ethyl  hexyl) phthalate in  the samples analyzed  is an  additional  factor
of 50-70  times the level observed in the blanks.
                                      60

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TABLE 5-13.   CHLORIDE CONTROL  CHECK  AND
       MATRIX SPIKE RECOVERY DATA
  Date         Work Order      Sample #         Description          ppm

10/8/87        P709026            13A          reagent  blank

10/7/87        P709026            UA         method blank  #1          NO

10/8/87        P709026            15A         method blank  2          NO

10/8/87        P709026            16A           Matrix  Spike         15.8

10/8/87        P709026            17A           Matrix  Spike         15.1
                                                 Duplicate

10/7/87                                      Check  Sample  #1         9.1
                                                 9.09  ppm

10/8/87            *               *           Check  Sample  #2         9.0
                                                 9.09  ppm
                                             Comments
                                              nitric  interferences
                                              98.1% recovery

                                              93.8% recovery


                                              99.89X agreement


                                              99.01 X agreement
                 61

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           Blank method chloride results are shown  in Table 5-13.  A method
 blank was  a  prepared and analyzed each day.  A reagent field blank was
 analyzed;  however, a nitrate  ion interference prevented the determination of
 chloride.  A  check of the reagent blank documentation, disclosed that nitric
 acid had been added to the sample prior to aliquoting for metals sample
 preparation.

 5.4.6      Duplicate Matrix Spike Analyses

           Because additional  train samples were not available for analysis,
 duplicate  matrix spike analyses were not performed for the Modified Method 5
 extracts.  Two matrix spike chloride samples were  analyzed by ion
 chromatography.  The chloride method recoveries (  93.8 and 98.1%) are shown in
 Table 5-13.

 5.5        Dioxins/Furans

 5.5.1      Instrument Tuning and Calibration

           The GC/MS instrumentation was tuned to meet the isotopic ratio
 criteria listed in Table 3 (Method 8280,  SW-846,  Third Edition) for
 polychlorinated dibenzodioxins and dibenzofurans.   Once tuning and mass
 calibration procedures were completed,  a column performance check mixture
 containing a mixture of PCDD and PCDF isomers was analyzed to check retention
 windows for each of the homologues,  to verify that the GC resolution of
 2,3,7,8- tetrachlorodibenzodioxin and 1,2,3,4-tetrachlorodibenzodioxin was
 adequate,  and that the relative ion abundance criteria listed in Method 8280
 for PCDDs  and PCDFs were acceptable.   The chromatographic peak separation
 between 2,3,7,8-tetrachlorodibenzodioxin and 1,2,3,4-tetrachlorodibenzodioxin
 showed a valley of <25%.   Adequate sensitivity for Method 8280 was verified by
 achieving  a minimum signal-to-noise ratio of 50:1  for the ion of mass 320 of
 2,3,7,8-tetrachlorodibenzodioxin obtained from injection of the 200 ng/mL
 calibration standard.   The concentration  levels for the calibration samples
were 200, 500,  1000,  2000,  and 5000 ng/mL.   Triplicate determinations of
                                    62

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response factors for each calibration standard were performed;  the percent
relative standard deviations were within 15%.  All dioxin/furan extracts were
analyzed using the QA/QC procedures outlined in Method 8280 (SW-846, Third
Edition), without significant modification.  The continuing stability of the
calibration was verified every twelve hours of operation.

5.5.2     System Performance

          System performance was verified daily by analysis of the 500 ng/mL
calibration standard with all analytes within 30% of the mean values
established by the initial  analyses of the calibration standard solutions. GC
column performance was demonstrated initially and verified prior to analysis
of any samples in the twelve-hour period.  The GC column performance solution
was analyzed under the same chromatographic and mass spectrometric conditions
used for other samples and standards.  The components of the GC column
performance solution are:

              tetrachlorodibenzodioxins
               1,3,6,8;  1,2,8,9;  2,3,7,8;  1,2,3,4;  1,2,3,7;  1,2,3,9
              pentachlorodibenzodioxin
               1,2,4,6,8;  1,2,3,8,9
              hexachlorodibenzodioxin
               1,2,3,4,6,9;  1,2,3,4,6,7
              heptachlorodibenzodioxin
               1,2,3,4,6,7,8; 1,2,3,4,6,7,9
              octachlorodibenzodioxin
               1,2,3,4,6,7,8,9
              tetrachlorodibenzofuran
               1,3,6,8;  1,2,8,9
              pentachlorodibenzodioxin
               1,3,4,6,8;  1,2,3,8,9
              hexachlorodibenzofuran
               1,2,3,4,6,8;  1,2,3,4,8,9
              heptachlorodibenzofuran
               1,2,3,4,6,7,8;  1,2,3,4,7,8,9
          t    octachlorodibenzofuran
               1,2,3,4,6,7,8,9 5.5.3
                                    63

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5.5.3     Continuing Analvte Calibration

          In the course of generating  a fifteen-point calibration for this
program,  response factors for the entire range of calibration compounds
exhibited a percent relative standard  deviation less than 15%.   The daily
calibration check with the 500 ng/mL calibration standard showed that the
measured  response factors were within  30% of the mean values established by
the initial analyses of the calibration standard calibration solutions.

5.5.4     Blanks

          A reagent blank was generated with each matrix in this sample set.
No target analytes were detected at or above their detection limits.  The
results of the analyses of the Reagent Blanks are shown in Table 5-14  (ash),
5-15 (feed), and 5-16 (scrubber water).

5.5.5     Duplicate Matrix Spike Analyses

          Since a surrogate analog of  dioxins and furans at each level of
chlorination was spiked into each sample, duplicate matrix spike analyses were
not performed.

5.6       Metals/Method 12

5.6.1      Instrument Calibration and System Performance

          All elements except arsenic were analyzed  by  ICPES.    All  metal
standards were prepared from certified  standards and ACS reagent chemicals.
The  samples were diluted to minimize interferences  from elements such  as  iron
and  aluminum.   In general,  samples were diluted  so  that  iron and aluminum
levels were below 50 ppm.   The reported numbers  from the ICPES  analyses  were
chosen so  as  to minimize  interferences, but at  a level  as  far above the  method
detection  limits as possible.  An  instrumental  detection limit  study was
                                      64

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                               TABLE 5-14.  DIOXIN/FURAN RESULTS
                                 ASH SURROGATE RECOVERIES (X)
Surrogate
Reagent Blank
A710003-3540-BL
   37022
ZSARM 1-2-A ASH
A710003-04A
   37020
ZSARM-II-5-A ASH
A710003-05A
   37021
13C-2,3,7,8-TCDD
13C-2,3,7,8-TCDF
13C-1,2,3,7,8-PCDD
13C-1,2,3,7.8-PCOF
13C-1(2,3,6,7,8-HxCOD
13C-1,2,3,4,7,8-HxCOF
13C-1,2,3,4,6,7,8-HpCDD
13C-1,2,3,4,6,7,8-HpCDF
13C-OCDO
13C-OCDF
     83
     89
     92
     89
     74
     88
     77
     76
     75
     78
   86
   94
   94
   93
   86
   96
   87
   83
   81
   84
   86
   98
   93
   91
   86
   94
   74
   73
   65
   70
                                              65

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                     TABLE 5-15.   DIOXIN/FURAN RESULTS
                       FEED SURROGATE RECOVERIES (%)
Surrogate
Reagent blank
   A710018
    37031
ZSARM 1-2-F
A710003-07-A
   37034
ZSARM-II-5-F
A710003-08A
   37035
13C-2,3,7,8-TCDD
13C-2,3,7,8-TCDF
13C-1,2,3,7,8-PCDD
13C-1,2,3,7,8-PCDF
13C-l,2,3,6,7,8-HxCDD
13C-l,2,3,4,7,8-HxCDF
13C-l,2,3,4,6,7,8-HpCDD
13C-l,2,3,4,6,7,8-HpCDF
13C-OCDD
86
89
89
86
80
78
70
70
61
71
68
95
82
77
76
74
79
58
78
80
91
87
76
92
53
61
50
                                          66

-------
               TABLE 5-16.   DIOXIN/FURAN RESULTS
               SCRUBBER WATER SURROGATE RECOVERIES,  (%)
                         Reagent blank      ZSARM 1-2-S      ZSARM-II-5-S
Surrogate                A710003-blank      A710003-01A      A710003-02A
                            37017              37018            37019

13C-2,3,7,8-TCDD              86               84               88
13C-2,3,7,8-TCDF              91               92               97
13C-1,2,3,7,8-PCDD            91               92               94
13C-1,2,3,7,8-PCDF            91               89               94
13C-l,2,3,6,7,8-HxCDD         89               87               72
13C-l,2,3,4,7,8-HxCDF         91               94              101
13 C-l,2,3,4,6,7,8-HpCDD      85               85               85
13C-l,2,3,4,6,7,8-HpCDF       81               85               82
13C-OCDD                      79               83               76
13C-OCDF                      84               87               84
                                          67

-------
performed and the results are presented in Table 5-17.   Method detection
limits are given in Tables 5-18 (Feed), 5-19 (Ash),  and 5-20 (Scrubber Water)
for each element.  Method detection limit values are given for the undiluted
samples.  It should be noted that most of the samples were diluted before
analysis and to obtain an accurate MDL for each element, the reported MDL must
be multiplied by the sample dilution.

          The arsenic analysis was done by graphite  furnace atomic absorption
spectrophotometry.  A blank and 4 upscale calibration points were used for
each calibration.  Instrumental detection limits are shown in Table 5-17.

5.6.2     Blanks

          Method blanks were analyzed with feed, ash, and scrubber water
samples. No problems were encountered for feed and ash blanks; however, the
method blank for scrubber water contained nickel and copper.  More copper is
present in this method blank than in any of the samples.  This contamination
problem is related to this particular blank.

5.6.3     Interference Check/Control Samples

          Interference check samples were analyzed at least twice per day
analysis day to  insure that there were no interference problems.   An
independent control sample was analyzed after the calibration and after every
ten samples, water blanks were analyzed after every ten samples, and standard
additions were made and analyzed for 10% of the samples.  For a given
analysis, all quality control was within 10% and all interference check
samples were within 20% or the analysis was redone.   Recoveries of 80 to 120%
were obtained for all standard additions.  For AAS analysis an independent
control sample was analyzed with the calibration standards and after 10 to  15
samples, and after the last sample of a given analysis run.   If the control
sample was not within 20% of the reported value, the samples were reanalyzed.
                                      68

-------
TABLE   5-17

259.94
Fe
Day 1 Resul t s 0 .039
0.042
0.036
0.043
0.045
0.045
0.046
Mf-1 0.003
Day 3 Results 0 .039
0.041
0.039
0.038
cr> 0.042
vo
0.039
0.040
"n-\ 0.0014
Day 5 Results 0.039
0.038
0.038
0.040
0.039
0.039
0.036
*-1 0.013
mean Tn- 1 )x3 0.002
= HDL 0.006
Alt. Method - 0.009
= S = = = = 3 = SEK = = = = = S = SS =

H
396. 1

0
0
0
0
0
0
0
0
0
0
0
0
0
0
-0
0
0
0
0
0
0
0
0
0
0
0
0
= a a s, =
A1
.06
.09
.03
.04
.07
.05
Toi
.03
.06
.03
.02
.04
.05
.01
.01
.024
.01
.01
.04
.03
.06
.05
.05
.02
.03
.09
.14
= s & =
i n i mum
5 1






0
1
0
1
1
1
1
1
1
1
0





0
1
0
0
0
0
======
Detection
97.20
AS
.097
.110
.059
.048
.069
.995
.206
.066
.119
.028
.060
. 141
.014
.084
.153
.055
.047
.084
.053
.065
.100
.981
.063
.038
.053
. 159
.231
Limits
205.55

0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
= =  = = =
Cr
.038
.039
.044
.043
.052
.033
.046
.006
.044
.043
.043
.049
.039
.043
.042
.003
.044
.032
.048
.045
.044
.033
.050
.007
.005
.015
.012
for
2

0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
z = = = s
Metals
13.86
Zn
.022
.019
.021
.019
.024
.018
.019
.002
.015
.016
.015
.017
.017
.018
.014
.0014
.014
.015
.015
.018
.014
.015
.016
.0014
.002
.006
.005
= = = = = = =
By I
CPES/
220.35

0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Pb
.708
.710
.678
.732
.759
.771
.735
.032
.699
.724
.704
.765
.688
.736
.690
.028
.706
.684
.668
.309
.725
.753
.674
. 151
.070
.210
.151
= =  = ~
G r aph i t
e AA
226.50


231 .60
Cd
0.
0.
0.
0.
0.
0 .
0 .
0.
0.
0.
0.
0.
0.
0.
0.
0.
0 .
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
040
039
040
038
038
038
037
001
043
041
044
040
039
041
042
002
037
044
039
041
040
036
041
003
002
006
010
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
N i
. 137
.132
. 124
.130
.121
.122
.123
. 006
. 33
. 35
. 34
. 40
. 33
. 34
. 35
.0024
. 37
. 35
. 28
. 42
. 32
. 30
. 32
.005
.005
.015
.030


327.40

0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Cu
. 179
. 181
. 188
. 179
.170
.170
. 178
.006
. 148
. 162
. 153
. 139
. 138
. 153
.151
.008
. 186
.193
.203
. 199
.197
.204
. 193
.006
. 007
.021
.047

-------
                                                     TABLE 5-17 CONTINUED


                                                         AA-MDL FOR AS
Day 1          .0058                           Day  2       .0063                         Day 3         .0048
               .0047                                        .0055                                       .0044
               .0054                                        .0050                                       .0048
               .0047                                        .0050                                       .0036
               .0047                                        .0055                                       .0040
               .0050                                        .0050                                       .0044
               .0039                                        .0046                                       .0050
         n-l  .0006                                        .0006                                       .0005
mean n-l .006 method Detection Limit = 3 x X n-l = .0018
                                  Alternate Method = .0023

-------
Table 5-18.  DUPLICATE MATRIX SPIKE RECOVEREIS FOR METALS IN FEED
,*nalyte (Analysis
! I Type
1
i 1
'|
'Arsenic GF AAS
-cm urn | I CAP
I
1
2-nc 1CAP
i
Lcaa | I CAP
i i
1
jTijin [ [CAP
I
1
| Nickel | ICAP
; |
i 1
1 opper | ICAP
1 1
Method
Detection
Limit
(ug/g) *
0.040
0.300
0.120
4.200
0.120
0.300
0.420
Sample used | Amount
for Spikes [ Spiked
P7-09-023-19a j in
(ug/g) | ug/g
=a=ssss=====ss i =s = s=ss=s
16.9 | 20.0
|
I
24.2 | 100.0
i
I
451 | 800.0
i
I
261 | 300.0
I
1
26.3 | 100.0
i
1
27.5 | 100.0
i
I
244 | 600.0
I
Matrix Spike
P7-09-023-25a
(ug/g)
28.8
115
1200
543
118
117
804
Matrix Spike j Matrix Spike
Recovery | Duplicate
P7-09-023-25a |P7-09-023-26a
(X recovery) j (ug/g)
ssaaisxssssssss I sssssxssssss==
78X| 30.3
93X| 121
i
1
96X| 1280
I
I
97X| 587
j
93X| 121
i
1
92X| 120
I
1
95X| 836
1
MS Dupl icate | Relative |
Recovery j Percent |
P7-09-023-26a (Difference]
(X recovery) | (a) j
82% | 5X|
i i
1 1
977. | 5X|
i |
1 1
1 02% | 6% |
i i
1 I
105X| 8% |
i i
I I
OAV I V/ f
TO/. | I
I I
I I
94X| 3Xf
| 1
1 1
99X| 4%|
1 1
"'I = Metfiod Detection Limit
   summg 5 g samples in 100  mL  total  volune.
    ;elative Percent  Difference  * (MS  -  MSD)/(0.5*(MSMS  +  MSD).
                                                                 71

-------
Table 5-19.   DUPLICATE  MATRIX  SPIKE  RECOVERIES  FOR METALS  IN ASH
|Analyte |Analysis| Method
1 I Type
! 1
! 1
1 	 1 	
(Arsenic | GF AAS
1 1
'Chromium] ICAP
1
Zinc
.000
C riCllii 1 UfTl
Nickel
1 Copper
ICAP
ICAP
!CAP
ICAP
ICAP
Detection
Limit
(ug/g) *
	
0.040

0.300

0.120
4.200
0.120
0.300
0.42C
Sample used
for Spikes
P7-09-023-10a
(ug/g)
37.7

(a) 9.8

217
56.2
< 1.48
11.8
111
Amount
Spiked
in
ug/g
20.0

100.0

1000.0
600.0
100.0
100.0
500.0
Matrix Spike

P7-09-023-168
(ug/mL)
55.9

101

1130
610
87.7
102
604
Matrix Spike | Matrix Spike
Recovery | Duplicate
P7-09-023-16a |P7-09-023-17a
(X recovery) | (ug/mL)
97X| 61.5
I
92X| 101
I
93X| 1170
i
I
93% | 604
I
1
88% | 87.6
i
91X| 103
i
I
99X| 585
I
MS Duplicate | Relative
Recovery | Percent |
P7-09-023-17a |Difference|
(X recovery) | (b) |
107X| 10X|
I I
92% | OX |
I I
96% | 3% |
i i
I I
92% | r/.|
I I
I I
33% | OX |
i i
I I
92% | IX |
i i
1 1
96% | 3%|
1 1
MDL - Method Detection Limit
" assuming 5 g samples in  100  mL  total  volume.
(u) Amount shown is  a  default  value,  but  agrees  with  the  amount  found
    in the undiluted sample.

-------
'able 5-20.  DUPLICATE MATRIX SPIKE RECOVERIES FOR METALS IN SCRUBBER WATER
Mnaiyte (Analysis) Method
| Type [Detection
| | Limit
| j (ug/mD*
= = == = = = = I = = = = = = = == = = = = = = = = =
'Arsenic | GF AAS | 0.001
i i
I I
,-on-ium! ICAP | 0.008
: i
I I
Zinc ICAP | 0.003
! 1
I I
.oaa | ICAP | 0.105
i l l
1 1
.C'.ium 1 ICAP | 0.003
i i
i 1
l Nickel | ICAP | 0.015
1
1
csper ICAP | 0.011
I I
[Sample used | Amount
[for Spikes | Spiked
[P7-09-023-01
j Cug/mD
!============
j 0.150
i
I
| 0.530
| 2.14
i
I
|(a) 1.75
i
I
j 2.35
in
ug/mL
========
0.500
2.500
7.500
7.500
15.000
i |
I I
| 0.320 | 2.500
I i
\
|(a) 0.595
1
3.750
| Matrix Spike
I
|P7-09-023-07a
j (ug/mL)
=j======:=r=====
| 0.700
1
1
| 3.60
1
1
| 10.9
I
I
| 9.51
1
1
| 19.3
l
1
| 2.96
| 4.32
1
Matrix Spike |
Recovery |
Matrix Spike
Duplicate
P7-09-023-07a |P7-09-023-08a
(X recovery) |
sssssssassssss f
108XJ
i
I
119X|
I
113X|
I
86X|
I
I
111%)

I
105X|
I
I
I
(ug/mD
=====:====::==;
0.760
3.39
11.1
9.83
18.6


2.93
4.26
[ MS Oupl icate |
| Recovery |
Relative |
Percent |
|P7-09-023-08a (Difference!
| (X recovery) |
|  |
1 117*1
1 i
1 1
1 112X|
i i
1 !
I
1
| 89V. ;
I
1
| 107*/.
I
1
| 104V.!
|
I
| 86%
I I
(b) [
========== I
8V. |
I
I
6V. |
i
]
2V. |
j
3V. |
i
I
i
l
|
2V. |
I
""L = Method Detection Limit
    Amount  snown is  a default  value,  but agrees with the amount found
    .n the  undiluted sample.
(D) Relative Percent Difference * (MS   MSD)/(0.5*(MS  MSD).
                                                                     73

-------
5.6.4     Duplicate Matrix Analysis

          A matrix spike and a matrix spike duplicate were prepared for feed,
ash, scrubber water, and Method 12 metal samples.  The matrix spike/matrix
spike duplicate recoveries and relative percent difference are given in Tables
5-18 (Feed), 5-19 (Ash), 5-20 (Scrubber Water), and 5-21 (Method 12). The
maximum relative percent difference for all samples was 10 percent.
                                        74

-------
Table 5-21.  DUPLICATE MATRIX SPIKE RECOVERIES FOR METHOD  12 METALS
METHOD 12 TRAIN SAMPLES
=========
| Analyte
i
!
i
I
|Arsenic
i
Chromium
Zinc
I
i
| Lead
1
j Caflmi urn
i
| Nickel
i
| Copper
1
Analysis
Type


GF AAS

I CAP
ICAP

[CAP

ICAP
ICAP
ICAP
Method
Detection
Limit
(ug) *
0.200

1.50
0.600

21.0

0.600
1.50
2.10
Amount
Spiked
in
ug
10.0

500.0
1000.0

500.0

500.0
500.0
500.0
= = = = = = =;=;= = = = = = = .
Method Spike


(total ug)
9.50

448
868

435

441
441
476
 = = = =;== s 5= ==s= ..
Method Spike
Recovery

(X recovery)
95%

90X
87X

en

887.
sax
95%
==S===S=E======.
Method Spike
Duplicate

(total ug)
9.80

439
857

434

435
434
463
E==Z====7=====Sv=======55
MS Duplicate Relative |
Recovery | Percent |
]Dif f erencej
(X recovery) j (a) |
98X| 3X|
I I
88XJ 2%|
i
1
86X| IX |
1
87X| OX|
I |
87%) 2% I
i i
1 1
87% | 2X|
i
1
93% | 3%|
1
MDL = Method Detection Limit
" assuming 100 mL  total  volume.
,a) Relative Percent  Difference  = (MS    MSD)/(0.5*
-------
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Seal Intact? Seal No. Seal Intact?






Condition
(damaged, loss of liquid, etc.)







\JoA




.






-------
                              SAMPLE SHIPPING/RECEIVING RECORD
            OF
                                                                         PM
                                                                                - 7
    2. SENDER
                               3. CARRIER
                                 Sigruturc
                                 n.t.     t?//f/&7
                                 B/L No.,
                            4. RECEIVER
                            Courier from Depot

                            Signature _____.
                            Date	
                                                            LAB CUSTODIAN
                                                                    /   I
                                                               Condition upon,
   5.  SHIPMENT DESCRIPTION

Number of Packages.

Sealed (yes or no)

Types
   Condition prior to Shipment.
                              O A/4
                                               Seal No.
                                                      Seal Intact?
                                    Seal No.
                                  Seal Intact?
   6. CONTENTS
      Sample I.D. No.
                      Type of
                      Sample
  Sealed
(yes or no)
Seal No.
 if any
        Condition
(damaged, loss of liquid, etc.)
                                                          M&fl
X
                       sfr*&
      ~ -a-*-*'*/***-
                                            fJ73
                                              $376
                                                         M

-------
                                      PEI ASSOCIATES, INC.
                              SAMPLE SHIPPING/RECEIVING RECORD
   2. SENDER
Signatu

n.t.  Q/^/f
             i
3. CARRIER

Company &1&2_,
                                 Signature
                                 B/L
               4.  RECEIVER
               Courier from Depot

               Signature ______
                                                                Condition upon

                                                                   "  t.

   5.  SHIPMENT DESCRIPTION
          of Packages

   Sealed (yes or no) 
        of
   Condition prior to Shipment.
                                                Seal No.
                                                       Seal Intact?
                                      Seal No.
                                  Seal Intact?
   6. CONTENTS
      Sample 1.0. No.
                      Type of
                      Sample
    Sealed
  (yes or no)
Seal No.
 if any
        Condition
(damaged, loss of liquid, etc.)
-
                                                S?/Z~ -L   N?Qft
                                                                        -"^***-<
\

-------
                 APPENDIX D



STACK GAS SAMPLING AND ANALYTICAL PROCEDURES
                     D-l

-------
     DETERMINATION OF PARTICULATE,  SEMIVOLATILE  POHC,  AND  HCL  EMISSIONS


     The following procedures are used to measure  particulate, semivolatile

organic, and HC1  emissions.   The sampling train  is a modified  Method  5 sam-

pling train as described in  Method  S008.*


SAMPLING APPARATUS

     The sampling train, which is shown in Figure  D-l, consists of the

following:

     Nozzle - Stainless steel (316) with sharp,  tapered leading edge  and
     accurately measured round opening.

     Probe - Borosilicate glass with a heating system  capable  of maintaining
     a minimum gas temperature of 250F at the exit end during sampling.

     Impingers - Five impingers are connected in series with glass ball
     joints.  The third, fourth, and fifth impingers are of the Greenburg-
     Smith design, modified  by replacing the tip with  a i-in.-i.d. glass tube
     extending to i in. from the bottom of the flask.   The first impinger is
     a 500 ml collection jar attached to the XAD-2 trap.

     XAD-2 Resin Module - Pyrex glass with a resin capacity of approximately
     25 g of XAD-2 with a glass frit on the outlet end and glass wool packed
     at the inlet end.

     Metering System - Vacuum gauge, leak-free pump,  thermometers capable of
     measuring temperature to within 5F, dry gas meter with 2 percent accu-
     racy, and related equipment to maintain an isokinetic sampling rate and
     to determine sample volume.  The dry gas meter is made by Rockwell, and
     the fiber vane pump is  made by Gast.

     Barometer - Aneroid barometer capable of measuring atmospheric pressures
     to 0.1 in.Hg.

     Recirculation Pump - Thomas submersible water pump to cool sample gas
     prior to resin module.

     Pi tot Tube  - A Type S pi tot tube, which meets all geometric standards,
     attached to measure stack gas velocity pressure.

     Temperature Gauge  - A Chrome1/Alumel Type  K  thermocouple  (or equivalent)
     attached to the probe to monitor  stack gas temperature within 1C  (2F)
     by the  use  of a digital  readout.
   Sampling  and Analysis Methods for Hazardous Waste Combustion.  EPA-600/8-
   84-002.   February  1984.
                                     D-2

-------
a
 i
CO
                                                                                     1.9-2.5 cm
                                                                                     (0.75 -1 in.)
                          1.8 cm (0.75
                                                                                               j
                                                                                         1h.) - f
                                                             4	THERMOCOUPLE
                                                               	PROBE

                                                               	PITOT TUBE
                                     HEATED AREA
   FILTER HOLDER
         NOZZLE
     S-TYPE
      PITOT
      TUBE
     THERMOCOUPLE
                                                                       SORBENT
                                                                         TRAP
                                                                   THERMOMETER
r<

ii

_ 	 _.
<

 	 ~
i
WRINGERS
	 	 ~
. 	 .*
^

                            TEMPERATURE
                              NDICATOR
RECIRCULATION
    PUMP
          THERMOMETER
                                                                                             ICE WATER BATH'
                                                                                                BY-PASS
                                                                                                 VALVE
             IUPIMGER COMTEMTS

            1. EMPTY

            2. EMPTY

            3. 100rrt0.1NNaOH

            4. 100ml0.1Nh4aOH

            5. SUCAGEL
                                                                                                      <	iSF-
                                                                         VACUUM
                                                                           LINE
                                                           VACUUM GAUGE
                                                                                                          MAIN VALVE
                                                                                              VACUUM PUMP
                                                Figure D-1.  Modified Method 5 sampling train.

-------
     Filter - A glass-fiber filter placed between the probe  and  resin  module
     to remove any particulate in the sample gas.
EQUIPMENT PREPARATION
     The probe, impingers, and all glassware used during the sampling  and
recovery are prepared according to procedures described in the Manual  of
Analytical Methods for Analysis of Pesticides in Human and Environmental
Samples.  These procedures consist of a soapy-water wash, a  distilled-water
rinse followed by a methanol rinse and methylene chloride rinse, and oven
drying.  After drying, all open areas of each component are  sealed with
aluminum foil to prevent contamination.
     The XAD-2 resin is purchased in a precleaned state; i.e., the resin has
been prepared according to EPA Level 1 specifications.*  This cleanup  in-
volves two washings with distilled water and two soxhlet extractions with
methylene chloride and methanol.   After an acceptable blank level  is  ob-
tained, the XAD-2 resin is stored in methylene chloride in an amber glass
bottle until just prior to use.  Approximately 1 week before the test, the
resin is dried and packed into the glass sorbent module.  The module is
capped with glass caps and wrapped in aluminum foil to protect the resin from
light.
SAMPLING PROCEDURE
     Samples are collected isokinetically according to the procedures  of EPA
Method 5.*  Sample train components are assembled in the sample preparation
  IERL-RTP, Procedures Manual:  Level 1 Environmental Assessments.  EPA-
  600/7-78-201.  October 1978.
                                     D-4

-------
area, as shown in Figure D-l.  The first impinger (condensate jar) and second
impinger were initially empty.  The third and fourth impingers were each
charged with 100 ml of 0.1 NaOH solution for HC1  collection.   The fifth
impinger was filled with silica gel.   Each impinger was weighed prior to
assembly so that the total moisture collected could be determined.  The
sampling train was leak checked at the sampling site prior to each test run
by plugging the inlet to the nozzle and pulling a 15-in.Hg vacuum, and at the
conclusion of the test by plugging the inlet to the nozzle and pulling a
vacuum equal to the highest vacuum reached during the test run.
     During sampling, crushed ice was placed around the impingers, and co-
oling water was circulated through the condenser coil to maintain the XAD-2
module inlet temperature at 68F or less.  Stack gas and sampling train data
were recorded at each traverse point and whenever significant changes are
observed in stack flow conditions.  Isokinetic sampling rates were set through-
out the sampling period with the aid of a programmable calculator.
SAMPLE RECOVERY PROCEDURES
     At the completion of the test, the sample was capped and transported to
the sample recovery area.  Figure D-2 is a schematic of the sample recovery
procedures.  The samples are recovered as follows:
     Container No.  1 - The particulate filter is removed and placed in a
     glass petri dish.
     Container No.  2 - The nozzle, probe, and connecting glassware between
     the probe and  filter were rinsed with methylene chloride.   A nylon brush
     is used to ensure complete removal of particulate matter.   Amber glass
     jars with Teflon-lined caps are used to recover the rinse.
  40 CFR 60, Appendix A, Reference Method 5.   July 1, 1987.
                                     D-5

-------
                            GLASS
                            FILTER
                        CAP OFF WRAP
                        3
                PROBE
                 AND
                NOZZLE
                  BRUSH AND
                    RINSE
o
en
                                                           IN FOIL
                                      100 ml
                                      0.1 N
                                       NaOH
                  100 ml
                  0.1 N
                   NaOH
                              GLASS DISH
                                           RINSE
                                            WITH
                                         METHYLENE
                                          CHLORIDE
                              WEIGH
                            CONTENTS

                                \
                            TRANSFER
           I
         WEIGH
        CONTENTS
            300 g
           SILICA
            GEL
                                                                               WEIGH
                                                                              CONTENTS
              WEIGH AND
               DISCARD
                                                   T
                                        I
          2. METHYLENE T"T
             CHLORIDE
u
                  AMBER GLASS
                   CONTAINER
                  AMBER GLASS
                   CONTAINER
                              0
 100ml
 AMBER
 GLASS
CONTAINER
                                                RINSE  WITH
                                             DISTILLED WATER
   1  liter
POLYETHYLENE
  CONTAINER
                      Figure D-2.  Recovery procedure Modified Method 5 sampling train.

-------
     Container No. 3 - The XAD-2 sorbent trap was removed from the train,
     capped with glass ball-joint caps, and wrapped in aluminum foil.   The
     sorbent trap was stored on ice until returned to the laboratory.

     Container No. 4 - After it was weighed, the condensate collected  in the
     first impinger was transferred to a 100-ml amber glass jar.

     Container No. 5 - The connecting glassware between the filter and the
     sorbent module and the first impinger is rinsed with methylene chloride
     and the rinse is stored in an amber glass jar.

     Container No. 6 - After each impinger was weighed, the NaOH  solution  was
     recovered into a polyethylene container.  Each impinger was  rinsed wit
     distilled water, and the rinse was added to the same container.

     Container No. 7 - At least 200 ml of methylene chloride was  collected in
     an amber glass jar for particulate blank analysis.

     Container No. 8 - One unused filter was labeled for particulate  blank
     analysis.

     Container No. 9 - With each set of samples, one unused XAD-2 sorbent
     trap was labeled for blank organic analysis.

     Container No. 10 - With each set of samples, one 100-ml portion  of
     methylene chloride was collected in an amber glass jar for blank  organic
     analysis.

     Container No. 11 - With each set of samples, 200-ml  portions of  NaOH
     solution was collected for blank HC1  analysis.

     The silica gel  impinger is weighed and the silica gel  is discarded.


ANALYTICAL PROCEDURES

     All analyses for the project were performed by Radian  Corporation.  See

Appendix C for methods and procedures.
                                     D-7

-------
                  DETERMINATION OF VOLATILE POHC EMISSIONS


VOLATILE ORGANIC SAMPLING TRAIN (VOST) PROTOCOL

Sampling Apparatus

     The sampling train, which was assembled by PEI personnel,  meets the gen-

eral design specifications of Method S012* and the VOST Protocol.**

     The sampling train is shown in Figure D-3.  It consists of:

     Probe - Stainless steel  sheath and glass liner with a heating system
     capable of maintaining an exit-end gas temperature of 130C  (266F).

     Particulate Filter - A plug of glass wool placed in the front of the
     probe.

     Four-way Valve - Stainless steel or Teflon four-way valve.

     Condensers - Glass coil  condensers with water jacket to cool  the sample
     gas stream to 20C (68F) or less before it enters the first  sorbent
     trap.

     Sorbent Traps - Borosilicate glass with dimensions of 1.6-cm  (0.63-in.)
     o.d. by 12.7 cm (5 in.)  with both ends necked down to 6.3-mm  (i-in.)
     o.d.  Traps are shown in Figure D-4.  The first trap contains a minimum
     of 1.6 g of Tenax TC and the second contains a minimum of  1 g of Tenax
     TC and 1 g of activated  charcoal.

     Flask - Borosilicate glass with 250-ml volume and screw cap bored to
     accept 6.3-mm (i-in.) o.d. tubing.  Teflon-backed silicone gaskets are
     used to make a leak-free seal.

     Drying Tube - Teflon container holding approximately 100 g of silica
     gel.

     Metering System - Vacuum gauges, leak-free diaphragm pump, calibrated
     rotameter, singer dry-gas meter measuring 1 liter/revolution  with 2
     percent accuracy for flow rates between 0.25 and 1.0 liter/min.
   Sampling and Analysis Methods for Hazardous Waste Combustion.  EPA-600/
   8-84-002.  February 1984.

** Protocol for the Collection and Analysis of Volatile POHC's Using VOST.
   EPA-600/8-84-007.  March 1984, as improved by recommendations in Valida-
   tion of the Volatile Organic Sampling Train (VOST) Protocol, Field Valida-
   tion Phase, EPA 600/S4-80-014.  April 1986.
                                     D-8

-------
                                                                               i    -i
                                GLASS
                                WOOL
                                PLUG
                                 V
 HEATED. TEFLON OR
CLASS-LINED SS PROBE
                          4-WAY. SS
                        OR TEFLON VALVE
                                          10 LEAK CHECH APPARATUS
                                                 TO PURGE SYSTEM

                                                        TO
                                                       PR08E
                                 STACK
                                  GAS
                                 FLOW
O
I
                                                                 DIGITAL
                                                               TEMPERATURE
                                                                INDICATOR
                                                                 SCREW CAP
                                                                   WITH
                                                                TEFLON-BACKED
                                                                  GASKtT
                                             Figure D-3.    Schematic  of  volatile organic  sampling train  (VOST).

-------
                                   TRAP
                                   I.D.
                                 NUMBER-
o
i
   1.6 g OF TENAX
                                           db
                                                  GLASS WOOL
1/4 In. SWAGELOK 316-SS
NUT AND CAP
(SUPELTEX M-l  FERRULES)
                                                       1.0 g TENAX
                                                                                                        1.0 g CHARCOAL
                                                    GLASS WOOL
                                                                                                     1/4 In. SWAGELOK 316-SS
                                                                                                     NUT AND CAP
                                                                                                     (SUPELTEX M-1  FERRULES)
                                                 Figure D-4.    Sorbent trap configurations.

-------
Trap Blank Check Apparatus

     Thermal Desorptlon Um't - Modified Supelco high-capacity gas purifier
     oven.A temperature controller was used to control  oven temperature and
     a thermocouple was used to monitor it.

     Purge and Trap Unit - Tekmar Model LSC-2 with all  Teflon transfer lines
     replaced with 1.6-mm (1/16-in.) o.d.  stainless steel  tubing.  The ana-
     lytical trap consisted of a 15-cm-long  section of Tenax, 3.7-cm section
     of silica gel, and a 3.7-cm section of  charcoal.

     Analyzer - Perkin Elmer Model 990 gas chromatograph  with a flame ioniza-
     tion detector (GC/FID).  The GC column  is a 6 ft  x 1/8 in. o.d. stain-
     less steel column packed with 1 percent SP-1000 on Carbopak B.

Analytical Apparatus

     The analytical system used in these tests is in accordance with Method

S012 and the VOST Protocol.

     Thermal Desorption Unit - Modified Supelco high-capacity, gas-puri.fier
     oven ("clamshell" oven).  A temperature controller was used to control
     oven temperature, and a thermocouple  was used to  monitor it.

     Purge and Trap Unit - Tekmar Model LSC-2 with all  Teflon transfer lines
     replaced with 1.6-mm (1/16-in.) o.d.  stainless steel  tubing.  The ana-
     lytical trap consisted of a 15-cm long  section of Tenax, 3.7-cm section
     of silica gel, and 3.7-cm section of  charcoal.

     GC/MS System - Finnigan Model 4023 with quadrupole mass spectrometer.
     The separation column is 1.848-m (6-ft) by 2-mm i.d.  glass, packed with
     1 percent SP-1000 on Carbopak B (60/80  mesh).  The mass spectrometer
     scans from 35 to 335 m/e every 2 seconds when methanolic standards are
     used, and from 20 to 335 m/e when gaseous standards  are used.   The GC/MS
     interface is an all-glass jet separator.  The data acquisition and
     processing system that controls the mass spectrometer consists of a Data
     General Nova 3 computer with Perkin-Elmer/Wangco  10  mega-byte dual-disk
     drive running Finnigan Incos software.

Reagent and Materials Preparation

     Tenax - 2,6-Diphenylene oxide polymer (35/60 mesh) Soxhlet extracted for
     24 hours with glass-distilled methanol  (Burdick and  Jackson pesticide
     residue grade or equivalent).  After  extraction,  the Tenax was trans-
     ferred to a clean ceramic evaporating dish and dried for 4 hours under
     an infrared lamp.  The Tenax and evaporating dish were then placed in a
     vacuum oven at 50C and 20 in.Hg vacuum for 6 hours  to complete drying.
     Finally, the Tenax was transferred to a clean amber  glass bottle with a
     Teflon-lined screw cap and placed in  a  glass aquarium containing acti-
     vated charcoal.
                                     D-ll

-------
Charcoal  - Petroleum-based charcoal  (SKC Lot 208,  Calgon-Type 6W20X50,
or equivalent) was prepared by heating to 190C in a vacuum oven under  a
slow nitrogen purge according to the following procedures:

1}   Charcoal was placed in a cylindrical metal container opened at the
     top and connected to a source of charcoal-filtered nitrogen at the
     bottom.

2)   Nitrogen purge flow was set at 50 ml/min.

3)   The charcoal and metal container were placed  in a vacuum oven set
     at 190C and approximately 5 in.Hg vacuum for 6 hours.

Glassware and Teflon Parts - All glass parts (traps, culture tubes,
flasks, and condensers), Teflon fittings, and sample-exposed connecting
lines were cleaned with a nonionic detergent (Alcojet) and rinsed thor-
oughly with charcoal-filtered deionized water.  The parts were then
oven-dried at 110C for 8 hours.  All parts were then wrapped in alumi-
num foil  and stored in sealed glass aquariums containing activated
charcoal.

Metal Parts - Sorbent trap end-plugs and stainless steel unions (used to
connect the traps to the sampling train) were ultrasom'cally cleaned for
15 minutes in a hot nonionic detergent solution, then rinsed with char-
coal-filtered deionized water, air-dried, and finally heated in a muffle
furnace at 400C for 2 hours.  Cleaned parts were  stored in amber glass
bottles, which were placed in sealed glass aquariums containing acti-
vated charcoal.

Glass Wool - Pyrex wool filtering fiber was Soxhlet-extracted for 16
hours with glass-distilled methanol, placed in a clean ceramic evaporat-
ing dish, and dried under an infrared lamp in an exhaust hood for 4
hours.  The glass wool and dish were then placed in a vacuum oven and
heated at 110C and 20 in.Hg vacuum for 6 hours.  The cleaned glass wool
was then stored in amber glass bottles with Teflon-lined screw caps
until it was used.

Water - Charcoal-filtered, deionized water was used for trap leak check-
ing prior to blank analysis.  Water used for analytical steps was fur-
ther treated by boiling for 15 minutes.

Nitrogen - For purging sorbent traps during thermal conditioning, nitro-
gen was passed through an inline gas purifier containing 5A molecular
sieve and activated charcoal.  The charcoal bed was replaced with each
new nitrogen cylinder.

Analytical Trap - The analytical trap consisted of the following compo-
nents!Tenax (60/80 mesh), chromatographic grade or equivalent; silica
gel, Davison Chemical (35/CU mesh), Grade 15 or equivalent; charcoal,
petroleum-based (SKC Lot 104 or 208, Calgon Type GW20X50,  or equiva-
lent).
                                D-12

-------
     Stock Standard Solution - The stock standard solutions were prepared
     weekly from pure standard material  by diluting with glass-distilled
     methanol.
     Bromofluorobenzene (BFB) Tuning Check Standard - A solution of 50 ug/ml
     BFB in methanol  was prepared and 1  yl of this standard was injected  on
     column each day for the MS tuning check.
     Internal  Standard - A known concentration of D6-Benzene and hexafluoro-
     benzene was prepared in methanol, such that a 4-yl on-trap injection
     produced an amount on column in the range of the amount of the target
     compounds.
Assembly and Conditioning of VQST Sorbent Traps
     Sorbents are loaded into the glass  tube by use of a modified rifle shell
loader.  Tenax tubes are loaded with 1.6 grams of Tenax, and Tenax/charcoal
tubes are loaded with 1.0 gram of each sorbent.  A small section of Teflon
tubing is used to help transfer the sorbent from the loader into the sorbent
tube.  Sorbent beds are held in placed by glass wool plugs.  Sorbent tube
ends are sealed with a Swagelok stainless steel cap and Supeltex M-l ferrule.
Each sorbent trap has a unique numeric code etched on the glass.  Each assembled
sorbent tube is stored in a clean glass  culture tube with a Teflon-lined
screw cap.  All culture tubes are stored in sealed glass aquariums containing
activated charcoal.
     Once assembled, the sorbent traps are conditioned by passing nitrogen
(30 ml/min) through the trap for 28 hours.  Traps are heated in an oven at
190C during conditioning.  After conditioning the traps are returned to a
culture tube and stored in a friction-top metal container, which also con-
tains activated charcoal.  Both the culture tubes and the metal can are
purged with nitrogen to remove air contaminants before the traps are placed
into them.
                                     D-13

-------
Blank Checking Procedure

     Each set of traps is blank checked to ensure that the tubes  contained

less than 5 ng of the target compounds or any other contaminant.   The target

compounds include the designated POHC's and acetone, benzene,  and hexane.

     The following procedures are used to blank-check each pair of sorbent

traps:

     1)   A pair of traps is connected with the charcoal  side  of the Ten-
          ax/charcoal tube connected to the inlet carrier gas.  The traps  are
          connected by stainless steel unions.

     2)   With the outlet of the paired traps (Tenax tube sampling inlet)
          still capped, the system is leak-checked at approximately 30 psig,
          either by immersing the traps in a pan of distilled  water and
          observing the water for bubbles or by checking around the fittings
          with a thermal conductivity gas leak detector (e.g., GOW-MAC ).
          Any leaks are corrected.

     3)   The outlet of the paired traps is connected to the Tekmar purge  and
          trap system.  The traps are then placed in the oven  and desorbed
          for 10 minutes.

     4)   After desorption, the sample collected in the purge  and trap
          apparatus is injected into the GC.

     5)   To minimize contamination, carrier gas flow is maintained at all
          times and traps are disconnected by the following procedure:

          a)   After cooling, the outlet of the paired traps is capped.

          b)   The union between the traps is disconnected and both ends are
               capped.

          c)   The outlet of the Tenax/charcoal tube is disconnected and
               capped.

     6)   Traps are  immediately placed back in their respective culture
          tubes, which are taped together to  keep the paired traps as a unit.

Sample Collection Procedure

     The VOST  train  is assembled at the exit  stack, as shown  in Figure D-3.

During sample  collection, the end caps of the sorbent traps are placed back

into  the culture tubes  in which the traps were stored.
                                     D-14

-------
     The heated glass probe is leak-checked at the beginning of each test day
by connecting a vacuum gauge, a shutoff valve, and a charcoal  tube device to
the inlet of the probe.  The four-way valve is turned to the leak-check/
probe-purge position and a 250-mmHg vacuum is pulled by use of a probe purge
pump (Figure D-5).  Any leak rate in excess of 2.5 mmHg/min in the vacuum
gauge is unacceptable.  At the completion of the leak check, the valve or the
probe leak check device is opened to allow charcoal-filtered air to enter the
probe and return pressure to ambient.
     The remainder of the sampling train is leak-checked by turning the four-
way valve to the leak-check/probe-purge setting, closing the control valve on
the leak-check system (Figure 0-6), and pulling a vacuum of at least 250-mmHg
(10 in.Hg) with the sampling pump.
     The control valve on the control module is closed to isolate the traps
and condensers from the pump, and the leak rate is measured.  At the comple-
tion of the leak check, the leak-check system control valve is opened to
allow charcoal-filtered ambient air to enter the train.
     At the completion of the leak check, the probe is positioned at the
desired sampling point in the gas stream; the probe purge pump (Figure D-5)
is activated, and the probe is purged with stack gas for 10 minutes at a rate
of 0.5 liter per minute.
     Immediately prior to the sampling, the dry gas meter volume is recorded
and the time clock is set at zero.  The four-way valve is then turned to the
sample position and the sample pump is started.  Sample flow rate is adjusted
to a constant sampling rate, and sampling is continued until a total volume
of not more than 20 liters is collected.  The sampling run is terminated by
closing the sample pump control valve and turning off the pump.  The final
                                     D-15

-------
*
I
D
I
I
 I
 I
 I
 I
 I
 I
  I
4-WAY
SAMPLE :
VALVE
SILICA
GEL
=3 H
CHAR
CONTROL
VALVE
T
Httxi=
rnAi
                                                                     VENT
                        LEAK-FREE
                          PUMP
Figure D-5.   Probe purge system.
LINE
4-WAY
FROM
VALVE ~*
V4
TEFLON
^~

in.
TUBING




CONTROL
VALVE
[\ 1 ^1
^
[^ ^\

CHARCOAL
TUBE
                                          ATMOSPHERE
   Figure  D-6.   Leak check system.
                                                  D-16

-------
dry gas meter reading is then recorded, and the four-way valve is turned to
the leak-check/purge position.
     The post-test leak check is conducted similarly to the pretest leak
check, but the vacuum is set at the highest vacuum attained during the run.
     The traps are then disconnected, capped, placed in the culture tubes,
sealed, and labeled.  All traps are placed in the culture tubes with point of
entry nearest the screw cap.  The culture tubes are then purged with char-
coal-filtered nitrogen and sealed.  The culture tubes are then placed back
into metal cans.  The metal can is also purged with nitrogen prior to sealing
at the end of the test day.
     At the end of a test run (3 to 6 sorbent samples), any condensate col-
lected in the flask is recovered as follows:   The condensate is poured from
the flask into 7-ml glass vials with Teflon lined septa and screw caps.
Other sizes of vials can be used so that, if possible, two completely full
glass vials are collected (one is a spare).  The volume of any remaining
condensate is measured and this portion is discarded.
     Several  blank sorbent traps are collected during the test series.  The
field blanks  are collected by connecting the sorbent traps to the sampling
train, leak-checking the train, and then disconnecting the traps.  Trip
blanks are traps carried to the field but left sealed in their culture tubes
until  analyzed.   If designated by the project plan, ambient field blanks are
collected by  uncapping a pair of sorbent tubes and laying them near the
sampling site for the amount of time required to assemble a pair of tubes in
the sampling  train, and lab blanks are traps  prepared and blank checked at
the same time as the sample traps, but left stored in the laboratory custody
room until  analyzed with the lot of field samples.
                                     D-17

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     All  samples are transported in an ice-chilled cooler and refrigerated in
the laboratory until analysis.
Analytical  Procedure
     Analysis was performed by Radian Corp.  See Appendix C for methods and
procedures.
                                      D-18

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                      DETERMINATION OF METAL EMISSIONS


     An EPA Reference Method 12 sample train, which  meets  design  specifica-

tions established by the U.S.  Environmental  Protection Agency,  was  used  to

determine emissions of select  metals for this test program.*  This  train was

be assembled by PEI personnel  and consists of the following items:

     Nozzle - Stainless steel  (316) with sharp,  tapered leading edge and
     accurately measured round opening.

     Probe - Borosilicate glass with a heating system capable of maintaining
     a gas temperature of approximately 121C (250F) at the  exit end
     during sampling.

     Pi tot tube - Type-S pitot tube that meets all geometric  standards.   It
     was attached to the probe to monitor stack  gas  velocity.

     Thermocouple - Type-K thermocouple capable  of measuring  stack gas tem-
     peratures within 2 percent.  It was attached to the probe.

     Filter holder - Pyrex glass with heating system capable  of maintaining a
     filter temperature of approximately 121C (250F)

     Draft gauge - An inclined manometer made by Dwyer with a range of 0 to
     10 in. H20.

     Impingers - Four impingers connected in series  with glass  ball joints.
     The second impinger was of the Greenburg-Smith  design.  The first,
     third, and fourth impingers were also of the Greenburg-Smith design, but
     modified by replacing the tip with a i-in.  i.d. glass tube extending to
     i-in. from the bottom of  the flask.

     Metering system - Vacuum  gauge, leak-free pump, thermometers capable of
     measuring temperature to  within 5F, dry gas meter with  2  percent accur-
     acy, and related equipment to maintain an isokinetic  sampling rate and
     to determine sample volume.  The dry gas meter is made by  Rockwell  and
     the fiber vane pump is made by Gast.
  40 CFR 60,  Appendix A,  Reference Method 12,  July 1987.
                                     D-19

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     Barometer - Aneroid type to measure atmospheric pressures  to within  2.5
     mmHg (0.1 in.Hg).

SAMPLING PROCEDURES
     Glass fiber filters* (3-in. diameter)  were desiccated for  at least 24
hours and weighed to the nearest 0.1 mg on  an analytical  balance.  One hun-
dred ml of 0.1 N HNOo was placed in each of the first two impingers;  the
third impinger will initially be empty; and the fourth impinger,  containing
approximately 300 to 400 g of silica gel, was be placed next in series.  The
train will be set up with the probe as shown in Figure D-8.   The  sampling
train was leak checked at the sampling site prior to each test  run by plug-
ging the inlet to the nozzle and pulling a  15-in.Hg vacuum,  and at the con-
clusion of the test by plugging the inlet to the nozzle and  pulling a vacuum
equal to the highest vacuum reached during  the test run.
     The pitot tube and lines were leak checked at the test  site  prior to and
at the conclusion of each test run.  The check was made by blowing into the
impact opening of the pitot tube until 3 or more inches of water  was  recorded
on the manometer and then capping the impact opening and holding  it for 15
seconds to assure it is leak free.  The static pressure side of the pitot
tube was leak checked using the same procedure, except suction  was used to
obtain the S-in.HpO manometer reading.  Crushed ice was placed  around the
impingers to keep the temperature of the gases leaving the last impinger at
20C (68F) or less.
*
  Whatman Reeve Angel 934AH.
                                     D-20

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o
I
ISJ
                                            HEATED AREA


                                   STACK WALL
FILTER HOLDER
                                  THERMOMETER
                     PITOT TUBE
              ICE WATER  BATH

         TOO ml 0.1 N HNO_
                                              THERMOMETER



                                         ORIFICE
                      VACUUM GAUGE
                                                                                                       VACUUM LINE
                                                                       VACUUM PUMP
                                              Figure D-8.   Metals  sampling train.

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     During sampling,  stack gas and sampling train data was recorded at each

sampling point and when significant changes in stack flow conditions occurred.

Isokinetic sampling rates was set throughout the sampling period with the aid

of a programmable calculator.  All  sampling data was recorded on the Parti-

culate Field Data Sheet.

Sample Recovery Procedures

     The sampling train was moved carefully from the test site to the desig-

nated sample recovery site.  Each impinger was weighed after the test to

determine the amount of moisture present.  Sample fractions was recovered as

follows:

     Container No. 1 - The filter was removed from its holder and placed in a
     petri dish, sealed, and labeled.

     Container No. 2 - An unused filter was taken as a blank.

     Container No. 3 - Loose particulate and 0.1 N HN03 washings from all
     sample-exposed surfaces prior to the filter was placed in a polyethylene
     container, which was then be sealed and labeled.  Particulate was removed
     from the probe with the aid of a brush and HN03 rinsing.  The liquid
     level was marked after the container is sealed.

     Container No.. 4 - A minimum of 500 ml of HN03 was taken for the blank
     analysis.  The blank was obtained and treated in a similar manner as the
     HN03 rinse.

     Container No. 5 - 0.1 N HN03 and condensate in the impinger section of
     the sampling train was placed in a polyethylene container.  The impin-
     gers and connecting glassware were rinsed with 0.1 N HN03, and this
     rinse was added to the container.  The container was sealed and labeled,
     and the liquid level was marked.

     The silica gel from the fourth impinger was weighed, and this value was

recorded with other pertinent data on the Sample Recovery and Integrity

Sheet.
                                     D-22

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Metals Analysis
     Analyses for the indicated metals was accomplished by procedures described
in SW846:  Methods 3050 for digestion and preparation of samples and Methods
7060 for arsenic (Atomic ABsorption) and 6010 for the remaining metals (Induc-
tively-Coupled Plasma (ICP) Spectroscopy) (see Appendix C).
                                      D-23

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   DETERMINATION OF CARBON MONOXIDE,  CARBON  DIOXIDE,  AND  OXYGEN  CONTENT  BY
                         CONTINUOUS EMISSION MONITOR

     Carbon monoxide (CO), carbon dioxide (C02),  and  oxygen  (Op) concentra-
tions were measured continuously throughout  the test  periods.  The sampling
procedures were those of EPA Method 10 for CO,  and Method 3A for 02 and  C02-
A schematic of the sampling system is shown  in  Figure D-9.
     The CEM sampling system consisted of a  stainless steel  probe with an
in-stack glass wool particulate filter, a three-way ball  valve at the probe
exit for calibration gas introduction, a stainless steel  condenser for mois-
ture removal, a Teflon sampling line, and a  Teflon diaphragm or  stainless
steel bellow pump to supply the analyzer sampling manifold.   The CO and C02
analyzers are NDIR detectors.  The 02 analyzer is an electrochemical cell
detector.  All analyzers were calibrated at the beginning and end of each
test run with three gas standards in the analytical range and zero nitrogen.
Span and zero checks were be conducted at the midpoint of each test run.
Calibration data were reduced by means of a linear regression analysis, and
the  linear equation was used to quantitate stack gas concentrations.  The
output from the analyzers was continuously recorded on analog-type strip-
chart recorders for a permanent record.
     In conducting these  tests, PEI performed all calibration and quality
assurance  tests required  by the EPA Methods.
     The following is a description of the analyzers that will  be used  and
the  reference method performance specifications.

CARBON MONOXIDE
     A Beckman Model 8501-5CA continuous  nondispersive infrared  (NDIR)  analyz-
er will be used to measure  CO. The following list  compares  the  Beckman  NDIR
                                       D-24

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                                                                            m   s
                                                                         3-WAY
                                                                       BATH  VALVE
                                         DQ
                                                                                   PROBE
                                                           316 SS
                                                         CONDENSER
                                                        IN ICE BATH
                                         CALIBRATION
                                            GASES
ro
ui
       EXCESS VENT

co2
ANALYZER



CO
ANALYZER



2
ANALYZER

r~\
100 ft
TEFLON
SAMPLE
 LINE
                                                                                                IN  STACK
                                                                                                 GLASS
                                                                                              WOOL FILTER
                                                                                                                 STACK SAMPLING
                                                                                                                   LOCATION
                                                                                                                  PLATFORM
                                                                 TEFLON  DIAPHRAGM
                                                                       PUMP
                                  Figure D-9.  CEM Sampling  System for CO, C0, and

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performance parameters with the minimum performance specifications given in
EPA Method 10.
   Parameter

Detector type

Analytical range


Minimum detectable
 ppm

Calibration re-
 quirement

  Linearity
  Precision
  Noise
  Zero drift
  Span drift
  Response time

  Interference ratio
    CO,
    H,0
    EPA Method 10
minimum specification

         NDIR

     0 to 1000 ppm


          20
   Bendix NDIR, manufacturer's
    performance specification

              NDIR

Available ranges:  0 to 50, 250,
 500, and 1000 ppm

0.5 ppm in 0 to 50 range
0, 30, 60, and 90% of   PEI will use Method 10 criteria
 span
     2% of span
     2% of span
     1% of span
     10* of scale
     10% of scale
 30 s to 90% of full
  response

       1000 to 1
       1000 to 1
1% of span
1% of span
0.5% of span
1% for 24 h
1% for 24 h
Electronic response time 0.7 s
 to 90% of scale

40,000 to 1
20,000 to 1
PEI will measure the actual performance of the analyzer on site during

initial setup.


OXYGEN

     A  Data Test Corporation Model 303 zirconia cell detector was used  to

measure oxygen.  The C02 analyzer was an Anarad model NDIR analyzer.  The  02

analyzer was  operated  in the 0  to 25 percent  range and was calibrated with

zero nitrogen and  gas  standards of 8, 15, and 21  percent  oxygen.  The C02

analyzer was  operated  in the 0  to 20 percent  range and calibrated with  gas

standards  at  4, 8, and 16  percent.  The  following is a list  of  EPA  Method  3A

performance  specifications.  The analyzers were  tested on site  to ensure that

all  performance specifications  are met.
                                       D-26

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                       METHOD 3A PERFORMANCE CRITERIA
          Parameter                          Specification
Analyzer type                 Not specified
Range                         So that average stack gas concentration  is  20
                              to 90% of span (4 to 19% for 21% span)
Minimum detectable concen-    2% of span (0.4% 02  or C02 for 21% span)
 tration
Calibration gases             20 to 30%, 50 to 60%, and 80 to 90% of  span
Analyzer calibration error    2% for all  calibration gases
Sensitivity                   Detect 0.5% change  in concentration
Zero and span drift           2% of span  per run
Accuracy                      5% of Method 3 value or 0.2% 02 or C02,  which-
                              ever is greater

PROCESS SAMPLING PROCEDURES (WASTE FEED, ASH, AND  SCRUBBER WATER)
     Basic sample collection procedures followed those described in Sampling
and Analysis Methods for Hazardous Waste Combustion, Arthur D. Little,  Inc.
EPA-600/8-84-002, February 1984.  This reference was added as a revision  to
the 2nd Edition of SW-846.  Analysis followed applicable procedures described
in SW-846.
Waste Feed Sampling
     Feed samples were collected from the screw feed hopper once an hour
during each run and composited into a 5-gallon metal container which was
covered between sampling events.  Samples were collected using disposable
scoops.  Hourly volatile grab samples were taken and placed in appropriate
containers immediately.  The composite was mixed using the scoop, and ali-
quots will be placed in appropriate sample containers for analysis.  Samples
                                      D-27

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were labeled and placed in coolers with vermiculite and ice for shipment to
the laboratory for analysis.
Bottom Ash Samples
     One composite sample of bottom ash was collected during each SARM test
run.  The ash was sampled from the dewatered ash bin after it is removed from
the rotary kiln ash quench box.  This ash is removed continuously by a paddle
wheel and dumped into the dewatered ash bin.  A sample of ash was collected
from this dewatered ash container using disposable scoops once each hour
following the start of each run, and placed in a separate 5-gallon metal
container which was covered between sampling events.  Hourly volatile grabe
samples were taken and placed in appropriate containers immediately.  The
composite was mixed, and from this individual aliqucts was taken and placed
in appropriate sample containers for analysis.
3.2.3  Scrubber Water Samples
     One scrubber blowdown sample was collected uring each test run.  Aliquots
were collected once an hour as the blowdown leaves the recycling chamber and
before it reaches the waste scrubber water storage tank.  Hourly volatile
grab samples were taken and placed in appropriate containers immediately.
The aliquots were composited in a 1-gallon glass container which was covered
between sampling events.  Aliquots of the composite were placed in appro-
priate containers for analysis.  Samples were labeled and then placed in
coolers packed with vermiculite and ice for shipment and analysis.
3.2.4  Sample Identification
     Each sample collected during the incineration testing was assigned a
unique alpha-numeric sampel identification number.  The coded number iden-
tified the facility, whether the sample is SARM I or SARM  II feed, scrubber
                                      D-28

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effluent, or incinerator residue (ash),  and  which  of the  three  replicate  Zink
runs it came from.
               Example Sample ID Number:   ZSARM-I-l-A
     In the example identification number given  above,  the first seven  digits
(ZSARM-I) specify the sample is from the John  Zink incinerator  (Z)  buring
SARM-I.  The next digit (1)  signifies that the sample was taken during  the
first test run.   The last digit signifies the  sampling  location from Figure
3-1 (A refers to the screw feeder).
Sample Containers
     In the determination of organics and metals,  containers can introduce
either positive or negative errors by 1) contributing contaminants  through
leaching or surface desorption, and 2) depleting concentrations through
adsorption.  Therefore, particular attention must be given to the collection
and treatment of a sample prior to its analysis.
Preparation and Handling of Process Sample Containers for Volatile  Organic
  Analysis
     Standard 40-ml, screw-cap, glass VOA  vials with Teflon-faced  silicone
septa were used for both liquid and solid matrices.  The vials  and  septa were
washed with soap and water and rinsed with distilled deionized  water.  After
the vials and septa had been thoroughly cleaned, they were placed in an oven
and dried at 105C for approximately 1 hour.
     During sample collection, liquids and solids were gently  introduced into
the vials to reduce any agitation that might drive off volatile compounds.
  Volatile organics analysis.
                                      D-29

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Liquid scrubber water samples were poured into vials  without introducing any
air bubbles within the vial during the process.  Should bubbling result from
overly aggressive pouring, the sample will be poured  out and the vial  refil-
led.  Each VOA vial was filled until  there was a meniscus higher than  the lip
of the vial.  The screw-top lid with the septum (Teflon side toward the
sample) was then tightened onto the vial.  After the  lid is tightened, the
vial was inverted and tapped to check for air bubbless.  If any air bubbles
were present, the sample was retaken.  Two VOA vials  were filled per sample
location and interval.  The scrubber water was cooled by passing it through a
coil of teflon tubing submerged in a ice-water bath prior to filling the
vial.
     The VOA vials for solid waste feed and ash samples were filled to the
extent possible.  During the filling process, the vials were tapped slightly
to  eliminate as much free  air space as possible.  Two vials were filled  per
sample location and interval.
     The VOA vials were filled and immediately  labeled at the point at which
the sample  was collected.  They were not  filled near a running motor  or  any
type of exhaust system because discharged fumes and vapors  can contaminate
the samples.  The  two vials  from  each  sampling  location were then  placed in
separate  sealed plastic bags  to prevent  cross-contamination between samples.
VOA samples from  SARM  I and  SARM  II were  kept in  separate  coolers  packed with
vermiculite and  plastic-wrapped ice.   Samples of  scrubbed  water  and ash were
kept in  separate  coolers.   Since  VOA  samples  also may  become contaminated by
diffusion  of volatile  organics  into  the  vial  through the  septum during ship-
ment and  storage,  a  VOA  trip blank prepared from  distilled deionized  water
was placed in each cooler containing  the scrubber water throughout the samp-
 ling,  storage,  and shipping process.
                                      D-30

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Preparation and Handling of Process Sample Containers  for Semivolatile
Analysis
     Glass wide-mouth jars with screw-top covers and Teflon liners  were  used
to collect samples for determination of semivolatile organics  compounds.
They were prewashed with soap and water and rinsed with methanol  (or iso-
propanol).
     One gallon of scrubber water and 250-mls of wate feed and ash  were
placed in the glass wide-mouth bottles.  Sample containers were filled
carefully to prevent any portion of the collected sample from  coming in
contact with the sampler's gloves and thereby causing contamination.  Samples
were collected or stored in the presence of exhaust fumes.
Preparation and Handling of Process Sample Containers for Metals Analys.es
     Two 4-ounce and one 1-liter plastic wide mouth jars with  screw top  lids
wre used to contain process samples of waste feed, ash, and scrubber water
for metals analysis.  The containers were prewashed with soap  and water  and
acid rinsed with a non-chromate product such as NoChromix.  After filling,
the aqueous scrubber water samples were acidified with nitric  acid  to a  pH of
less than 2 as a preservation step; the solid waste feed and gas samples were
not acidified.  All containers were labeled and placed in coolers with
vermiculite for shipment to the laboratory.
Preparation and Handling of Process Sample Containers for TCLP Analyses
     Half-gallon wide mouth glass jars with screw top plastic  lids  and Teflon
liners were used to contain process samples of waste feed and  bottom ash for
TCLP analysis.  The containers were precleaned with soap and water followed
by an acid rinse using a non-chromate product such as NoChromix.  The con-
tainers were filled as full as possible to minimize head space losses of
volatiles.  They were labeled and placed in coolers with ice (wrapped in
plastic) for shipment of U.S. EPA.
                                     D-31

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Cleaning and Storage of Lab Glassware
     In the analysis of samples containing contaminants in the parts-per-
million range, the preparation of clean glassware is mandatory.   Failure to
do so can lead to a myriad of problems in the interpretation of the final
chromatograms resulting from extraneous peaks caused by contamination.
Particular care must be taken with glassware such as Soxhlet extractors,
Kuderna-Danish evaporative concentrators, sampling-train components, or any
other glassware coming in contact with an extract that will be evaporated to
a lesser volume.  The process of concentrating the compounds of interest in
this operation may similarly concentrate the contaminant and thereby seri-
ously distort the results.
     The basic cleaning steps are:
     1.   Removal of surface residuals immediately after use.
     2.   Hot soaking to loosen and flotate most particulate matter.
     3.   Hot-water rinse to flush away flotated particulates.
     4.   Soaking with an oxidizing agent to destroy traces of organic
          compounds.
     5.   Hot-water rinse to flush away materials loosened by soaking in a
          deep penetrant.
     6.   Distilled-water rinse to remove metallic deposits from the tap
          water.
     7.   Methanol rinse to flush off any final traces of organic materials
          and to remove the water.
     8.   Flushing the item immediately before use with some of the same
          solvent that will be used in the analysis.
     Each of  these eight fundamental steps are discussed  in their order  of
appearance.
     1.   As  soon as possible after glassware  (i.e., beakers, pipets, flasks,
          or  bottles) has come in contact with sample  or  standards, it  should
                                      D-32

-------
     be methanol-flushed before it  is  placed  in  a  hot  detergent  soak
     bath.  If this is not done, the  soak  bath may serve  to  contaminate
     all other glassware placed therein.

2.   The hot soak bath consists of  a  suitable detergent  in water of 50C
     or higher.   The detergentpowder or  liquidshould  be  entirely
     synthetic and not have a fatty acid base.   Very few  areas of  the
     country have water with sufficently low  hardness  to  avoid the
     formation of some hard-water scum due to the  reaction of calcium
     and magnesium salts with a fatty-acid soap.   This hard-water  scum
     or curd would have a particular  affinity for  many chlorinated
     compounds,  and being almost entirely  water-insoluble, it would
     deposit as  a thin film on all  glassware  in  the bath.

     Many suitable detergents are available on  the wholesale and retail
     market.  Most of the common liquid dishwashing detergents sold at
     retail  are  satisfactory, but they are more  expensive than other
     comparable  industrial products.   Alconox, manufactured  by Alconox,
     Inc., New York, in powder or tablet form,  is  marketed by  several
     laboratory supply firms.  Sparkleen,  another  powdered product,  is
     distributed by Fisher Scientific Company.

3.   No comments required.

4.   The most common and highly effective  oxidizing agent for  removal  of
     traces of organic compounds is the traditional chromic  acid solu-
     tion made up of H?SO. and potassium or sodium dichromate.   For
     maximum efficiency, the soak solution should  be  hot (40  to 50C).
     Rigid safety precautions must  be observed  in  the  handling of  this
     solution.  Prescribed safety gear should include  safety goggles,
     rubber glvoes, and an apron.  The bench  area  where  this operation
     is conducted should be covered with  flurocarbon  sheeting  because
     spattering will disintegrate  any unprotected surfaces.

     The great potential hazards associated with the  use of  a  chromic
     sulfuric acid mixture have been  well  publicized.   Current commer-
     ically available substitutes possess  the advantage  of safety  in
     handling, and claims indicate  that these biodegradable  concentrates
     have a cleaning strength equal to that of chromic acid  solution.
     They are alkaline  (equivalent  to approximately 0.1  N NaOH upon
     dilution) are are  claimed to remove dried blood,  silicone greases,
     traces, etc.  They will not attack glass or have a  corrosive effect
     on skin or clothing.  One such product,  "Chem Solv  2157,"  is  manu-
     factured by Mallinckrodt and available through laboratory  supply
     firms.  Another comparable product,  "Detex,"  is a product of Borer-
     Chemie, Solothurn, Switzerland.

5, 6, and 7.  No comments required.

8.   Between the time the glassware is washed and  its next use,  it could
     pick up some contamination from either the air or direct contact.
     The  practice of flushing  the  item immediately before its use with
     some of the same solvent  that will be used in the analysis helps to
     ensure agains this.
                                 D-33

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     The drying and storage of the cleaned glassware are critical  to prevent-
ing the nullifying of the beneficial  effects of the cleaning.   Pegboard
drying is not recommended because contaminants can be introduced to the
interior of the cleaned vessels.   Neoprene-coated metal  racks  are  suitable
for such items as beakers, flasks, chromatographic tubes, and  any  glassware
that can be inverted and suspended to dry.  Small articles such as stirring
rods, glass stoppers, and bottle  caps can be wrapped in  aluminum foil  and
oven-dried for a short time if oven space is available.   Under no  circum-
stances should such small items be left in the open without protective cov-
ering.  Clean glassware can easily be recontaminated by  a dust cloud raised
by the daily sweeping of the laboratory floor.
Process Sample Preservation
     The required containers, preservation procedures, and holding times for
the aqueous scrubber water samples are presented in Table D-l.  In accordance
with generally accepted practice, solids such as the waste feed and ash  will
be placed in glass containers with Teflon-line caps and  cooled to 4C without
jeopardizing the sample.  Toxicity Characteristic Leaching Procedure (TCLP)
samples must be obtained as separate samples; no preservatives are added, and
samples are stored and shipped at 4C.
     Scoops and dippers or thiefs were used to prepare all process samples.
Gallon glass jars and 5-gallon metal pails were used for compositing purposes
prior to placement of sample aliquots in final sample containers to analysis.
Separate containers were used for each run so that no decontamination of the
compositing vessels was required in the field.
                                     D-34

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    TABLE D-l.  REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR AQUEOUS SAMPLES
Measurement parameter              Container3          Preservation             Maximum holding times0


Purgeable organics                     G               Cool  to 4C,      .       14 days
(EPA Method 8240)              Teflon-lined septum     protect from light

Extractable organics                   G               Cool  to 4C,             7 days until  extraction,
(EPA Method 8250)              Teflon-lined cap        protect from light       40 days after extraction

Metals                                P,G              HN03  to pH <2            6 months



  Polyethylene (P) or glass (G).
L
  Sample should be preserved immediately upon sample collection.
c Samples should be analyzed as soon as possible after collection.  The times listed are the  maximum  times
  that samples may be held before analysis and still be considered valid.  All  data obtained  beyond the
  maximum holding times will be flagged.
d
  Add 0.08% Na2S203 if residual chlorine may be present in aqueous samples.

Reference:  BOAT Generic QAPP

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                 APPENDIX E



EQUIPMENT CALIBRATION PROCEDURES AND RESULTS
                       E-l

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                     CALIBRATION PROCEDURES AND RESULTS

     All of the manual  stack sample equipment used was calibrated according
to the procedures outlined in "Quality Assurance Handbook for Air Pollution
Measurement Sytems. Volume III" EPA-600/4-77-927b.

NOZZLE DIAMETER
     The nozzles were calibrated by making three separate measurements using
different inside diameters and calculating the average.   If a deviation of
more than 0.002 inch was found, the nozzle was either discarded or reamed out
and remasured.  A micrometer was used for measuring.   These calibration data
are shown in Figure E-l.

PITOT TUBE CALIBRATION
     The pitot tube us.ed in sampling was constructed  by  PEI Associates, Inc.,
and met all requirements of EPA Mehtod 2, Section 4.1.    Therefore, a
baseline coefficent of 0.84 was assigned to each pitot tube.  See Figures E-2
and E-3 for alignment requirements of Method 2, and Figures E-4 and E-5 for
actual inspection data of the pitot tubes used during the test program.
  40 CFR 60, Appendix A, Reference Method 2, July 1987.
                                       E-2

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                     NOZZLE CALIBRATION
Date
                         Calibrated
Nozzle
identification
number
'Af (&S--S.7)
/ - \

D^, in.
.3**


D2, in.
 Zof


D_, in.
,-zn


AD, in.
s
\s

avg
/ 3^9


where :
AD =
          nozzle diameter measured on a different diameter,  in.
          Tolerance  =  measure within 0.001 in.

          maximum  difference in any two measurements,  in.
          Tolerance  =  0.004 in.
    avg
        = average of  D, ,  D_,  and D...
               Figure E-l.  Nozzle calibration data.
                              E-3

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Date
          NOZZLE CALIBRATION


                   Calibrated by
Nozzle
identification
number
4^- /^O

D^, in.
0.25

D2, in.
g&5
d.J?gl
D-, in.
O.ZBI

AD, in.
0-0*3

avg
o. Zt
x- '^l
where:
     AD
    avg
nozzle diameter measured on a different diameter,  in.
Tolerance - measure within 0.001 in.

maximum difference in any two measurements, in.
Tolerance - 0.004 in.
          average  of D,,  D./ and D^.
             Figure E-l continued.  Nozzle calibration data.
                               E-4

-------
                TRANSVERSE
                 TUBE AXIS
                          \
                                    FACE
                                *~ OPENING"
                                    PLANES

                                 (a) ENDV1EW
LONGITUDINAL
 TUBE AXIS
          
      A-SIDE PLANE
	L
                                                           NOTE:
0.48 cm < Ot  <  0.95  cm
(3/16 1n.)     (3/8  1n.)
                                                           1-05  Dt  <  P  <  1.50  Dt
                                                                PA  =  PB
                                 B-SIDE PLANE

                                (b)
                                  A or B
                                   (O
  Figure E-2.  Properly constructed Type S pitot tube, shown in:   (a) end view;
  face opening planes perpendicular to transverse axis; (b) top view; face open-
  Ing planes parallel to longitudinal  axis; (c) side view; both legs of equal
  length and centerlines coincident, when viewed from both sides.  Baseline
  coefficient values of 0.84 may be assigned to pitot tubes constructed this way.
                                         E-5

-------
              TRANSVERSE
              TUBE AXIS
LONGITUDINAL fg
   TUBE AXIS Q	
                                                          Bl (+ or -)
                                         (e)
                       ~
                                                    
                                                   i
                                     (f)
    Figure E-3.  Types of face-opening misalignment that can result from field
    use or improper construction of Type S pitot tubes.  These will not affect
    Cp so long as ai and a? <10. Bi and B? <5, z <0.32 (1/8 1n.)*and w <0.08
    cm (1/32 1n.).
                                     E-6

-------
                      PITOT TUBE  INSPECTION DATA SHEET



Pi tot Tube No.    5CH         Date   I.VoJi-'Sk    Inspector
3'
al
Degrees
0
<10
a2
Degrees
1
<10
Degrees
i
<5
Degrees
1
<5

Dt
Inches
O,3"75
0.185  Pt O.380
P
Inches
Q~,,
-
1.05 Dt
Inches
^, ?"<-/
-
1.50 Dt
Inches
.1 - 5(, ^
-

Y
Degrees
3r
-
Degrees
G*
-
Inches
tf.o^-X
<0.125
Inches
C'~GC-
<0. 03125

Inches
,50-z.
1.05 D, 
-------
Pitot Tube No.
PITOT TUBE INSPECTION  DATA  SHEET
        Date   13 -J3 -ftk    Inspector
d-
al
Degrees
Cf
<10
a2
Degrees
Oc
<10
'l
Degrees
3?
<5
Degrees
1


Dt
Inches
, llfi
0.185 < Pt <0.380
P
Inches
.vis-
-
1.05 Dt
Inches
,3"^
-
1.50 Dt
Inches
- 5f,~^
-

Y
Degrees
6*
-
Degrees
1
-
Inches
O.fQS
<0.125
P  (
-------
            o
       < GLASS TUBE
      '  THERMOMETER

        N

UMBILICAL I
          I
     KETER  BOX ^	
    PRESSURE
    CONTROL
    VALVE
                                                              U - TUBE
                                                             MANOMETER
                  MET TEST METER
                   Figure E  6   Calibration setup.
DATE
                                       MtTt* MX NO.
WUtOHTTRIC
                          in.
                                       OUT CAS Mm* HO.
Or if lc*
Mnoejeter
eettinq
AH
In. HjO
0.5
i.e
l.S
2.0
3.0
4.0
Ci voluoe
wet test
eter
V
ftJ
S
S
10
10
10
10
(* volume
dry 
tr
Vd"
ft3











Met tt Dry  Mtr
tar

r











Inlet
*i-
F











outlet
**n'
r











kvrrag*
*
r






Tl*
 ,
in






t






AM







AH
O.S
1.0
l.S
2.0
3.0
4.0

AH
O.OJ4I
0.0737
0.110
0.147
0.221
0.2*4
T
v % 






AM
0.0317 AH (
9^ (t.  4*0)
b d |_
lw  4*0) ") 2
' J






    1  lutie of eeurcy of vt t*t aetcr te dry tt tvr.  Tolrnc   0.01
  AM  Orifice of prcisur* differential that fives 0.7S efa of air et 70*r and 2.2 inches of
        aarcury. in j>.  Tolerance  0.1S.


                         Figure 1-7.   Calibration data  sheet.


                                    E-9

-------
                      PAKTICUATt SAMPLING *TE* MX INITIAL CALlWttTJON
DATE: 	

CALIBRATOR: .



Leak Checks:
            1-3-8&
                                        ICTCK IOX NO.
                                            lAROMCTRIC MtSSURE (PJ
                                                               D
         (minimum 5 In.   _ .   ________
 Negative (vntt'n 3 in. Hg of abwlute):
*tot to exceed O.OOi
                                                           2.7.5   tn.
                                                                           in.  Hg
Orifice
aunometer
jetting
  AH
1n
       Volume
      et test
        eter
        ft
                   Volume
                  dry pas
                    eter
                     ft
      Temperatures
et test
wter
   Dry 9s mter
Inlet  Outlet  Average

Duration
  of
  test
   f
  In
Vacuum
setting
  1n
  Nfl
                                                                              AH*
                                                  In
  0.5
           s.o
                                            77.75
                                                                SO 0
                                            /.cot,
                                          A5-7J
  1.0
      IO.O
                             72
                               8TI
                             72
                                                               /o.o
                                            /.col
  1.S
          /0.O
                            71
                                      77
              Oft.Ztl
                                                      *&
                                                            /O.o
                                            1.600
  2.0
                            72.
                                      7?
                  utf.b/3
                        7Z-
                                               . S
                       jfV/i
                        .
                                                                /O.O
                                            t.ooz
  3.0
                                   S
                                          s-/
                                            9H
                                                                lO.o
  4.0
                             72-
                                      fr/
                             7Z-
                                                                          I.&1L
T wst not deviate by more than +0.02 Y.
AH* must not deviate by more than 0.15 In HjO.
                                                         Average
                                                                       ,111
AH
                          )(T + 460)
                    AH/13.6)(TW * 460)
                                            (0.0317K  AH    )
                                                                        460)l
O.S
1.0
          *
                           &37.75.
                            &*.  \
      ( to.o M t-9.SC>  \{&9.25
-------
                     WMTUCaATt SAMPLING ICTC* DO* INITIAL
DATE:
                                                 IOZ NO.
CALIBRATOR:   \T.
                                        AUOWTHIC MttSSUHt (tj  ff?. 7C)    In. Mg
Ltak Checks:
                                           y
 Positive (minimum 5 1n.
 Negative (w^ttnn 3 in. Mg'of absolute):   t7.QOCT
hot to exceed 0.001 c must not deviate by acre than +0.02 >.
AHP must not deviate by acre tharT 0.15 In H^O
                                                               AM*
                           )(T, + 460)
               )(Pb * AH/13.6)(TW + 460)
                                             (0.0317)1  AH    )

                                             (  rV  )(T, + 460)
                                        (TM    460)(I) l
0.5
                     74
                                                7/7
                                     il
1.0
                   tf-70
                  lff-71  M
                                                   if
 1.S
               )(
       U0.W4M   vf$l   )(
                                                             L(   /^
2.1
                                                                         itfltf/
                                                                            >T2
 3.0
       t 10. 1  M
     ^
_H
                  Mil-  H
                                       .(
 4.0
       i Iff   w  W10

                        V
                                                                  .{   1O
      Figure  E-8 continued.   Particulate sampling  meter  box initial
                                calibration.
                                              E-ll

-------
DATE:   7-7
BAROMETRIC PRESSURE (Pbar):

PLANT:  T 7
                                   n.  Hg
PROJECT MANAGER:
METER BOX NO.

PRETEST Y:  ^
PROJECT NO.
CALIBRATOR:
                                                           P~T- 3
Orifice
manometer
setting
AH
in. H-0
1.1
1.7-
/.-Z-
Wet test
meter
volume
V
w
ft3
\o
w
//
Dry gas
meter
volume
Vd
ft3
fa (Td
        460>
                                                          "(T*460)(   0
                                                            w
                                                                  w
    10
                                        C.
-------
                                           nc.ict\ DUA
                           POST-TEST CALIBRATION
DATE:	
BAROMETRIC PRESSURE (Pbjr): 39 */Qln.  Hg

PLANT:  V| CALIBRATOR: T- Mfcf^fL
Orifice
manometer
setting
*
AH
In. H20
1.3
/.3
/.3
Wet test
meter
volume
V
w
ft3
l(p
10
10
Dry gas
meter
vol ume
Vd
ft3
M-P3r1
IW.Oil
W-ott
170.676
I106K?
win
 , 	
Temperatures
Wet test
meter
T
w
F
11
11
11
11
11
11
Dry jas meter
Inlet
Tdi
"F
&
%1
37
fl
?1
n
Outlet
Tdi
F
7^
77
77
77
"77
77
Averaqe
7d "
F
?5L7S
?a.
X?.^
Vacuum
setting
**
In. Hg
$

5
Duration
of run
(5
m1n
^97
llrMsff
iW-fl
Post-test average***
 -~ -
Y
155
.1%
frff
MS
___.
~    
AH(?
(ft
1.10
w
/.f?
                                                     AMI?
     w
               bar
                                        (0.0317)(   AH  )
         )(Pbar + AH/13.6)(Tw + 460)
(   li,
                                                          (53/
                                                         u
                                                                         n   2
  'To be the average AH used during the test series.
  'To be the highest vacuum used during the test series.
  'Post-test Y must be within the range, pre-test y *
   Post- test AH@ must be within the range, pre-test AH(? +0.15
        Figure E-9 continued.
                               Participate sampling  meter box post-test
                               calibration.
                                            E-13

-------
THERMOCOUPLES
     The thermocouples were calibrated by comparison against an ASTM-3F
thermometer at approximately 10F intervals between 50 and 180F.   The thermo-
couples read within  2F of the reference thermometer throughout the entire
range.  The thermocouple was checked at ambient temperature at the test site
to verify the calibration.  Calibration data are presented in Figures E-10
through E-13.

DIGITAL INDICATOR FOR THERMOCUPLE READOUTA
     A digital indicator was calibrated by feeding a series of millivolt
signals to the input, and comparing the indicator reading with the reading
the signal should have generated.  Error did not exceed 0.5 percent when the
temperatures were expressed in degrees Rankine.  Calibration data are shown
in Figure E-14.

DRY GAS THERMOCOUPLES
     The dry gas thermocouples were calibrated by comparison against an
ASTM-3F thermometer at approximately 32F, at ambient temperature, and at
approximately 110F.  The thermocouples agreed within 5F of the reference
thermometer.  The thermocouples were checked at ambient tmeprature prior to
the test series to verify calibration.  Calibration data are included in
Figures E-15 and E-16.

TRIP BALANCE
     The electronic mettler balance was calibrated by comparing it with
Class-S standard weights, and it agreed within 0.5 gram.  Calibration data
are shown in Figure E-17.
                                      E-14

-------
Date:
Calibrator:
METHOD 4 THERMOCOUPLE CALIBRATION  DATA SHEET


         	 Thermocouple  No.:  	

         Je.i.          Reference:    XS '7"A?
                ">
Correction factor:
Reference
point
No.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
Recommended
temperature,
OF
50
60
70
80
90
100
110
120
130
140
150
160
170
180
i
Reference
thermometer
temperature ,
op*
So
60
70
fo
3d
/&
//o
/20
/1C
/to
!$0
160
>-;}
/M
Thermocouple
temperature,
op
sz>
fo
70
&>
in
/M)
i/n
/2O
130
^
/Vf
IM
17 1
I*!
i 
Difference ,
op* *
Q
 ' ^
LX
O
0
0
0
0
&
0
O
1
/
1
i
 *Reference  thermometer must be ASTM.
**Difference must be less than or  equal to +2F over  entire
  range.


    Figure  E-10.  -Method 4 thermocouple calibration  data-sheet.
                                    E-15

-------
DRY GAS METER AND ORIFICE METER
     Figure E-6 was the setup used for the initial  and post-test calibration.
A wet-test meter with a 2-cubic-feet-per-minute capacity and  1 percent
accuracy was used.  The pump was run for approximately 15 minutes at an
orifice manometer setting of 0.5 in.H20 to heat up the pump and wet the
interior surface of the wet-test meter.  The information in Figure E-7 (ex-
ample calculation sheet) was gathered for the initial  calibration and then
the ratio of accuracy of the wet-test meter to the dry-test meter and the AH@
were calculated.
POST-TEST METER CALIBRATION CHECK
     A post-test meter calibration check was made on the meter box used,
during the test to check its accuracy against its last calibration check.
This post-test calibration must be within  5 percent of the initial cali-
bration.  The initial calibration was performed as described in APTD-0576.
The post-test calibration was performed using the same the initial calibra-
tion.  Three calibration runs were made using the average orifice setting
obtained during each test run and with the vacuum set at the maximum value
obtained during each test run.  After running the post-test calibration check
                                                                         *
all three runs were within the  5 percent range allowed by EPA Method 5.
     The initial and post-test meter box calibration data are resented in
Figures E-8 and E-9.
  40 CFR 60, Appendix A, Reference Method 5, July 1987.
                                      E-16

-------
Date:
METHOD 4 THERMOCOUPLE CALIBRATION DATA  SHEET


                                          \vj.l)
Calibrator:
Correction  factor:
Thermocouple  No.:

Reference:  /\STM  "of
Reference
point
NO.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
Recommended
temperature,
op
50
60
70
80
90
100
110
120
130
140
150
160
170
180
Reference
thermometer
temperature,
op*
50
,0
70
ko
C|O
loo
no
130
1^,0
140
150
\GO
no
/so
Thermocouple
temperature,
op
M
q
14
sq
c\q
|0
-------
                        IMPINGER THERMOCOUPLE
                       CALIBRATION DATA SHEET
      Date:

Calibrator:
Thermocouple No:

      Reference:
Reference
point
No.

1
2

Source1


1
2
Reference
thermometer
temperature
dec. F
75.
3^

Thermocouple
temperature
dec. F
72-
33s.


Difference
dec. F"
o
<2
            'Source:  1)   Aabient
                      2)   Ice bath

           "Difference aust be less than  2 deg.  F at both points
  Figure E-12.  Impinger thermocouple calibration data sheet.
                                    E-18

-------
                        IMPINGER THERMOCOUPLE
                       CALIBRATION DATA SHEET
c.iib,.t.r=
Thermocouple No:

      Reference :
                                                           ~ )
~ 3 /
Reference
point
No.

1
2

Source*


1
2
Reference
thermometer
temperature
deg. F
H3
Rl

Thermocouple
temperature
deg. F
~1?>
^1


Difference
deg. F"
o
C>
            'Source:   1)   Ambient
                      2)   Ice bath

            'Difference must be less than  2 deg.  F at both points
 Figure E-13.   Impinger thermocouple calibration data  sheet.
                                   E-19

-------
                  THKT.'QUPLE DIGITAL IIOiCATCR
                      CALIBRATION DATA SHEET
              DATE:   O.
                     /
           OPESATCR:
CAilSRATiCN DEViCE NO:
              SERIAL NO:
z
TEST PQ IK!
NCI
1
2
3
4
5
6
7
8
9
10
HILL' VOLT
SIGNAL
-0.692
1.520
3.8:9
6.082
8.314
10.560
22.251
29.315
36.155
42.722
ESU1VALENT
TEHFESAT-JSt,
dej. F
0
100
200
300
400
500
1000
1300
1600
1900
DIGITAL INDICATOR
TE-rEiATURE READING,
de(. F
O
/ 01
1*0,
Sot
37?
Sec
/coo
/2??
/$
-------
                          GAS  TKERMC'-O'.iFLE
                          RaTiON DATA SHEET
:/i t;
Tr;er!T.ocGup It  No:

      Reference:
                                                         /'"/''"
r.e fer ence
re int
N; .

-
'-
-

o j:ce*


-
^
-
net er en: e
t her (T'on-et*:
t tripe: at ur -
or c . F
?2
32
/yv

Triermocoudi e
t e rr. : e : s t - J r e
de  . F
^
32.
/
-------
Calibrator:
                        DRY <5A? THEF.MO'Cl'JFLE
                       CALIENT; ON DATA SHEET
Tnermocouple No:

      Reference:
O p-
IHLET
Ref erence
point
No.

1
-
-

Source'


1
'V
-
ftelerence
thermometer
temper sture-
Qrv. F
TO-
3^
UH

Thermocouple
terr.per a^ur e
dec. F
73
33-
IM


Dl ffer snce
deg. F"
/
0
0
  i t-L:
Refer ence
point
No.
1
*
3

Source'
1
2
5
Refer ence
theme-meter
tenperature
deg. F
13-
32-
w

Thermocouple
temperature
deg. F
no
32
iw

Dif Terence
dej. F' *
SL
?
0
            'Source:  1;  Ambient
                      2)  Ice bath
                      3)  Water bath

           ''Difference Bust be less than  5 def. F at both points

  Figure  E-16.   Dry gas thermocouple calibration data sheet.
                                 E-22

-------
                    TRIP BALANCE CALIBRATION DATA SHEET
Balance
  No.
Date
Calibrator
                               Mass determined for
5 9
Error
50 g
Error
100 g
Error
                  J
                              as
                         sai
                       100.1
                          a/
 m
        J.
                  a/
           &.0
                   IQO.O
                  00
                 f.
                              a/
                         $0.3-
                       loo. (
                         O.I
                 j.
                        S-0
                               0-0
                             O.o
                                       (J-O
                                           o.o
                                      too. o
                             0.0

                  7 fvJeese
                                           a/
                                            O.I
Error must not exceed 0.5 grams at each point.
             Figure -17.  Trip balance calibration data sheet.
                                      E-23

-------
BAROMETER
     The field barometer was calibrated to within 0.1 in.Hg of an NBS-trace-
able mercury-in-glass barometer before the test series.   It was checked
against the reference barometer after each series to determine if it read
within 0.2 in.Hg.  The barometer read within the allowable limits each
time.  Calibration data are included in Figure E-18.
VOST DRY GAS METER
     The dry gas meter for the VOST sampling train was calibrated against a
500-ml bubble meter at a flow rate of 1 liter/min.  After the bubble meter is
connected to the gas meter inlet, the meter is operated for 5 minutes to
stabilize flow.  After warmup, three separate calibrations are made with a
total metered volume of 5 liters and at least seven bubble meter flow rate
readings.  Bubble meter readings are acceptable if the ratio of the shortest
time to the longest time is greater than 0.95.  The meter calibration factors
for all three runs must agree within  0.02 Y.  The calibration data for the
meter used in this test are shown in Figure E-19.
                                      E-24

-------
                         BAROMETER CALIBRATION LOG
BAROMETER
   NO.
Hoe
                                             ft?
PRETEST
                                                            &#<
BAROMETER
READING


REFERENCE
BAROMETER
READING
                                    3.
DIFFERENCE
              0.01
           0,0
                                             .of
DATE
t-IO-17
CALIBRATOR
POST-TEST
BAROMETER
READING
                            17.X7
REFERENCE
BAROMETER
READING
                  Z1.&
DIFFERENCE**
                                        t\
DATE
CALIBRATOR
    >>
 *Barometer .is adjusted so  that difference does* not exceed 0.05 in.  Hg.
**Barometer  is not adjusted.   If difference exceed O.'IO in. Hg, inform  project
  manager  immediately.

    Figure E-18.  Barometer calibration log.
                                      E-25

-------
                                          DIY GAS nrrat POST-TEST CALIBEATION
                                              OW aOV (1 LITEt/IIIIWTE)
                   WTE:

                  PUNT:
                       _

          PIOJECT IUNAGEB:
                       .
           CALIBiATION BT=
                                /2c
       HETQ CONSOLE NO:

      NOMINAL FIM UTE:
                    .
        KULE IfTQ M):
                                                                                    PKTEST I:
                                                                                            *"
                                                                                          LSTEtS/rllNUTE
                                                                                 WTO. SETTING:
                                                                                            :   /
                                                                                            ..J..
                                                                                                     7
                       UN II
BUBBLE HETQ CONDITION:           NT CAS HETQ CONDITIONS

  ola (Vbi!: ^f  liters   wluie initial(Vii): -       liters

   IMP. (Tbi): nd  M|- F     *|UM MuMViO: .-^      liters

bubble Mter tins (seconds)   tew. initial(Tdfti):  i*,     K|.  F
         (tiM.bii                          -"&-
l:*r. fttt.   5:_/rf_iec.  titp. final(Mfif):  /  y    de(.  F

                                                   di.  F
        BUBBLE HETQ CONDITIONS          DBT CAS HETER CONDITION:

          voluM (Vbi):   /   liters    toluM initiaKVii):^^^.  liters

           tttf. (Tb):rfj   M(. F     roloM fiiiHW):^ c,^ liters
                                                                     ):rtj
                                                          bubble Mter UMS (seconds)   tnp. initial (Tdpi)',  /.y    dej. F
                                                                   (tiw.M)                          	
                                                                  tec.
                                                                                MC.
                                                                                          alcalited F f
                                                                                                     r.l/
                                                                                                        i-O
                       UN 13
BUBBLE HETEE CONDITIONS          MT CAS HETD CODITIONS

              I    liters   toluM UitiaMVii): a/  /vw, liters
                                                                 (VbiXSO)
                                                          *
   tMf.
                                        ): AI
                                                               Uvf.
                                       |. Tdp460)(tiK.d|i)
                  de(. F     wloM liwHtaf):
liters
                                                                        QM
babble Mter UMI decoMi)   tMf. iiitUKTdni):  /n/  M(. F
         (tiM.b.)                          -^*-
                                                  Ml. F
                                                    I.  F
                                                           AVQACE POST-TEST T>
                                                                                AM.
        Figure E-19.   Dry gas  meter  post-test  calibration  (low flow approximately
                          1  liter  minute)
                                                       E-26

-------