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
-------
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.
-------
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.
-------
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
-------
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
-------
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
-------
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
-------
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., 1800°F in
the kiln, 2000°F 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
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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 1800°F. 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 compounds—chloroform 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 68°F, 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 180°F 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
i
ro
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
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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
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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%
±2°F
Y ± 0.05Y
post-test
±2°F
±0.5g
±0.10 in.Hg
±5°F
±5°F
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%
+1°F
+1°F
-0.034
0.0°F
0.0°F
0.0 g
0.01 in.Hg
+1°F
+0°F
+1°F
+2°F
+3°F
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 error—the 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
Li«1t *
(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= S£r'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-H£v 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 (in—t^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 .......... Barc«etric 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, te»c 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 st£C(- 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 •,,.
'"
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£
» III
m >ii 4- -
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t. ai ai
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-o -o t^v r- r ~ r- r- i ,
Cr- -^* ~i —< ^-» '^> to i 4
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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 (acf«i; 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 PA»TICULftTE, 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 68°F 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 (68°F, 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 20°C, 760 mm Hg
sta (68°F, 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, 528°R/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
. i >ii
iii), i
i.i
1 1
,', :( '.'
i > :ii
in
'it
• 1 1 . t MI
m »
-i "
1 1 ii i
• • . i i •
• i* «n
• „ i
i
; • _"•
:•, ,, .,r
.1 1 'II-
1 i > I .1 ii •!• i
t 1 1 | 1 1 1M < M'
II MI • - \ III '' 1 '
t < 1 I 1 III ' f
t 1 1 . I 1 II Ml III
111 i . • i" M!
tit - i j
i - t
-
• M * . - . • • •• » t i •;
1 1 1 1 1 i ,1 i t . MII
. - i
li > i in
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|| <• >
. i - ii
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-\
\ \
^\M
\ '
\
f^fi
^
A./
^"^
/••
j
^y
/
/U L
/
T^
r / '
SK^
f s/
1
r(J _
P '
vx
J
^
,
^^- >
^
af
^ / y ^
' ^
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 /<£/ -in.
ORIFICE K
Orifice
manometer
reading
AH,
in.H20
/**
FACTOR: ^VS^X/r'' AUDITOR: <§S
^"^^
Dry gas
meter
reading
ft3
5*9.?
2l3,o
Temperatures
Ambient
°F
?*
9t
Average
°F
fy
Dry gas meter
Inlet
VT1f
°F
??
91
Outlet
VTof
°F
77
?Z-
Average
Tm-
V
Duration
of
run
0
min.
'£:*<{:¥*
Dry gas
meter
/*,^
Vtd'
ft3
/*.*/*
Vfnacf
ft3
«.a^
Audit,
Y
.111
Y
devia-
tion, %
o.\ '
Audit
AHG»,
in.H20
f.trO
AH@ Devi a-
tion, in.H20
-.<* '
m
std
m
act
17.647(Vm)(Pbar + AH/13.6)
*•/
1203(
(Ta + 460)
1/2
ft3
ft3
Audit Y *
Y deviation
m
'std
Audit Y - Pretest Y
Pretest Y
x 100 =
Audit AH@ = (0.0317)(AH)(P. J(T + 460)
oar m
Audit Y must be in the range, pretest Y ±0.05 Y.
Audit AH@ must be in the range pretest AH@ ±0.15 inches H20.
in.H20
B-14
-------
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 + 460°F
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
'
I
I I M t I Vli
Mil
_
/4.
UMTIIM. lOUIIIM
Qiti(i4d\ 1 1 MI i M
iA**U UN
I I I I I i I I
IUB M.
OTIMIOI
1INP Mlii.
(•'I H" "91
"H" ''l»l"'!'
MA1IC
MIU
iw «/o»
n!..1Hi.|ii
'II ••|«»£»»^*~ ""^"^^^^^t;^ ^^^
.7fi14fa?g rtf.4, 6/.7.
Illltl MMMMS)
.....
M*C« IkSIM
DIM*. IIKMS)
^4 1111 i A i
SS5
(77
I
MOM IU4IM «M UN
. Pftte . ,
•iiin. «.o. luurulMiu | mm
~l • I *> | III llOlMlMIMJ •«•
Mill Ui
(Ml« f
IU» CMC«
IH. ml cm
FMTM
fACIW
MUI UI
»noi
luM
t>
n|ii|ii
rxiM
nE
tut
llll«ll»ll
!_U H"lrl
V7
•fart* <4CL\
MUI Ml
M'.
»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^S«a_
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 - fLt£T 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]4lJ«4|«»ji»|M|j;|l>|v»h%|>«J»))ilI»»JKljn|»j|nj»4J»
_*_*-• I I •! f •^••••^••^•••••••••••••^••^ * • ••^•^••••i I ^—^L.«.fci 1 i ^•J—^••-^•Ajaa^—A^«
I I I
im
>t[»|ti|4>|i»|n|>i|»i|i«|»|n|i)|)t|>t|i
OM1AIM
T'l'M
i i
' ' '''
HUT
CM
tune
rim
(!• M^
(iiui
CO
i
ro
.|i|*l»fi|»|iM.»lMpF
•aim.
1 •
•Ml. VUVK
(t) '101 kO
Tm^T
.. IWIII I Mill
kOIMlMtt • M •
mm CM.
(Mini »
Jl|4»|4l|4l
ACM
Sl*£« IkSIM
DIMM. (MCHd)
ruoi
IUM
O
><|H{H|4l|H 4<|4>|t4|tl|4«|n|U|ll|U ll|
IMM
I | _J I A I I
rut
IUK CMtCK
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K
FACIM
.iMh
C
MCI
;|4IJM|4>
MUI Ml
MUI Ul
,.TnHi,
•I'.
Rj
I4|lil)4|ll
•IOWO
MU
•III
iijiiiiaiulfcMunirii
3»|39UOJ4T
HL
57
VOINT
CiVOCB tlM
l>« kr
V&LOC1TT
wince russuu
oirrcuMTiAL
|4)N|.ln.M}OI
CTACI
our CAS NCTCM
TCNPLRATUkC
iwl
CAMFU BOX
IT !••»
IT. !.«»
VACUUM*
!•..*«
VEMTCKAIVM
out
A'
'^7
A^
M
2
jd£i
/2
M
fz-
i&
/ol
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
S
i
s
5
i
i
l
• i
55
il
VI
•( oJ
-sj
?y
III!
a/
JU
*^
B-23
-
r
> j
CAS NCTC
NPL«ATUk£
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
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~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 %-s«ent
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
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Container No. fe>6bv /T
Back rinse
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Container No. 1/75/#
•Blank Container No. £757*9
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Container No.
Liquid Levtlf
Remarks
/ Samples stored and locked
Received by
Remarks
LABORATORY CUSTODY
Date
B-30
-------
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Plant
LEAD SAMPLE RECOVERY AND INTEGRITY SHEET
Sample date
ilnli?
Sample location Ou,^*£ @LMtf Recoverv date tfl/lf/f/
XOO
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Filter number (s) Q' J)(J\
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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
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% spent
Total moisture / 7 9/t+* g
/
Filter container number(s)
Description of particulate on
Acetone probe
rinse container no.
Acetone blank
container no.
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rinse container no. tsO/^
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container no. 1$ ' *** )5
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container no. t-"~"~
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Remarks
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Remarks
RECOVERED SAMPLE
L&M8 Sealed (/
filter T^J
Liquid level
marked
Liquid level
marked
^ Liquid level /
1 /r marked \/
- £>, Liquid level /
H marked ^/ ^
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/
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
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9
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RECOVERED SAMPLE
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Filter container number(s) j. if /
Description of particulate on filter
Sealed
% spent
Probe rinse
Container No.
Back rinse
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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
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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- &
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Remarks
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marked
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Remarks
LABORATORY CUSTODY
Date
B-36
-------
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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.
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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
-------
I—I—I I I I I \ I 1 1 I "1
-------
LEAD SAMPLE RECOVERY AND INTEGRITY SHEET
4>9
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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.
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time
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Total Volume of Condensate in Vials, -"
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-------
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SAMPLING DATA
Date
Location
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V-
Run No.
- V~
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Meter Console No.
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VOST SAMPLING DATA
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-------
VOST
Date
Location
T."st Condition
Trap Nos. &3O
'
Sampling Train No.
SAMPLING DATA
Run No.
tor
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time
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volume
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liter
Rota-
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setting
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2*0
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tempera-
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2-79
/
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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-
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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
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I1ters/m1n
Sampling
time,
min.
0
Clock
time
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Keter
volume
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liter
Rota-
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setting
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In.Hg
Dry
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tempera-
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Primary
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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 &•<•/ in.Hg/min at /^ 5 in.Hg vacuum
n.Hg Ambient Temperature g0 °F Probe Purged /£ minutes at /. O liters/min
Sampling
time.
min.
Clock
tine
(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
JO
-3-3
7
ML
Avg.
?w
CO
I
01
Post-Test Leak Check fi.Q
Flow Direction Harked?
in.Hg/min at tf.Q In.Hg Vacuum Trap Pair Label No.
Condensate Recovered? VGA Label Nos.
Total Volune of Condensate in Vials,
Traps and V1a1 Stored in Can No.
ml Remaining Condensate "2-tj mis Total Condensate Vol,
on Ice? *s^ Culture Tubes and Can Purged With N2'
ml
nts:
Probe Leak Check Data:
Correspondlng Blank Nos.
1) V td « Vm, liters x Y x 17.647 x '
m*
-------
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 <£?,
flow Direction Marked?
in.Hg/min at
Condensate Recovered?
in.Hg Vacuum Trap Pair Label No. S/tTZ"" v~
VOA Label Nos. SATT- (X-/
Total Volume of Condensate in Vials, /y ml Remaining Condensate ^f mis Total Condensate Vol. ^o ml
Traps and Vial Stored in Can No. /^ on ^ce? ^__ Culture Tubes and Can Purged With N,?
Comments:
Probe Leak Check Data:
Corresponding Blank Nos.
1) V$td = Vm, liters x Y K 17.647 K
liters /
m1
-------
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 - /
A«blent 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/£/i£ed £/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 - [C«1. «» 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/$'7
or'
37«2Y-?
A-3E--C.0 ~ 2 *~Q ?
Chart divisions
Of$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
*
# ^ ) -^ 9 2- 7^»
^> i n ' Z., *- ^
/Vj^ " / 7 -r i V
' ' ' A /
:£> -TzWM ~Lx &l~ ** \
1.1,1^ 1
* 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
-------
CD
CO
oo
-------
B-89
-------
B-90
-------
16-8
-------
NO 44r.-17
B-92
-------
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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 (<100°C) emission samples were analyzed according to Method 5040, SW-846,
semivolatiles by EPA Method 8270, dioxins/furans by EPA Method 8280, and
semivolatile compound ( > 100°C ) 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
80°C
200°C
220°C
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 45°C;
45°C to 220°C at 10°/min; hold at
220°C 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
180°C
12 min
220°C
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
5°C for 2 min, then 6°C/min to 200°C,
hold at 200°C for 10 min
70 eV, nominal
Unit
35 -250 amu
Scan Cycle
Interface Oven Temperature
Injector Temperature
Manifold Temperature
1 sec/cycle
200°C
100°C
100°C
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
180°C
15.0 min
200°C
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
150°C
280°C
95°C
270°C
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 35°C for 4 min, then program at
10°/min to 270°C; 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
200°C
Electron lonization
70 eV, nominal
Unit
275°C
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 (35°C)
Direct source coupling
Initial hold of 0.5 min,
then 35-200°C at 3°C/min,
then 200-310°C at 4°C/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
D«t 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=XXZZ«ZZXXXZ»XZX=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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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 = S£S =
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=======5£5
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*
-------
ATTACHMENT 1
76
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-------
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 250°F 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 5°F, 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 1°C (2°F)
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 68°F 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 130°C (266°F).
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 20°C (68°F) 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
d±b
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 50°C 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 190°C 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 190°C 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 110°C 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 400°C 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 110°C 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
190°C 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
-------
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
-------
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 121°C (250°F) 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 121°C (250°F)
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 5°F, 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
-------
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
20°C (68°F) or less.
*
Whatman Reeve Angel 934AH.
D-20
-------
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.
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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 105°C 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
-------
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
-------
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
-------
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 50°C
or higher. The detergent—powder or liquid—should 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 50°C).
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
-------
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 4°C 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 4°C.
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
-------
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 4°C, . 14 days
(EPA Method 8240) Teflon-lined septum protect from light
Extractable organics G Cool to 4°C, 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
-------
APPENDIX E
EQUIPMENT CALIBRATION PROCEDURES AND RESULTS
E-l
-------
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
-------
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
-------
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'~G°C-
<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
C«i voluoe
wet test
•eter
V
ftJ
S
S
10
10
10
10
(•*• volume
dry «••
•«t«r
Vd"
ft3
Met t«»t Dry ••• Mt«r
••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 •eeur«cy of v«t t«*t aetcr te dry t«»t ••tvr. Tol«r«nc« • « 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 9«s 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 10°F intervals between 50 and 180°F. The thermo-
couples read within ± 2°F 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 32°F, at ambient temperature, and at
approximately 110°F. The thermocouples agreed within 5°F 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 +2°F 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
d»i. 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.
|. Tdp«460)(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
------- |