United States Office off Air Quality
Environmental Protection Planning and Standards
Agency Research Triangle Park, NC 27711
EMB Report Cl-ASP-10
September 1001
Air
ASPHALT
Emission Test Report
Mathy Construction Company
La Crosse, Wisconsin
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Note: This is a reference cited in AP 42, Compilation of Air Pollutant Emission Factors, Volume I Station
Point and Area Sources, AP42 is located on the EPA web site at www.epa.gov/ttn/chief/ap42/
The file name refers to the reference number, the AP42 chapter and section. The file name
"ref02_c01s02.pdf" would mean the reference is from AP42 chapter 1 section 2. The reference may be
from a previous version of the section and no longer cited. The primary source should always be check
AP42 Section: 11.1
Reference Number: 24
Title: Emission Test Report, Mathy Construction Company Plant #6,
LaCrosse, Wisconsin,
EMB-N0.91-ASP-11,
Emission Assessment Branch, Office Of Air Quality Planning And
Standards,
U. S. Environmental Protection Agency, Research Triangle Park,
NC,
February 1992.
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DCN: 92-275-026-48-01
EMISSION TESTING FOR
ASPHALT CONCRETE INDUSTRY
EMISSION TEST REPORT
Mathy Construction Company
Plant 6
EMB File No. 91-ASP-10
Work Assignment 1.44
Contract No. 68-D-90Q54
Prepared for:
Dennis Holzschuh
Work Assignment Manager
Emission Measurement Branch, MD-14
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
Prepared by:
Radian Corporation
3200 E Chapel Hill Road/Nelson Highway
Post Office Box 13000
Research Triangle Park, North Carolina 27709
February 27, 1992
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TABLE OF CONTENTS
Section Page
1. INTRODUCTION ____ . ........................................ 1-1
1.1 Background ........................................... 1-2
1.2 Brief Process and Site Description ...... . ................... 1-3
2. SUMMARY OF RESULTS ...................................... 2-1
2.1 Emissions Test Log ........................... . ......... 2-2
2.2 Metal And Polynuclear Aromatic Hydrocarbon Results .......... 2-5
2.3 Paniculate Matter ...................................... 2-17
2.4 PM10/CPM Results ................................ . ____ 2-17
2.5 Aldehyde Results ...................................... 2-20
2.6 Continuous Emissions Monitoring Results .................... 2-31
3. FACILITY DESCRIPTION ...................................... 3-1
3.1 Process Description ..................................... 3-1
3.2 Process Conditions During Testing ........ . ................. 3-2
4. SAMPLING LOCATIONS ....................................... 4-1
5. SAMPLING AND ANALYTICAL PROCEDURES .................... 5-1
5.1 Particulate Matter And Metals Emissions Testing
Method .......................... ... ................ 5-1
5.2 Emissions Testing For Particulate Matter Less Than 10
Microns/Condensible Particulate Matter ..................... 5-18
5.3 Aldehydes Emissions Testing .............................. 5-28
5.4 Nonmethane Hydrocarbon Analysis By Method 25 A And C1-C6
By Method 18 ......................................... 5-35
5.5 EPA Methods 1-4 ...................................... 5-37
5.6 Continuous Emissions Monitoring Methods ... ................ 5-38
5.7 Polynuclear Aromatic Hydrocarbon Emissions
Testing .............................................. 5-46
5.8 ASTM Methods ........................................ 5-58
6. QUALITY ASSURANCE AND QUALITY CONTROL ................. 6-1
6.1 Quality Assurance/Quality Control Definitions
And Objectives . ................... , ................... 6-2
6.2 Manual Flue Gas Sampling Quality Assurance ................. 6-3
6.3 Analytical Quality Assurance .............................. 6-8
6.4 Continuous Emission Monitoring Quality Assurances ............ 6-15
6.5 GC Quality Assurance ............... , ................... 6-29
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TABLE OF CONTENTS, continued
APPENDICES
A EMISSIONS TESTING FIELD DATA SHEETS
A.1 PM/Metals
A.2 PM10/CPM
A3 Aldehydes
A.4 PAH
B PROCESS DATA SHEETS
C SAMPLE PARAMETER CALCULATION SHEETS
C.1 PM/Metals
C.2 PM10/CPM
C.3 Aldehydes
C.4 PAH
D CEM DATA
D.I CEM DAS Printouts
D.2 Stripchart Tracings
E GC DATA
F ANALYTICAL DATA
F.I PM/Metals
F,2 PM10/CPM
F.3 Aldehydes
F.4 PAH
F.5 Sample Log
G CALIBRATION DATA SHEETS
H SAMPLE EQUATIONS
I PROJECT PARTICIPANTS
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111
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TABLE OF CONTENTS, continued
SAMPLING AND ANALYTICAL PROTOCOLS
J.I PM/Metals
J.2 PM10CPM
J.3 Aldehydes
J.4 PAH
J.5 CEM and GC
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FIGURES
Page
1-1 General Process Flow Diagram for Batch-Mix Asphalt Plants 1-4
2-1 Emission Rates for PM10 (Ib/hr) , 2-23
2-2 Concentrations of PM10 (grains/dscf) 2-24
2-3 Filter Recoveries of Pm10 (in grams) 2-25
4-1 Sampling Location Arrangement , 4-2
4-2 Traverse Point Layout at Stack , 4-3
5-1 Schematic of Multiple Metals Sampling Train 5-2
5-2 Metals Sample Recovery Scheme 5-12
5-3 Metals Sample Recovery Preparation and Analysis Scheme 5-16
5-4 PM/CPM Sampling Train 5-19
5-5 PM10/CPM Sample Recovery Scheme 5-23
5-6 Pm10/CFM Analytical Scheme 5-26
5-7 Analytical Data Sheet 5-27
5-8 Aldehyde Sampling Train 5-29
5-9 Schematic of CEM System 5-36
5-10 PAH Sampling Train Configuration 5-47
5-11 PAH Field Recovery Scheme 5-53
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TABLES
2-1 Emissions Test Log 2-3
2-2 Summary of Metals/PM and PAH Emission Factors and Process
Operating Data 2-6
2-3 Metals Concentration Emission Rates 2-8
2-4 PAH Concentration Emission Rates 2-10
2-5 Ratio of Metals to Paniculate Matter 2-12
2-6 Metal Amounts in Flue Gas Samples by Sample Fraction - Blank
Corrected 2-13
2-7 Metals/PM Emissions Sampling and Flue Gas Parameters 2-14
2-8 PAH Amounts in Flue Gas Samples - Blank Corrected 2-15
2-9 PAH Sampling and Flue Gas Parameters 2-16
2-10 Paniculate Matter Concentrations Emissions 2-18
2-11 Summary of PM10/CPM Emission Factors and Process Operating Data .... 2-21
2-12 Pm10 Emissions Test Results 2-22
2-13 Summary of Aldehyde Emission Factors and Process Operating Data 2-26
2-14 Aldehydes Concentration and Emission Rates , 2-28
2-15 Aldehydes Amounts in Rue Samples - Blank Corrected 2-29
2-16 Aldehydes Emissions Sampling and Flue Gas Parameters . , , 2-30
2-17 Continuous Emissions Monitoring Daily Test Averages for
Actual Concentrations , 2-32
2-18 Hydrocarbon Emission Rates and Concentrations . 2-34
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TABLES, continued
3-1 Summary of Process Operating Data Collected During Emission
Testing - September 19, 1991 ..................... , . ............. 3-3
3-2 Summary of Process Operating Data Collected During Emission
Testing - September 20, 1991 .................................... 3-4
3-3 Summary of Metals and PAH Emission Factors and Process Operating
Conditions .................................................. 3-5
3-4 Summary of Aldehyde Emission Factors and Process Operating
Conditions .................................................. 3-6
3-5 Summary of PMi0/CPM Emission Factors and Process Operating
Conditions .................................................. 3-8
5-1 Sampling Checklist ........................................... 5-8
5-2 Approximate Detection Limits ................................... 5-15
5-3 CEM Operating Ranges and Calibration Gases ...................... 5-43
5-4 Glassware Cleaning Procedure ................................... 5-49
5-5 PAH Sample Components Shipped to Analytical Laboratory ............ 5-54
5-6 PAH Compounds Analyzed ..................................... 5-55
6-1 Summary of Precision, Accuracy, and Completeness Objectives ........... 6-4
6-2 Leak Check Results for Manual Sample Trains ...................... 6-5
6-3 Isokinetic Sampling Rates for Manual Sampling Test Run .............. 6-6
6-4 Dry Gas Meter Post-Test Calibration Results . ....................... 6-7
6-5 Metals Field Blank Results Compared to Test Run Results ............. 6-9
6-6 Metals Amount in Flue Gas Method Blank Result .................... 6-11
6-7 Metals Method Spike Results .................................... 6-12
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TABLES, continued
Page
6-8 PM10/CPM Field Blank Results Compared to Test Run Results 6-13
6-9 Aldehydes Field Blank Results Compared to Test Run Results 6-14
6-10 Aldehydes Flue Gas Method Blank Results , 6-16
6-11 Aldehydes Method Spike Results 6-17
6-12 PAH Field Blank Results Compared to Test Run Results 6-18
6-13 PAH Flue Gas Method Blank Results , , 6-19
6-14 PAH Method Spike Results 6-20
6-15 PAH Surrogate Recovery Results 6-21
6-16 Method 3A Oxygen Analyzer and Drift Summary , 6-23
6-17 Method 3A Carbon Dioxide Analyzer and Drift Summary 6-24
6-18 Method 10 Carbon Monoxide Analyzer and Drift Summary 6-25
6-19 Method 6C Sulfur Dioxide Analyzer and Drift Summary 6-26
6-20 Method IE Nitrogen Oxides Analyzer and Drift Summary 6-27
6-21 Method 25A Total Hydrocarbon Analyzer and Drift Summary 6-28
6-22 GC Response Factor Drift Values 6-30
JBS336 V1J1
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1. INTRODUCTION
Radian Corporation, under contract to the U.S. Environmental Protection
Agency's (EPA) Emission Management Branch (EMB), has conducted a testing program
to quantify the emissions of criteria and other air pollutants from the Mathy
Construction Company's Facility No. 6, a batch-mix asphalt paving plant located in
LaCrosse, Wisconsin. The results of this testing will become part of an updated emission
factors database, which will be used by the EPA's Emission Inventory Branch (EIB) to
update the asphaltic concrete plant section of the Compilation of Air Pollutant Emission
Factors, an EPA document commonly referred to as AP-42.
The specific pollutants of interest in the testing program were the following air
pollutants: particulate matter (PM); PM less than 10 ^m (PM10); condensible PM
(CPM); sulfur dioxide (SO2); nitrogen oxides (NOX); carbon monoxide (CO); total
hydrocarbons (THC); polynuclear aromatic hydrocarbons (PAH), excluding aldehydes
and ketones; and trace metals, excluding mercury (Hg). Mathy's Facility No. 6 was
selected as one of the two asphaltic concrete plants studied for the revision of AP-42
because it was judged by EMB and the National Asphalt Paving Association (NAPA) to
be representative of the processes, equipment configuration, and production rate of
batch-mix asphalt paving plants currently in use in the United States.
Testing was performed on September 19 through 20, 1991, and the principal
objectives of testing were the following:
• Determine levels of CO, SO2, NOX, and THC emitted from the plant stack.
• Determine the levels of toxic metals being emitted from the stack including
lead (Pb), chromium (Cr), cadmium (Cd), beryllium (Be), thallium (Tl),
arsenic (As), nickel (Ni), antimony (Sb), barium (Ba), silver (Ag), zinc
(Zn), phosphorus (P), copper (Cu), manganese (Mn), and selenium (Se).
The Hg levels were not analyzed because it was not expected to be present
in the process stream.
• Determine the filterable PM10 and CPM fractions emitted from the stack.
• Determine the levels of PAHs emitted from the stack.
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• Determine the quantities of benzene, toluene, xylene, and methane present
in the stack exhaust gas,
• Monitor the process operating conditions including aggregate flow rate,
moisture, and ambient moisture. Also, determine the fuel high-heating
value, and ultimate analysis.
In order to ensure repeatability of results, the measurements above were repeated
in triplicate at near-design operating conditions while the plant was operating on natural
gas,
The concentrations of CO2, O2, NOX, SO2, and CO in the flue gases were
determined using continuous emissions monitoring (CEM) systems designed in
accordance with EPA Methods 3A, 7E, 6C, and 10, respectively. Emissions of THC
were determined by CEM following EPA Method 25A. The EPA's Method 18 was
followed in the gas chromatography (GC) analysis for flue gas concentrations of benzene,
toluene, xylene, and methane. Samples of PM and metals were collected during three
sampling train runs, performed according to EPA Method 5/Combined Train SW 846
Test Method 0031. The EPA SW 846 Test Method 0010 and 0011 were used in the
collection of PAHs and speciated THCs, respectively. PM10 and CPM were sampled by
means of three test runs following a combination of protocols outlined in EPA
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continuous-ink plant and the other is the batch-mix plant. Following this precedent and
the recommendation of NAP A, EPA instructed Radian to direct its testing efforts at
these two types of plants. The testing program described in this report is one of two
testing programs being conducted by Radian in support of efforts to revise AP-42's
asphaltic concrete section. The other emissions tests were conducted on Mathy
Construction's Facility No. 26, a continuous-mix asphalt paving plant. Mathy Facility
No. 6, the plant discussed in this report, is a batch-mix plant. The plants owned and
operated by Mathy Construction Company have been recommended by NAPA to be
representative of both types of asphalt paving plants in the United States.
1.2 BRIEF PROCESS AND SITE DESCRIPTION
In general, batch-mix plants operate in the following manner. The cold feed
materials, known as aggregate, are sorted by size and stored in a series of bins that each
feed aggregate to a common conveyor belt. The aggregate is then dispensed from the
bins in a mix that achieves the desired aggregate size distribution and weight for the
batch of asphaltic concrete. The conveyor carries the aggregate to a rotating drum,
where it is mixed and dried at approximately 300°F. The dried aggregate is then carried
to a gradation control unit, which separates and stores the aggregate by size. The
necessary amount of each size of aggregate is then dropped into a weigh hopper and
then into a pug mill, where is it thoroughly mixed with hot liquid asphalt. The hot mix is
then transferred to storage silos, from which it is dispensed into paving trucks.
Figure 1-1 is a diagram of a generic batch-mix asphalt plant.
The burner in the drum dryer is natural gas fired. The air from this process is
drawn into the system by an exhaust fan located on the baghouse. After it passes
through the burner and mixing drum, the air passes through the baghouse. The air is
discharged to the atmosphere from a stack connected to the baghouse.
The stationary batch plant at Mathy Facility No, 6 has been rated at a
300 ton-per-hour production rate. Several factors affect this production rate. As a
stationary plant, Facility No. 6 operates only when there is a demand for asphalt. If
paving is stalled or slowed, the plant production must respond accordingly. Paving and
plant operation are also shut down during rainy periods. In addition, the burner for
JBS336 1~3
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drying the aggregate must be fired at a level suited to the moisture content and
composition of the aggregate being used.
The rest of this report is structured as follows. Section 2 contains a summary of
the test results. The process is discussed in Section 3, and the sample locations and
sampling and analytical procedures are presented in Sections 4 and 5, respectively.
Section 6 presents results of implementing the the quality assurance/quality control
(QA/QC) procedures followed in the test program. Section 7 contains references used
in developing this report. Appendices to this report include detailed methods and
procedures, field and laboratory data, and complete calculations used in deriving the
results presented here,
JBS336
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Benzaldehyde = 1.41 x KT1 Ib/ton of product;
Butyaldehyde/
Isobutyraldehyde = 0.428 x 10" Ib/ton of product;
Crotonaldehyde = 0.358 x 10" Ib/ton of product;
Formaldehyde = 19.4 x 10" Ib/ton of product;
Hexanal = 0.201 x 10" Ib/ton of product;
Methyl ethyl
ketone = 0.701 x 10" Ib/ton of product;
Propionaldehyde = 0.710 x 10" Ib/ton of product;
Quinone - 4.05 x 10" Ib/ton of product;
Valeraldehyde = 0.427 x 10" Ib/ton of product.
The following sections present more detailed summaries of the results of this test
program.
2.1 EMISSIONS TEST LOG
Emissions testing was conducted over a two-day period from September 19 to
September 20, 1991. Table 2-1 shows the emissions test log. This table shows the test
date, sample location, run number, test type, run times, and average production rate
during testing. Testing was performed using EPA manual test methods for six different
types of substances. Testing was conducted in triplicate for each type of analyte.
Particulate matter and metals were sampled in the same sampling train by
employing a combination of EPA Method 5 and EPA SW 846 Test Method 0031.
Particulate matter was determined gravimetrically from the front half filter catch then
combined with the back half for total metals analysis.
The PAHs was sampled concurrently with the PM and metals by EPA SW 846
Test Method 0010 using a dual probe arrangement. The dual probe arrangement
allowed both trains to operate side-by-side with their nozzles in approximately the same
sample location.
Sampling for aldehydes was conducted in a separate train using EPA SW 846 Test
Method 0011.
Testing for PM10 and CPM was performed in a single train employing a
combination of EPA Method 201A and EPA Method 202. An in-stack cyclone with a
backup filter composed the front half of this train. The cyclone captured PM greater
than 10 microns. The backup filter caught PM of 10 microns or less. The CPM was
caught in the back half impingers.
JBS336
2-2
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Table 2-1. Emissions Test Log
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JBS336
2-3
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Table 2-1, continued
Date
09/19/91
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Exact times GC samples were shot. Individual results were averaged over the time period during which
manual sampling was conducted.
JBS336
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2. SUMMARY OF RESULTS
This section provides results of the emission test program conducted at Mathy
Construction Company's Plant 6 from September 19 to September 20, 1991. Included in
this section are results of manual tests conducted for trace metals excluding Hg, PM,
PM,0> CPM, aldehydes and ketones, and PAHs. This section also contains the results of
the continuous emissions monitoring for CO2/O2, CO, SO2, NOX, and THC gases as well
as gas chromatography (GC) results for benzene, toluene, xylene, and methane.
Stated briefly, the significant emissions from Mathy Construction's Plant 6 are as
follows:
» Of the 15 metals analyzed, 9 were found in detectable quantities. Their
emission rates are:
Ba = 1.23 x W* Ib/ton of product;
Cd = 0.351 x 10* Ib/ton of product;
Cr = 0.810 x 10-6 Ib/ton of product;
- Cu = 1.86 x 10"6 Ib/ton of product;
Pb « 1.02 x 10"6 Ib/ton of product;
Mn = 11.8 x W* Ib/ton of product;
Ni = 6.39 x 10"6 Ib/ton of product;
Ag = 0.621 x W6 Ib/ton of product;
Zn = 6.29 x W6 Ib/ton of product.
• Of the 19 PAHs analyzed, 2 were found in detectable levels. Their average
emission rates are:
2-Methylnaphthalene = 0.117 x 10"4 Ib/ton of product;
Naphthalene = 0.320 x 10"4 Ib/ton of product.
• For PM and PM10 (actually PMg; see explanation in Section 2.4.1), the
average emission rates are;
PM = 0.005 Ib/ton of product;
PM10 = 0.008 Ib/ton of product.
• Of the 18 aldehydes analyzed, 11 were found in detectable quantities.
Their average emission rates are:
Acetaldehyde = 6.92 x 1Q4 Ib/ton of product;
Acetone = 105 x 10J Ib/ton of product;
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Eleven other analytes were sampled for by a combination of CEM and GC
instruments. These tests were conducted concurrent with the manual method tests to the
extent possible. Continuous emissions monitoring was operated continuously and results
were averaged over the manual test period in which they were performed. Gas
chromatography measurements were taken on a semicontinuous basis and multiple
readings were averaged over the manual test period in which they were performed.
2.2 METAL AND POLYNUCLEAR AROMATIC HYDROCARBON RESULTS
2.2.1 Overview
The PM/metals and PAH manual sampling trains shared a dual-probe
arrangement, which allowed testing to be conducted simultaneously in separate trains at
the same port location. The PM/metals sampling train was used to determine emission
rates of 15 metals (Sb, As, Ba, Be, Cd, Cr, Cu, Pb, Mn, Ni, P, Se, Ag, Tl, and Zn) and
PM. The PAH sampling train was used to quantify emission rates of 19 PAHs
(aeenaphthylene, ancenaphthene, anthracene, benzo(a)anthraeene, benzo(a)pyrene,
benzo(b)fluoranthene, benzo(g,h,i)perlyene, benzo(k)fluoranthene, ehrysene,
dibenz(a,h)anthraeene, dibenzofuran, 7,12-dimethyibenz(a)anthracene, fluoranthene,
florene, indeno(l,2,3-cd)pyrene, 2-methylnaphthalene, naphthalene, phenanthrene, and
pyrene).
Three manual sampling runs for PM/metals and PAHs were performed to ensure
representative test results. The back half sample bottle from Run 2 was broken during
shipment, so only the front half was analyzed for PM and metal content.
Section 2.2 presents process operations. The average emission rates in ^g/dscm,
corrected to 7 percent O2, and g/hr are summarized in Section 2.2.3. The metals-to-PM
ratios are presented in Section 2.2.4, and flue gas-by-sample fractions are presented in
Section 2.2.5.
2.2.2 Process Operation
Table 2-2 summarizes the metals and PAH emission factor results with the
process operating data. Sampling was performed in two separate trains simultaneously
using a unique dual-probe arrangement. Total asphaltic concrete production varied
between 222 tons/hr and 245 tons/hr (73 to 82 percent of capacity), while natural gas
JBS336 2-5
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Table 2-2
SUMMARY OF METALS/PM AND PAH EMISSION FACTORS AND PROCESS OPERATING DATA
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Dale
Production Rale (tons/nr)
Virgin Asphalt Rate (tons/Jir)
Recycled Asphalt Race (tons/lir)
Asphalt Cement Rale (lons/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Fuel Flow (cubic fool/hr)
Heai Imput Rate (1000 cubic fooi/hr)
Burner Setting - Flame Meter (%)
Ambient Temperature (depee F)
Ambient Humidity (%)
Kiln Exit Temperalure (degree F)
Slack Flow Rale (dscfrn)
Stack Flow Rale (dscf/ton of product)
Stack Terrtperatrue (degree F)
Slack Moisture (% volume)
Slack CO2 (volume % dry)
Stack O2 (volume % dry)
Stack CO (ppmV)
Control Device
Barium (Ibs x 10(-6)/ton of product) *
Cadmium (Ibs x 10(-6)/lon of product) *
Chromium (Ibs x 10(-6)/ton of product) '
Copper (Ibs x 10(-6)/ton of product) "
Lead (Ibs x IO(-6)/ton of product) •
Manganese (Ibs * 10("6)/lon of product) "
Nickel (Ibs x IO(-6)/lon of product) •
Silver (Ibs x lO(-6)/ion of product) *
Zinc (Ibs x 10(-6)/lon of product^'
Particulate Matter (Jbs/ion of product)
2-McihylnaphthaIene (Ibs x I0(^t)/ton of product) ••
(Ibs x 10 (-4)/1000 cubic fool) ' '
Naphthalene (Ibs x 10(^)/ton of product) "
(Ibs x 10 (-4)/lOOO cubic foot) "
^iislis^sisisS
09/19/91
245
230.8
0
14,2
82
4-3
S2SO
5-25
78
43
&5
339
342SO
8390
240
27-5
S.7
14.1
> 1000
Baghouse
1.27
0,477
1.47
1.82
0.150
16.0
12.5
0.862
4.69
0.00690
0.116
5,42
ND
ND
09/19/91
244
229.8
0
14.2
81
4J
5280
5.28
80
51
54
341
32660
8030
236
28.4
S.S
12.5
> 1000
Baghousc
0.785
ND
ND
ND
ND
7.05
ND
0.381
ND
0,00386
0.100
4.63
ND
ND
09/20/91
222
209,1
0
12.9
73
4.4
5190
5.19
81
53
70
349
31570
8530
244
28,1
5.2
14,2
1362
Baghousc
1.64
0.225
0.151
1.90
1.90
12.4
0.246
ND
7.90
0.00500
0.133
5.69
0.320
13.7
237
223.2
0
13.8
79
4.3
5240
5.24
80
49
70
343
32840
8320
240
28.0
5.6
13.6
1362
1.23
0.351
0.810
1.86
1.02
11.8
6.39
0.621
6.29
0.00595
0.117
5.25
0.320
13.7
ND-NuDclconl
• - 11 !<>(-«) or (O.Onni}
" - i I KH^torjaML'll
NOTE - Run averaga vtn calculated (mm reading! laken periodically throughout the duration of tbe m
Sec Table 3-1 nod J-2 for u» individual rudrngi.
Mciab and PAH compound! analyzed, but not deuued, are not included in tbii uble.
oonccnmuoni have Bern blank carrcoed.
2-6
-------
consumption ranged from 5190 ft3/hr to 5280 ft3/hr. Metals emissions from this facility
are generally associated with aggregate processing because natural gas is used exclusively
in the kiln. Facilities that alternate fuels may realize different or increased metal
emission factors because of the chemical composition of fuel oils, which can be burned
in similar kilns. Therefore, these results are only applicable to natural gas-fired kilns
and not fuel oil systems.
The PAH emissions from asphaltic concrete plants may originate from fuel
combustion; the volatile fraction of the asphalt cement, if any; and organic residues
commonly found in recycled asphalt (i.e., gasoline, engine oils). No recycled asphalt was
processed during these tests, nor were data found in the literature indicating the
contribution of PAH from asphalt cement. Therefore, the emission factors presented are
expressed in Ib/ton of product and lb/ft3 of natural gas consumed. The former units
allow for an unknown volatile fraction to be present in the asphalt cement, whereas the
latter units assume no volatile fraction in the asphalt cement and that all PAHs result
from fuel combustion in the kiln. In either case, the emission factors do not apply to
product containing recycled asphalt. During the emission tests, the plant was operating
at the normal plant capacity, with Run 1 at 82 percent, Run 2 at 81 percent, and Run 3
at 73 percent. This allows a comparison of the emission tests during the three runs. The
production rates were 245 tons/hr, 244 ton/hr, and 222 tons/hr for Runs 1, 2, and 3,
respectively.
Only the metals and PAHs detected are given in Table 2-2, The other metals and
PAHs were analyzed, but they were not collected in detectable amounts. Nine metals of
the 15 analyzed were detected (Ba, Cd, Cr, Cu, Pb, Mn, Ni, Ag, and Zn). Only 2 of the
22 PAHs analyzed were detected. These were 2-methylnaphthalene and naphthalene.
The PAHs detected were blank corrected and reported as shown.
2.2.3 Emissions
Metals
Table 2-3 presents the metals emissions results for the test conditions. Also
shown for each run are the date, metered volume (in dscm), O2 concentration, and flue
gas flow rate. Flue gas concentrations are given in terms of /^g/dscm and //g/dscm
JBS336
-------
Table 2-3
METALS CONCENTRATION EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Barium
Cadmium
Chromium
Copper
Manganese
Nickel
Silver
Zinc
(ug/dscm)
{ug/dscm @ 7% O2)
(g/hr)
(ug/dscm)
(ug/dscm @ 7% Q2)
(g/hr)
(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)
(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)
(up/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)
(ug/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)
2,46
5.11
0.141
0.932
1.92
0.0530
2.87
5.91
0.163
3J6
7.32
0.202
0.293
0.603
0.0167
31.2
64.2
1.77
24J
50.4
1.39
1.68
3.47
0.0958
9.17
18.9
0.521
1.60
2.65
0.0368
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
14.4
23.8
0.780
ND
ND
ND
0.775
1.29
0.0421
ND
ND
ND
3,13
6,57
0.165
0.429
0.900
0.0227
0.2S8
0.603
0.0152
3.63
7.61
0.192
3.62
7.58
0.191
23.7
49.7
1.25
0.469
0,983
0.0245
ND
ND
ND
IS.l
31.6
0.795
2.40
4.78
0.131
0.680
1.41
0.0378
1J8
3.26
0.089
3.59
7.47
0.197
1.95
4.09
0.104
23.1
45.9
1.27
12J
25.7
0.709
1.23
2,38
0.0689
12.1
25.2
0.658
ND = Noc Detected
NOTE: Hun 2 impingcr umple bonle broke during shipment, therefore, only the from
hall a recorded. The ivcrage b baud on Rum 1 and 3.
MclaJs inalyzed, bui DOI delected, an DOI included in lh» lablr.
2-8
-------
corrected to 7 percent O2. Oxygen concentrations were determined from CEM data (see
Section 2.6). It should be noted that Run 2 results are from the analysis of the front half
only because of sample breakage. Therefore, Run 2 was not used in averaging the runs,
During the emission tests, Mn had the highest average mass rate with 1.27 g/hr,
followed by Ni with 0.709 g/hr. These emission rates correspond to an average emission
factor of 11,8 x 10"6 Ib/ton of product and 6.39 x W4 Ib/ton of product. After blank
correction, Sb, As, Be, P, Se, and Tl were not collected in detectable amounts for any of
the runs during these emission tests. Metal values ranged from 1.77 g/hr of Mn in
Run 1, to 0.0152 g/hr of Cr in Run 3.
The metal values for the emission tests are not significantly different between
Runs 1 and 3, except for Cd, Pb, and Ni. Cadmium fluctuated from 0.0690 to 0.104 g/hr.
Lead fluctuated from 0.0911 g/hr to 0.259 g/hr. Nickel fluctuated from 0.169 to
1.53 g/hr.
Polynuclear Aromatic Hydrocarbons
Table 2-4 presents the PAH emission results for three test runs. Also shown for
each run are the date, metered volume, O2 concentration, and flow rate. Flue gas
concentrations are given in terms of g/dscm and g/dscm corrected to 7 percent O2.
Oxygen concentrations were collected from CEM data.
During the emission tests, naphthalene had the highest average mass rate with
23.2 g/hr, followed by 2-methylnaphthalene with 12.5 g/hr. These emission rates
correspond to average emission factors of 13,7 x W4 lb/1000 ft3 of natural gas and
5.25 x 10"4 lb/1000 ft3 of natural gas, respectively. It should be noted that these
compounds may be a degradation by-product of the XAD absorbent used in the sample
train. However, these results have been blank corrected and are reported as shown.
The other compounds listed were not collected in detectable amounts for any of these
emission tests. The PAH values ranged from 23.2 g/hr of naphthalene in Run 3 to
11.1 g/hr of 2-methylnaphthalene in Run 2.
The PAH values for the emission tests did not change significantly from Runs 1 to
3, except for naphthalene, which was detected in Run 3, but not in Runs 1 or 2.
2-9
JBS336 ^ •*
-------
Table 2-4
PAH CONCENTRATION EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
2-Methylnaphthalene (ug/dscm)
(ug/dscm @ 1% O2
(g/hr)
Naphthalene
(ug/dscm)
(ug/dscm @ 7% O2
(g/hr)
222
456
12.9
ND
ND
ND
199
331
11,1
ND
ND
ND
250
525
13.4
432
905
23.2
224
437
12.5
432
905
23.2
ND = Not Detected
NOTE; Concentrations given have been blank corrected. PAH compounds analyzed, but not detected, are not included
in this table.
2-10
-------
2.2.4 Ratios of Flue Gas Metals to Particulate Matter
A summary of the ratios of metals to PM for the emission tests is presented in
Table 2-5. Metals-to-PM ratios are given in units of milligrams of metals per gram of
PM collected by the sampling train. The values ranged from 0.0217 mg of Pb per gram
of PM during Run 1 to 2.49 mg of Mn per gram of PM during Run 3. Manganese had
the highest ratio for Run 1 with 2.31 mg metal/gram PM.
2.2.5 Flue Gas Sampling Fraction and Sample Parameters
Metals
Table 2-6 presents the metal amounts in the flue gas samples by fraction for the
emission tests. All metals detected were collected in the highest proportions in the front
half (filter, nozzle/probe rinse), except for Cu, which was collected in the highest
proportions in the back half fraction. Laboratory analytical results for each sample
fraction are presented in detail in Appendix E.I.
Sampling and flue gas parameters for the PM/metals runs are shown in Table 2-7.
Total sampling times, sample volume, and isokinetic results for each sampling run are
presented. Appendix C,l contains a complete listing of these and additional sampling
and flue gas parameters for each run. The field data sheets are contained in
Appendix A.l.
Polvnuclear Aromatic Hydrocarbons
Table 2-8 presents the PAH amounts in the flue gas sample for the emission tests
in total fig for each run. Laboratory analytical results for each sample are presented in
detail in Appendix E.4.
Sampling and flue gas parameters for the PAH runs are shown in Table 2-9.
Total sampling times, sample volume, and isokinetic results for each sampling run are
presented. Appendix A.4 contains a complete listing of these and additional sampling
and flue gas parameters for each run along with the field data sheets.
JBS336
-------
Table 2-5
RATIO OF METALS TO PARTICULATE MATTER
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Barium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Silver
Zinc
0.184
0.0692
0.213
0.264
0.0217
2.31
1.82
0.125
0.681
0.203
ND
ND
ND
ND
1.82
ND
0.0985
ND
0,329
0.0451
O.Q302
0,382
0,380
2.49
0.0493
ND
1.58
0.239
0.0571
0.122
0.323
0.201
2.21
0.934
0.112
1.13
ND = Not Detected
NOTE: Run 2 impinger sample bottle broke during shipment. Therefore,
only the front half is recorded. The average is based
on Runs 1 and 3.
Metals analyzed, but not detected, are not listed in this table.
Participate matter is based on the front half ony.
2-12
-------
K>
Table 2-6
METAL AMOUNTS IN FLUE GAS SAMPLES BY SAMPLE FRACTION - BLANK CORRECTED
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
ND
ND
4.35
ND
1.35
3.97
ND
ND
53.1
41.7
ND
ND
2.95
ND
2.20
ND
ND
ND
ND
0.282
1.06
6.23
0.513
1.56
1.22
ND
ND
ND
ND
13.9
ND
4.35
ND
1.63
5.03
6.23
0.513
54.6
42.9
ND
ND
2.95
ND
16.1
ND
ND
2.68
ND
ND
ND
ND
ND
24.1
ND
ND
ND
1.30
ND
ND
ND
ND
4.70
ND
ND
ND
ND
4.61
36.6
ND
ND
ND
ND
ND
13.4
ND
ND
0.410
ND
0.700
0.469
5.92
1.29
2.09
0.765
ND
ND
ND
11.2
ND
ND
5.11
ND
0.700
0.469
5.92
5.90
38.7
0.765
ND
ND
ND
ND
24.6
NOTE: Run 2 impinger sample bottle broke during shipment, Therefore, only the from half is recorded, The average is based on Runs 1 and 3.
ND = Not Deieci&d
-------
Table 2-7
METALS/PM EMISSIONS SAMPLING AND FLUE GAS PARAMETERS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Total Sampling Time (min)
Average Sampling Rale (dscfm)
Metered Volume (dscf)
Meiered Volume (dscm)
Average Stack Temperature (F)
O2 Concentration (%V)
CO2 Concentration (%V)
Stack Gas Moisture (%V)
Volumetric Row Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Particulate Catch (grams)
125
0.490
61.9
1.752
241
14.2
5.6
29.7
33350
948
104
0.0236
125
0.470
59.2
1.677
236
12.5
5.8
29.3
32000
906
104
0.0132
125
0.460
57.6
1.631
245
14.3
5.4
29.3
31100
880
104
0.0155
NA
0.473
59.6
1.687
241
13.7
5.6
29.4
32200
911
NA
0.0174
NOTE: Run 2 impmger sample bottle broke during shipment.
NA = Not Applicable
2-14
-------
TABLE 2-8
PAH AMOUNTS IN FLUE GAS SAMPLES - BLANK CORRECTED
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
^^^^^^ii^^^^^^^^^^^^M^^^^^^^^^^^^^^
's^^^^M^K^i^^^Sim^^^^^SS^i^^^^m
-Vftayf&sW&^iv&gv^';*^
Acenaphthylene
Acenoaphthene
Anthracene
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
2-ChIoronapthalene
Chrysene
Dibenz(a,h)anthracene
Dibenzofuran
7,l2-Dimethylbenz(a)anthracene
Fluoranthene
Fluorene
Indeno(l,2,3-cd)pyrene
2-Meihylnaphthalene
Naphthalene
Perylene
Phenanthrene
Pyrene
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
408
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
348
ND
ND
ND
ND
jpstsij-M^^
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
417
719
ND
ND
ND
mm'msm&iifffxis-K-isx-'if:
f&&tej8&&&im&&^tty&^
•W>frWwSKflTO'{>>>K'!-&X»KjC'»K--:->>W1>--'.
!O?C«£'j»^W.<>XjK;!-X-:->:':v:-:<;-;:;:-:<:l;:>>;
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
(2,36)
751
ND
ND
ND
( ) = Estimated Value
ND = Noi Deiected
2-15
-------
Table 2-9
PAH SAMPLING AND FLUE GAS PARAMETERS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Total Sampling Time (min)
Average Sampling Rate (dscfm)
Metered Volume (dscf)
Metered Volume (dscm)
Average Stack Temperature (F)
O2 Concentration (%V)
CO2 Concentration (%V)
Stack Gas Moisture (%V)
Volumetric Row Rate (dscfm)
Volumetric P.ow Rate (dscmni)
Percent Isokinetic
125
0.520
65.0
1.840
240
14.2
5.6
27.5
34300
971
107
125
0.490
61.6
1.745
236
12.5
5.8
28.4
32600
925
106
125
0,470
58.8
1.665
244
14.3
5.4
28.1
31600
894
105
NA
0.493
61.8
1.750
240
13.7
5,6
28.0
32800
930
106
NA = Not Applicable
2-16
-------
2.3 PARTICULATE MATTER
2.3.1 Overview
Particulate matter emissions were measured using the front half participate catch
collected in the combined PM/metals train. Before metals speciation analysis, the filter
and front half acetone rinse (e.g., rinsate from nozzle, probe, and filter holder) were
analyzed gravimetrically as described in Section 5. The sampling and flue gas
parameters have been presented previously in Table 2-5. Detailed sampling parameters
are provided in Appendix C.I and analytical results in Appendix E.I.
2.3.2 Particulate Matter Results
Table 2-10 summarizes the results of the gravimetric analyses. Exhaust grain
loadings, corrected to 7 percent O2> ranged from 0,0057 gr/dscf to 0.0121 gr/dscf with an
average of 0.0089 gr/dscf, and emission rates ranged from 0.941 Ib/hr to 1.69 Ib/hr with
an average of 1.24 Ib/hr.
Table 2-2 summarizes emission factors for total PM which varied from
0.00386 Ib/ton of product to 0.00690 Ib/ton of product with an average of 0,00595 Ib/ton
of product. The variance may be related to transient emission conditions associated with
process start-up, which coincided with sampling Run 1. The emission factors generated
from sampling Runs 2 and 3 are in relatively close agreement, whereas the first run
emission factor represents the high endpoint of the data set.
These emission factors are less than those currently published in AP-42
(0.02 Ib/ton after baghouse control, from data from circa 1973-74). This difference may
be attributable to a variety of factors, including product specifications for different
testing programs or differences in baghouse design, operation, and maintenance between
facilities tested.
2.4 PM10/CPM RESULTS
2.4.1 Overview
Three test runs were conducted to determine the concentration and emission rate
of PM10. The testing procedures followed EPA Method 201A for the determination of
PM10 emissions using the constant sampling rate (CSR) procedure coupled with EPA
Method 202 for determining condensible emissions from the impinger's back half. The
JBS336 2-17
-------
N>
i—>
oe>
Table 240
PARTICULATE MATTER CONCENTRATIONS EMISSIONS
MATHY CONSTRUCTION COMPANY PLANT6 (1991)
-------
CSR employs normal isokinetic sampling procedures except that the sample duration at
each sampling point is proportional to the gas velocity at that point.
It should be noted that the smaller PM10 nozzles that would allow 100 percent
isokinetic sampling and a cut size at 10 microns were several inches longer than a
standard nozzle and would have required a 4-in. ID sampling port. The existing ports
were only 3 in. ID, and therefore, a nozzle with a shorter, larger diameter had to be
used. This resulted in a PM cut size of 7.9 microns rather than the expected 10 microns.
The net effect on the results is that the fraction of PM present between 7.9 and
10 microns cannot be determined from the data collected. Therefore, these results are
not comparable to PM10 data collected from other similar facilities, if they were collected
at the targeted 10-micron cut size.
A full description of the method procedures can be found in Section 5 as well as
in the EPA Reference Method located in Appendix 1,2. The final results from this test
procedure are presented in terms of the phase of PM caught as well as the cut
size. The following PM weight fractions were determined:
• Noncondensible PM > 8 microns (cyclone fraction);
• Noncondensible PM < 8 microns (filter fraction);
• Inorganic CPM associated with the water fraction (< 8 microns); and
• Inorganic CPM associated with the methylene chloride fraction
(<8 microns).
Stack gas velocities measured prior to PM10 sampling were up to 15 percent
higher than those recorded for the other sampling trains. This difference may have
resulted from reduced dampening of the exhaust between the fan and the sampling ports,
but this is not certain. All other process parameters (e.g., production rates, fuel
consumption rates, aggregate moisture) appear comparable to those monitored for the
other tests.
2.4.2 PMB Emissions
The average emission rate and emission factor for PM less than 8 microns were
equal to those for PM greater than 8 microns (1.65 Ib/hr and 0.008 Ib/ton of product,
2-19
JBS336 *• i7
-------
each). Although the PM8 emissions ranged from 45 to 55 percent of the total PM
measured, the equal distribution of emissions above and below the cut size may be
coincidental because only Runs 2 and 3 measured condensible emissions in both the
water and methylene chloride fractions. No organic condensibles were found in the
methylene chloride fraction of Run 1. This anomaly may be related to the process
conditions or possible sampling or analytical errors, but a specific cause is not apparent.
Table 2-11 summarizes the PM10 emission factors and process operating data.
Table 2-12 summarizes the analytical results, and Figure 2-1 illustrates the particle size
contributions to mass emission rates. Figure 2-2 shows the particle size contributions to
flue gas PM concentrations under actual conditions and conditions corrected to 7 percent
O2. Figure 2-3 illustrates the relative contribution of each sample fraction to total PM
catch for each sample run.
2.5 ALDEHYDE RESULTS
2.5.1 Overview
A single sampling train was used to collect samples for analysis for 18 aldehydes
(acetaldehyde, acetone, acetophenone/o-tolualdehyde, acrolein, benzaldehyde,
butyraldehyde/isobutyraldehyde, crotonaldehyde, 2,5-dimethylbenzaldehyde,
formaldehyde, hexanal, isophorone, isovaleraldehyde, MIBK/p-tolualdehyde, methyl ethyl
ketone, propionaldehyde, quinone, m-tolualdehyde, and valeraldehyde). Three sampling
runs were performed in order to ensure representative test results.
2.5.2 Process Operation
Table 2-13 presents the aldehyde emission factors with a summary of process
operating data for the three test runs. During the emission tests, the plant was operating
at slightly below normal load of 76 and 65 percent for Runs 1 and 3, but at a normal
load of 95 percent for Run 2. Therefore, only Runs 1 and 3 will be used in averaging
the operating data. The production rates were 229 tons/hr, 284 tons/hr, and 194 tons/hr
for Runs 1, 2, and 3, respectively. Natural gas consumption varied from 5000 ft3/hr
(Run 3) to 6947 ft3/ft/hr (Run 2).
Only the aldehydes detected are presented. The other aldehydes were analyzed,
but they were not collected in detectable amounts. Of the 18 aldehydes analyzed,
JBS336
2-20
-------
Table 2-11
SUMMARY OF PM10/CPM EMISSION FACTORS AND PROCESS OPERATING DATA
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Daie
Production Rate (tons/hr)
Virgin Asphalt Rate (tons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cement Rate (tons/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Fuel Flow (cubic fooi/hr)
Heat Impul Rate ( 1000 cubic foot/hr)
Burner Setting - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exit Temperature (degree F)
Stack Flow Rate (dscfm)
Stack Flow Rate (dscf/ton of product)
Stack Tempeiatrue (degree F)
Stack Moisture {% volume)
Stack CO2 (volume % dry)
Stack O2 (volume % dry)
Stack CO (PPmV)
Control Device
Paniculate Emissions < Cut Size (Ibs/ton of product)
Paniculate Emissions > Cut Size (Ibs/ton of product)
Parliculate Emissions Total (Ibs/ton of product)
09/19/91
224
211
0
13
75
4.3
5180
5.18
74
51
57
340
33530
8981
241
28.5
5.1
14.1
> 1000
Baghouse
0.009
0.008
0.017
09/20/91
213
200.6
0
12.4
71
4.4
4990
4.99
79
53
61
350
32660
9200
255
28.5
5.4
14
1496
Baghouse
0.007
0.008
0.015
v5Wft'9SJ<<:*flJKi:JiSjSjiw
:*5>:^>:j^K5Jj^.j!j3^^!5f5;
09/20/91
215
202.5
0
12.5
72
4.7
5230
5.23
76
58
46
348
32100
8960
242
27.6
5.6
13.6
1567
Baghouse
0.007
0.007
0.014
217
204.7
0
12.6
73
4.5
5130
5.13
76
54
55
346
32840
8320
246
28.2
5.4
13.9
1532
0.008
0.008
0.016
NOTE - Run averages were calculated from readings taken periodically throughout ihe duration of (he
See Table J-I and J-2 (or the individual reading.
emission test run.
2-21
-------
Table 2-12
PM10 EMISSIONS TEST RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Corrected Barometric Pressure (in. Hg)
Stack Static Pressure (in. H2O)
Average Stack Temperature (degree F)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Stack Moisture (%V)
Stack Gas Velocity, Vs (fps)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (dscfm)
Stack Viscosity (micropoise)
$5[g;«ft|jfe>ij^:;;J:jj:5g?;
•; jjw £JK£ KjUEft!" Jfc8:<'%'
29.68
0.80
241
5.10
14.12
80.78
28.5
75.6
63500
34000
199
»>j;W::JPWHPll Cut Size (grains/dscf)
Particulate Cone. > Cut Size (grains/dscf @7%
Particulate Cone. Total (grains/dscf)
Paniculate Cone. Total (grains/dscf @7% O2)
Particulate Emissions < Cut Size (Ibs/hr)
Particulate Emissions > Cut Size (Ibs/hr)
Particulate Emissions Total (Ibs/hr)
7.80
0.0111
0.0034
0.0101
0.0000
0.0246
0.0071
0.0145
0.0058
0.0120
0.0129
0.0265
2.07
1.70
•3.77
7.82
0.0102
0.0029
0.0037
0.0015
0.0183
0.0047
0.0098
0.0059
0.0124
0.0106
0.0222
1.39
1.75
3.14
8.04
0.0074
0.0020
0.0038
0.0016
0.0148
0.0047
0.0089
0.0047
0.0089
0.0093
0.0177
1.49
1.49
2.98
7.89
0.0096
0.0028
0.0059
0.0010
0.0192
0.0055
0.0111
0.0055
0.0111
0.0110
0.0221
1.65
1.65
3.30
2-22
-------
8 microns
Run 1 Run 2 Run 3
* Sample port and nozzle considerations reduced cut size to approximately 8 microns.
Figure 2-1. Emission Rates for PMjQ (in Lbs/hr)
Mathy Construction Company Facility No. 6
2-23
-------
< 8 microns
> 8 microns
NOTE: Values
reported in
grains/dscf and in
grains/dscf at
7%02.
Run 1 Run 2 Run 3
(at 7% O2) (at 7% O2) (at 7% 02)
• Sample port and nozzle considerations reduced cut size to 8 microns.
Figure 2-2. Concentrations of PM^Q (in grains/dscf)
Mathy Construction Company Facility No. 6
2-24
-------
0.025i
0.02-
0.015-
0.01-
0,005-
40.0246
MeC! Back Half
H2O Back Half
PM10 Filter
Cyclone
Run 1 Run 2 Run 3
* Sample port and nozzle considerations reduced cut size to approximately 8 micorns.
Figure 2-3. Filter Recoveries of PMj^ (in grams)
Mathy Construction Company Facility No. 6
2-25
-------
Table 2-13
SUMMARY OF ALDEHYDE EMISSION FACTORS AND PROCESS OPERATING DATA
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Date
Production Rate (ton/hr)
Virgin Asphaii Rate (jion/hr)
Recycled Asphalt Rale (lon/hr)
Asphalt Ccmeni Rate (lon/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Fuel Flow (cubic foot/hr)
Heat Imput Rate (1000 cubic fooi/hr)
Burner Setting - Rame Meter (%)
Ambient Temperature ^degree F)
Ambient Humidity (%)
Kiln Bitit Temperature (degree F)
Slack Flow Rate (dscfm)
Stack Flow Rate (dscf/ton of product)
Stack Temperature (degree F)
Stack Moisture (% volume)
Stack CO2 (volume % dry)
Stack O2 (volume % dry)
Stack CO (ppmV)
Control Device
Acetaldchydc (Ibs x lO(-4)/ton of product) "
(Ibs x 10(-4)/100Q cubic foot) "
Acetone (Ibs x 10(-4)/ton of product) *
(Ibs x 10H)/1000 cubic foot) "
BenzaWehyde (Ibs x 10(-4)/ton of product) "
(!bs x 10H)/1000 cubic foot) '
Butyraldehyde/Isobutyraldehyde (Ibs x 10(-4)/ton of product) "
(Ibs x IO(-4)/lOOO cubic foot) '
Crotonaldehyde (Ibs x 10(-4)/ion of product) "
(Ibs x 10{-0/1000 cubic foot) »
Formaldehyde (Ibs x 10(-4)/ion of product) *
(Ibs x 10(-4)/1000 cubic foot) «
Hexanal (Ibs x 10(-4)/ion of product) *
(Ibs x 10(-4)/1000 cubic fool) •
Methyl Ethyl Kctone (Ibs x 10(-4)/lon of product) *
(Ibs x 10(-4)/1000 cubic foot) '
Propionaldehyde (Ibs x 10(-4)/ton of producl) *
(Ibs x 10(-»)/1000 cubic foot) '
Quinone (Ibs x 10(-4)/ion of product) "
(Ibs x 10(-4)/100Q cubic fool) '
Valeraldehyde (Ibs x 10(-4)/ton of product) *
(Ibs K lQ(-4)/lOOQ cubic fool) *
09/19/91
229
215.7
0
13.3
76
4.3
5393
5.39
70
49
58
341
33187
8695
240
28-7
6,3
13.5
> 1000
Baghouse
5.07
215
105
4460
1.23
52.2
0.290
12.3
0.229
9.72
1S.1
770
0.251
10.7
ND
ND
ND
ND
0.301
12.8
ND
ND
09/20/91
284
2675
0
165
95
4.7
6947
6.95
84
40
80
347
32988
6969
238
295
6.6
12.4
> 1000
Baghouse
5.35
219
235
962
1.02
41.8
ND
ND
0.152
6.22
23.0
941
0.323
13.2
ND
ND
ND
ND
0.139
5.69
ND
ND
09/20/91
194
182.7
0
11-3
65
4.7
5000
5.00
75
58
46
348
32475
10044
234
27.1
5.6
13.6
1567
Baghouse
8.78
341
ND
ND
158
61.4
0566
21.9
0.488
18.9
20.7
803
0-150
5.82
0.701
27.2
0.710
275
7.80
303
0-427
16.6
Illpeiiiii
212
199.2
0
12.3
71
45
5197
5.20
73
54
52
345
32831
9370
237
27.9
6.0
136
1567
6.92
278
105
4460
1.41
56.8
0.428
17.1
0,358
14.3
19.4
787
0.201
8.24
0.701
27.2
0.710
275
4.05
158
0.427
16.6
ND a Not Detected
* •» Iil0(-4)ofa0001
NOTE; Run averages were calculated from reading! taken periodkaEly ibrougboui Ube dura [kin of ihe exDutuon leu run.
See Table 3-1 and 3-2 for the individual neadlop.
Aldehyde compound! analyzed, but not deteaed, are net ineiuded in tbli table.
Aldehyde compound eoaeencraEiicinj bjvc feecti blank corrected
Run 2 w&i noc calculated in the average. Rum 1 &. 3 were « 3 minimum prodyciion bad, whcrem Run 1 wu at a maximum producUon load
AJ! iftree tdU were imenrupted by plam ihytdown, Traini were removed from ti&dL ind were not operated dunng down LUEOCI.
2-26
-------
11 were detected. These were acetaldehyde, acetone, benzaldehyde, formaldehyde,
cutyraldehyde/isobutyraldehyde, crotonaldehyde, hexanal, methyl ethyl ketone, quinone
propionaldehyde, and valeraldehyde. Aldehyde emissions from this plant are most likely
a function of fuel consumption and any volatile fraction of the asphalt cement. The
emission factors generated for aldehydes follow the same assumptions applied to the
PAH emission factors.
2.5.3 Emissions
Table 2-14 presents the aldehyde emissions results for the three test runs. Also
shown for each run are the date, metered volume (in dscm), O2 concentration, and flow
rate. Flue gas concentrations are given in terms of g/dscm, and g/dscm corrected to
7 percent O2. Oxygen concentrations were collected from CEM data.
During the emission tests, acetone had the highest average mass rate with
1090 g/hr, followed by formaldehyde with 185 g/hr. After blank correction,
acetophenone/o-tolualdehyde, 2,5-dimethylbenzaldehyde, isophorone, isovaleraldehyde,
MIBK/p-tolualdehyde, and m-tolualdehyde were not collected in detectable amounts for
any of the runs during these emission tests. Aldehyde values ranged from 1090 g/hr of
acetone in Run 1, to 1,80 g/hr of quinone in Run 2.
The aldehyde values for the emission tests did not change significantly from Runs
1 to 3, except for acetone and quinone. Acetone fluctuated from 1090 g/hr in Run 1,
303 g/hr in Run 2, and not detected in Run 3. It should be noted that acetone is a
compound that contaminates easily. This should be taken into consideration when
accounting for it. Quinone varied from 3.13 g/hr in Run 1, 1.80 g/hr in Run 2, and
68.6 g/hr in Run 3. At this time, there are not enough data points on this compound to
suggest a reason for the variation.
2.5.4 Flue Gas Aldehydes bv Sample and Sample Parameters
Table 2-15 presents the aldehyde amounts in the flue gas sample for the emission
tests in total /jg for each run. Laboratory analytical results for each sample are
presented in detail in Appendix E.3.
Sampling and flue gas parameters for the aldehyde runs are shown in Table 2-16.
Total sampling times, sample volume and isokinetic results for each sampling run are
2-27
JBS336 z *•'
-------
Table 2-14
ALDEHYDES CONCENTRATION AND EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 6 (l»l)
(ug/dsenj@7%O2)
(ug/dscra)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
Aceialdehyde
Acetone
Benzaldehyde
BulyTaldehyde/boburyraldebyde (ug/dseoi)
(ug/dscm @ 1% O2)
CroionaJdchyde
Formaldehyde
Hexanal
Methyl Elhyl Kelone
Fropiocjldebyde
Quinone
VaJeraldehyde
(ug/dscm)
(ug/dscm @ 7% O2)
(g**)
(ug/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
(6/bf)
(ug/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/d»ra @ 7% O2)
9J4
1610
52.7
19400
33500
1090
226
390
118
53.4
n.2
3.01
422
7Z8
2.M
3340
5770
m
46.3
79.9
ND
ND
ND
ND
tfD
ND
515
-------
TABLE 2-15
ALDEHYDES AMOUNTS IN FLUE SAMPLES - BLANK CORRECTED
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Acetaldehyde
Acetone
Acetophenone/o-Tolualdehyde
Acrolein
Benzaldehyde
Butyraldehyde/Isobutyr aide hyde
Crotonaldehyde
2,5-DimethyIbenzaldehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehyde
MIBK/p-ToLualdehyde
Methyl Ethyl Ketone
Propionaldehyde
Quinone
m-Tolualdehyde
Vaieraldehyde
822
17060
ND
ND
199
47.0
37.1
ND
2940
40.7
ND
ND
ND
ND
ND
48.8
ND
ND
1040
4560
ND
ND
198
ND
29.5
ND
4460
62,5
ND
ND
ND
ND
ND
27.0
ND
ND
1170
ND
ND
26.7
211
75.4
65.0
ND
2760
20.0
ND
ND
ND
93.5
94.6
1040
ND
56.9
ND
6640
ND
ND
ND
ND
ND
ND
10.7
ND
ND
ND
ND
ND
ND
ND
ND
ND
NOTE; Concentrations given have been blank corrected.
f
2-29
-------
Table 2-16
ALDEHYDES EMISSIONS
MATHY CONSTRUCTION
SAMPLING AND FLUE GAS PARAMETERS
COMPANY PLANT 6 (1991)
Total Sampling Time (min)
Average Sampling Rate (dscfm)
Metered Volume (dscf)
Metered Volume (dscm)
Average Stack Temperature (F)
O2 Concentration (%V)
CO2 Concentration (%V)
Stack Gas Moisture (%V)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
62.5
0.500
31.1
0,880
240
12.9
6.2
28.7
33200
940
105
62.5
0.480
29.8
0.843
238
12.4
6.6
29.6
33000
934
101
62.5
0.470
29.5
0.836
234
13.4
5.6
27.1
32500
920
102
NA
0.483
30.1
0.853
237
12.9
6.1
28.5
32900
931
NA
NA « Not Applicable
2-30
-------
presented. Appendix A.3 contains a complete listing of these parameters and additional
sampling and flue gas parameters for each test run along with the field data sheets.
2.6 CONTINUOUS EMISSIONS MONITORING RESULTS
2.6.1 Overview
Continuous emissions monitoring was conducted at the outlet to the air pollution
control device (APCD) during the two days of testing. Concentrations of O2, CO2, CO,
NOX, and SO2 were determined on a dry basis by extracting the gas from the flue,
transferring it to the CEM trailer through heated Teflon tubing (heat trace), passing it
through gas conditioners to remove moisture and directing it to each respective analyzer.
A full description of Radian's CEM system and methods is given in Section 5.
Concentrations of THC were also monitored, with gas concentrations determined on a
wet basis, by allowing a slipstream from the heated sample line to bypass the sample
conditioners so that the wet flue gas was directed to the analyzer as it exited in the flue.
All CEM data were recorded as 30-second averages from
multiple-readings-per-second input by Radian's CEM data acquisition system (DAS).
The resulting CEM data files were averaged over the duration of each test run. The
averages are presented in Section 2.7.2. The 30-second data are included in Appendix D
along with the following additional CEM information:
LOCATION CEM DATA TYPE
• Appendix D.I CEM Tables
• Appendix D.2 Calibration Drifts
• Appendix D.3 Calibration and QC Gas Responses
• Appendix D.4 Response Time, NOX Converter Tests
Linearity Calculation
2.6,2 CEM Results
The CEM averages are presented in Table 2-17. The average O2 runs varied
from 12.4 to 14.2 percent by volume. Carbon dioxide values were approximately 5 to 6
percent by volume. Nitrogen oxides concentrations were approximately 30 to 50 ppmv,
dry at the stack. There were no SO2 emissions. Concentrations of THC were also
monitored, with the resulting concentrations consistently 50 to 70 ppmv/wet. The
averages were taken over the time period that the CEM was on-line.
JBS336 2-31
-------
Table 2-17
CONTINUOUS EMISSIONS MONITORING DAI]^ TEST AVERAGES FOR ACTUAL CONCENTRATIONS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
«^x lOOQppmv)
b = CO monitor sel to 25% of instrument range
-------
2.6.3 Nonmethane Hydrocarbon Emission Test Results
EPA Method 18 analysis of the flue gas was performed using gas chromatography
(GC) to separate the hydrocarbon species (C^-Cg) present in the flue gas stream. Several
samples were injected into the GC during each test day. Methane, benzene, toluene,
ethylbenzene, and xylene were determined by this method. Total hydrocarbon emissions
as methane were determined by EPA Method 25A.
Table 2-18 presents the hydrocarbon concentrations and emission rates in ppmv
and Ib/ton of asphalt produced. The nonmethane hydrocarbon emissions as methane
were calculated by subtracting the methane concentration measured by the GC from the
total hydrocarbons as methane measured by the total hydrocarbon analyzer (CEM) at
the time of sample injection into the GC. The average nonmethane hydrocarbon
emissions were 0.0103 to 0.0143 Ib/ton for the two test days. The average emission
factors of benzene, toluene, ethylbenzene, and xylene for the first test day were 0.00013,
0.00019, 0.000011, and 0.00017 Ib/ton, respectively. The average emission factors for the
second test day were 0.00023, 0.00019, 0.000011, and 0.00017 Ib/ton, respectively. The
data variability is believed to have resulted from process variability.
JBS336 2-33
-------
Table 2-18. Hydrocarbon Emission Rates and Concentrations
;••' ;- :*>: wV'X'i'j1'""*' •'-•'• '•'''•'••'-';•-'•
vT%-^^>Av:xv:v,"vA-X',"-i:-t',-v:
:-> ::::>::::::>;:;:: v;::::-;::-;:;-;::-:">; -r^Ji
:>^x";y::>>::>:'':>"'~«V'':''V"''*"V'
..;.;•;.>•-;-• -:;-"-;•:-:•;••-«-"--••- .v.v.-, -.--•
:-:o:v;-;-:;v:'>".vv.-f-Kv-v;-.-:-i-K.
-:-:;:>::v<:>;;:::::;:::K:::::Xv:vX;:::;.;:
:fev;:;::"::::-ir:::x-'-:h.-:::::-::x!:o>:
|||l;Dale:|||i
09/19/91
iiiiiisiii
':;:|x|:::|5|:|:|:|:i:|r|:::|:|:-:|x;:^:;.
^mrnm^^
"v;vX;X;y.X;l;Xy;;:vH;ii;:;:;
;;;:::;:i-:::::-5:"-:-:-;:'"?;:;:;-;:;-i-;:;:.':;
ISSfiiiwiii
0836
1059
1341
1425
1505
1536
i|^^f^wiS[!3ColS^^
tssfca*®;^
f STANDARD DEVlATlONi;
09/20/91
0801
1025
105J
1151
1246
14S1
1520
i;il:|SS?AVTEi(AOT||lili:
|[CTAlTO^^^l|wi«mpN|
llptisajf
ilii'io»Ji
ilRiiell
ltdsafmjl
jM-Xagte-S
ii'fplfl
33472
33187
31982
31982
31982
31982
l-3243ll|
>"''-;''';~i':'i-;';<;'f"x'?>:-:'f'"'
32988
31086
31086
31086
32656
32105
32475
HswiSli
S|8ifi||ssf|:
fjf?A^iMit|f|
|product(o||
fllfj&ielfll
§i(ten^rJll
245
224
244
244
244
244
284
222
222
222
213
215
194
]y?:!&&: 23S S:;':::::": VS
Ilillllil
IMetiiiincl
|||^;OCl|
ll(w!?yill
239
ND
ND
62-25
39.86
ND
IBS!!!
13.68
5.77
ND
7.47
1.25
6,32
ND
ii:4'S3il?
It HyOTSafrJonsx?
lil^OTGiiS:
•;••-:-;'•-:-;•:-:-• v - •-. --.•----.-- •--•-- .-:•,--•--,-.".
rnm:($pmv)mm:
::>::^::::.>::-7™TV: -•-:-: -•./.•:;:•>:•:•:-:•'.-.•
51.9
a
54
71,9
71.7
64.9
iiili^S&SiS
^:sS5s:jS2,4-^s:jS5
o.-.oyox'i'.-iiVji ,-«J.:'V:;L:'-V:'.:::::'"
55J
54,6
62.3
52-3
41,4
54.8
0
lllllliiHilll
IllllKlllll
?I$I S isten metjuwie Stiii'
;?V;: P>ip
4(RHD»)|
ai.oo
NA
5-1,00
9,65
3184
64.9
Miiiwll
ii^ill
41.82
4)(fi3
62,3
4-1 S3
40.20
4JJJO
ft.OO
lliiSali
llmo'll
934E-03
NA
1.76E-02
3.15&03
1.04R02
2.12E-02
llbl&iwf
1.21E-02
1.70E-02
2.17E-4H
1JAB412
134E-02
L81Bfl2
0,0
•litJtHWBM
':-:<-:':->;-:<-T-x-:-:-;-:-:-;-:';-f:-:i-:-:-:-r':-:'r':':-':°:":-;i:'::;':-;:r--
;>: «: V^VK;'.; :-.,> :•,*,*' •,-,•;• ;:::;:':'.::; ;•;•: :sx-"-.'''''--— -;-;"•-
•,<*\;:>!':;:;X;:;:':-:'M]:>X":"I*^
s'ill!tenzenelit::il
gill&ilfiliiiii
0.338
ND
ND
0117
ND
0.027
lojiaioll
•:•:';':*:';' j»*'I"l' :*,";'!*:';'.
:Si:i¥0.1-;iH:5i'.
0,305
0.167
0.022
0.332
ND
ND
0.156
?!0:l4b;:Ji:
lill
ilBitli
5.61E-04
0.0
0.0
1.S6E-O4
0.00
4.30E-05
Il32i-Mll
:|lllllil:l
4.31B-04
2.B4&04
3.74E-05
5.65&04
0,0
0,0
3.17E-04
JS2J3B-04SS
S::S::S::^S^:fe:J
|i|P|||^UJ««^||||||||
IXPfw>||
5.401
ND
ND
7350
ND
ND
IPtall;
POSlt
0.001
0.009
0.579
0.073
0.003
ND
ND
IS!!
illlll
|'(y^Sn)|
1-06E-02
0.0
0.0
l.ME-02
0,0
0.0
;:II;66Epl
'••':-r-:-:':-:x-: >!':•>!':•>: :-:":'
1.66E-06
1.81E415
1,16&«3
1.47E-04
6J9E-06
0.0
0.0
|it91Ept
slilllS
Ili-slEthylbCTzeiic'!- ;•;«
liXp^nw)*'
0.267
ND
ND
1370
17.470
14530
lljWp
;Ii7.4'p:|
0.001
0.008
ND
0.001
0.019
0.003
ND
P0.005S1
lli>ii
%(ibsAon):;:
&£•••••:••'.!•':. - '*.;.
:8:>H ;'7r:._';Hs;;
6.O4E4M
0
0
3.40E-03
3.79&02
3.15E-02
l:i;22E;02l:
'.->::• '":"'••'. :'•-:•.- o.":';v!': .•'
1.92BO6
1A5E-05
0
232B4J6
4.82E-05
7.41E-06
0
i;-i;i2E-05p;
-;• '' '.'.'.-'.•- •;•:•••;<•-',• i-^'-."
•:*•;":*•*,-.*•';•:* ,* '•••••
•>x>.^ ;-;:',•.,-* ',;,-'". •; •: -
•:l::';'- -^"IXylcne ;-•-', .
iiPPW):
'>lMf:f$s!? ?.
0.027
ND
0.037
0,495
38 .51
1.98
mtMm
|lp;2:|||
0596
0.003
0.026
ND
ND
ND
0,003
iPJwow
^(Ibs/ion)
6.10E-05
0
8.02E-05
1.07B-03
8,35 B-02
4.29E-03
€ft«E-o2-;i
:pf|.v .:
1.15E4)3
6.95Er06
6.Q2B-05
0
0
0
8J1E-06
*L74&fl4*V
m'^v^
alnslrument off-line
ND = Not Delected
NA = Not Applicable
JBS349
-------
3. FACILITY DESCRIPTION
This section provides a description of the Mathy Construction Company's Facility
No. 6 asphaltic concrete plant located in LaCrosse, Wisconsin. The process equipment
and production materials used and the process parameters recorded during the emissions
test are discussed.
3.1 PROCESS DESCRIPTION
The Mathy Construction Facility No. 6 is a typical batch asphaltic concrete plant
with a rated production capacity of 300 tons/hour. The plant consists of the following
components:
• Aggregate storage piles;
• Cold aggregate storage bins;
• A rotary kiln for aggregate drying;
• Hot screens and storage bins for dried aggregate, classified by aggregate
size;
• A heated asphalt storage tank; and
• A pug mill for mixing hot aggregate and asphalt.
The aggregate must be dried to product specifications in the natural gas-fired rotary kiln
before it is separated and classified by size by the hot screens and before it is mixed with
asphalt in the pug mill. The asphalt is an amorphous solid that must be heated to a
liquid state for injection into the pug mill where it is mixed with the dried aggregate.
The final product leaving the pug mill may be loaded onto trucks or transferred to a hot
mix storage bin.
Aggregate fines become entrained in the combustion exhaust leaving the rotary
kiln and are transported to a cyclone, which returns heavier particles to the kiln. The
exhaust gas then enters a fabric filter where smaller fines are collected. Process fugitive
PM and VOCs from the hot screens, hot bins, and pug mill are also routed to the
cyclone inlet. Emissions of VOCs from fuel combustion and asphalt mixing are not
JBS336
-------
controlled by the cyclone or fabric filter, nor are any VOC emission control devices used.
The exhaust flow is an induced draft; that is, a clean-air-side fan is used.
The data collected only reflect emissions from vented process equipment as
described above and do not include emissions from process and area fugitive sources
such as:
• Aggregate storage piles and cold aggregate transport;
• Cold asphalt and hot mix storage tanks; or
• Plant vehicular traffic.
Point source PM, PM10, and metal emissions are attributable primarily to
aggregate-drying and hot transport mechanisms. Condensible PM, PAH, and aldehyde
emissions are generally associated with fuel combustion products and the volatile fraction
of the liquid asphalt, although relative contributions are not found in the literature. The
aggregate/asphalt throughputs are functions of the desired product specifications,
whereas fuel consumption is determined by the drying requirements, aggregate moisture,
and throughput of the aggregate. For the emission factors developed, the final product
composition is 5.8 percent asphalt cement by weight, and the kiln fuel is natural gas.
The emission factors developed in this study reflect these constraints, and the effects of
changes in these parameters on emission factors have not been evaluated.
3.2 PROCESS CONDITIONS DURING TESTING
Production monitoring data for all tests are presented in Tables 3-1 and 3-2.
3.2.1 Process Conditions DiirinE Metals/PAH Testing
Table 3-3 summarizes the production and operating conditions associated with the
metals and PAH test data. Production rates for 3 runs varied from 222 tons/hour to
245 tons/hour (74 to 82 percent of capacity), while natural gas consumption ranged from
5170 ft3/hr to 5250 ft3/hr. Sampling runs for these trains experienced no interruptions of
process upset conditions.
3.2.2 Process Conditions JDuring^Aldehydejresting
Table 3-4 summarizes the production and operating data associated with aldehyde
test data. Production rates varied from 194 tons/hr to 284 tons/hr (65 to 95 percent of
capacity), while natural gas usage ranged from 5000 ft3/hr to 6950 ft3/hr. Sampling
JBS336
3-2
-------
Table 3-1
SUMMARY OF PROCESS OPERATING DATA COLLECTED DURING EMISSION TESTING - SEPTEMBER 19,1991
M ATI IV CONSTRUCTION COMPANY PLANT 6 (199H
Tim*
(24hr)
6; 29
6:43"
6:55
7;12
7:25
7:48
8:19
8:40
8:56
9:34
9:37
10:27"
11:00
11:20
11:46
12:01
13:24
13:30'"
14:00
14:30
15:00
15:30
15:44
15:46
Actual
FlMtUa*
Natural
Oat
100(cu.fL)
Bumar Setting
Flam*
Maiar
<*)
Flam*
Eyt
(micro-
amps)
Kiln
Eitt
Tamp.
(dagre* F)
Production
Rate
(lorw/hr)
Injection
Rate
(tona/hr)
Mix
Tamp,
(degree F)
Exhtmt
GM
Twnp.
(degrteF)
Baghoua*
Prmaura
Drop
{*.•-)
Inlet
T«np.
(degra* F>
Outlal
Tamp.
-------
Table 3-2
SUMMARY OF PROCESS OPERATING DATA COLLECTED DURING EMISSION TESTING - SEPTEMBER 20, 1991
MATIIV CONSTRUCTION COMPANY PLANT 6 (1991)
Time
(24hr»
7:01
7:36'
7:45
7:55
8:00
8:15
8:30
8:47
9:30
9:38
10:00
10:30
11:07
11:36
12:05
12:39
12:59
13.35
14;12'"
14:30
15:00
15:27
15:30
Actual
Fuel Use
Natural
Ga*
100(cu.fL)
Burner Setting
Flame
Meter
<%)
START OF WARM-UP
4
93
Flame
Eye
(mlcro-
•«JEfl
Kiln
ExN
Temp.
(degree F
Production
Rate
(tonB/hr)
Asphalt
Injection
Rate
(tons/hr)
Mix
Temp,
(degree F
Exhauet
Gas
Temp.
(degree F
Baghouae
Presure
Drop
(«.g.)
Inlet
Temp.
(degree F
Outlet
Temp.
(degree F
1.9
358
0
—
310
0.9
250
155
Amplent
Temp.
(degree F
36.0
36.0
Relative
Humidity
(*)
Exhaust
Damper
Portion
(*)
82
Not Taken
42.0
START OF ALDEHYDES
16
6
17
21
9
83
83
83
82
1.9
1,9
1.9
1.9
SHUTDOWN
339
358
351
350
0
360
240
300
141
20.9
13.9
17.4
8-2
300
325
—
—
318
325
320
1.0
1.1
1.7
1-7
262
269
274
272
229
242
249
249
36.8
37,2
37,8
41.6
Not Taken
Not Taken
Noi Taken
80
42,0
42.0
410
42.0
RESTART PLANT
8
22
27
31
25
26
30
87
83
83
79
82
78
78
1.9
1.8
1,8
1.9
1.9
1.9
1,9
338
348
349
350
348
348
352
STOP
13
4
6
16
24
100
79
71
78
1.9
1.8
1.8
1.8
314
347
350
348
113
286
220
219
228
228
212
195
17
77
283
140
6-5
16.6
12.8
12.7
13.2
13.2
12.3
11.3
1.0
4.5
16.4
8.1
—
—
—
—
—
302
—
320
325
315
315
320
315
315
1.7
1,9
2.2
2.0
2.4
3.0
2.9
260
269
269
265
270
269
269
221
249
249
249
250
250
252
45.2
51.2
52.8
55.4
51.4
79
Noi Taken
Noi Taken
Noi Taken
Noi Taken
61
Noi Taken
40.0
40.0
40.0
42.0
43.0
44,0
42.0
...
...
...
300
305
305
310
310
2.8
2.3
2.9
2.2
260
254
252
252
220
224
230
235
56,0
58.0
59.0
Noi Taken
46
Not Taken
40,0
40.0
41
41
END OF PM TEST
28
75
1.9
350
250
|_ 14.5
...
310
1.8
258
244
61.0 | Not Taken) 41
Siui Production
R«lan
-------
Table 3-3
SUMMARY OF METALS/PM AND PAH EMISSION FACTORS AND PROCESS OPERATING CONDITIONS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Date
Production Rate (tons/hr)
Virgin Asphali Rate (lons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cemeni Rate (tons/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Fuel Flow (cubic foor/hr)
Heat Imput Rate ( 1000 cubic foot/hr)
Burner Setting - Flame Meier (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exit Temperature (degree F)
Stack Flow Rate (dscfm)
Stack Flow Rate (dscf/ton of product)
Slack Temperatrue (degree F)
Stack Moisture (% volume)
Stack CO2 (volume % dry)
Slack O2 (volume % dry)
Stack CO (PpmV)
Control Device
:8p;S]fe8SSsgpjg:
:fifeli:S:S-m%lsf..^
6.23
245
230.8
0
14.2
82
4.3
5250
5.25
78
43
85
339
34280
8390
240
27.5
5-7
14.1
> 1000
Baghousc
P§IP:$:||I^£|$I
ND
244
229.8
0
14.2
81
4.3
5280
5.28
80
51
54
341
32660
8030
236
28.4
5.8
12.5
> 1000
Baghousc
5.92
222
209.1
0
12.9
73
4.4
5190
5.19
81
53
70
349
31570
8530
244
28.1
5.2
14.2
1362
Baghouse
237
223.2
0
13.8
79
4.3
5240
5.24
80
49
70
343
32840
8320
240
28.0
5.6
13.6
1362
NOTE = Run averages were calculated from readings taken periodically throughout I he duration of the emission lesl run.
See Table 3-1 and 3-2 for the individual readings
3-5
-------
Table 3-4
SUMMARY OF ALDEHYDE EMISSION FACTORS AND PROCESS OPERATING CONDITIONS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Date
Production Rate (ton/hr)
Virgin Asphalt Rate (too/hi)
Recycled Asphalt Rate (ton/hr)
Asphalt Cement Rate (ton/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Fuel Flow (cubic foot/hr)
Heat Irnput Rate (1000 cubic foot/hr)
Burner Setting - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exit Temperature (degree F)
Stack Flow Rate (dscfm)
Stack Flow Rate (dscf/ton of product)
Stack Temperature (degree F)
Stack Moisture (% volume)
Stack CO2 (volume % dry)
Stack O2 (volume % dry)
Sfarlr m /"rtnrnV*
__ _ ^ ^Pj,— _ . f
Control Device
&kv&:::;j:;::&>:-3
X'l-xvKvM-loai'X-K'f :•>?:•§
SS^SS^ft-ttvftv:?!-;
09/19/91
229
215.7
0
13.3
76
4.3
5393
5.39
70
49
58
341
33187
8695
240
28.7
6.3
13.5
> 1000
Baghouse
09/20/91
284
267.5
0
16.5
95
4.7
6947
6.95
84
40
80
347
32988
6969
238
29.5
6.6
12.4
> 1000
Baghouse
*&£••$>%>$$*$?%?$?•
09/20/91
194
182.7
0
11.3
65
4,7
5000
5.00
75
58
46
J^*\3
32475
10044
234
27.1
5.6
13.6
1567
Baghouse
212
199.2
0
12.3
71
4,5
5197
5.20
73
54
52
345
32831
9370
237
27.9
6.0
13.6
1567
NOTE ; Run averages were calculated from readings taken periodically throughout ihe duration of the emission lesi run.
See Table 3-1 and 3-2 for the individual readings.
Run 2 was not calculated in the average. Runs 1 & 3 were at a minimum production load, whereas Run 2 was at a maximum production load.
Ail three tests were interrupted by plant shutdown. Trains were removed from stack and were not operated during down times.
3-6
-------
Run 1 was temporarily interrupted while aggregate moisture was measured, and sampling
did not proceed during this stoppage. Sampling Run 2 was interrupted by a full plant
shutdown. Sampling Run 3 was also interrupted by a full plant shutdown. In all cases,
sampling was suspended and sampling equipment was removed from the stack and
capped to prevent contamination during plant shutdowns.
3-2-3 Process Conditions During PM10/CPM Testing
Table 3-5 summarizes the production and operating data that correspond to the
PM10/CPM test results. For three sampling runs, total asphaltic concrete production
varied between 213 tons/hr and 224 tons/hr (71 to 75 percent of capacity), while natural
gas consumption ranged from 5000 ft3/hr to 5230 ft3/hr. No PM10/CPM sampling runs
were interrupted by process upsets.
JBS336
-------
Table 3-5
SUMMARY OF PM10/CPM EMISSION FACTORS AND PROCESS OPERATING CONDITIONS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
^<*cr::::i*::S^^:£^*;::<::rtv'::'::W:;&.*^^
ilflj^iBlw8B^^^^s^^w?w.slli^^^^^^^^^^^^^^^
Date
Production Rate (lons/hr)
Virgin Asphalt Raie (tons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cement Rate (tons/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Fuel Flow (cubic fooi/hr)
Heat Imput Rate ( 1000 cubic foot/hr)
Burner Setting - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exit Temperature (degree F)
Stack Flow Rate (dscfm)
Slack Flow Rate (dscf/ton of product)
Stack Temperairue (degree F)
Stack Moisture (% volume)
Stack CO2 (volume % dry)
Stack O2 (volume % dry)
Stack CO (ppmV)
Conirol Device
09/19/91
224
211
0
13
75
4,3
5180
5,18
74
51
57
340
33530
8981
241
28.5
5.1
'14.1
> 1000
Baghouse
09/20/91
213
200.6
0
12.4
71
4.4
4990
4.99
79
53
61
350
32660
9200
255
28.5
5.4
14
1496
Baghouse
09/20/91
215
202.5
0
12.5
72
4.7
5230
5.23
76
58
46
348
32100
8960
242
27.6
5.6
13.6
1567
Baghouse
217
204.7
0
12.6
73
4.5
5130
5.13
76
54
55
346
32840
8320
246
28.2
5.4
13.V
1532
NOTE = Run avenges were calculated
See Table 3-1 and 3-2 for the
from readings taken periodically throughout (he duration of the emission lesi run.
individual readings.
3-8
-------
4. SAMPLING LOCATIONS
This section describes the locations where samples were taken during the emission
testing program at Mathy Construction Company Facility No. 6. All samples collected by
manual methods including PMi0 samples were collected from six sampling ports at equal
heights in the exhaust stack. Samples for the CEMS were collected from a single point
near the manual sampling ports. The sampling location arrangement is shown in
Figure 4-1.
The test ports were located according to EPA Method 1. The nearest upstream
disturbance was 3.3 equivalent diameters away and the nearest downstream disturbance
was 1.2 equivalent diameters away from the test ports.
The minimum number of traverse points required for manual sampling was 24.
Five points at each of the six ports were used as shown in Figure 4-2.
JBS336
-------
n n n n n n
Top
View
42"
Tl
4%"
48"
TTO U U U U
Li
4
Mathy Plant #6
T
55"
i
149"
6 x 4" ID Ports
evenly spaced
CEMPort
Baghouse
Blower
(ID Fan)
Damper
Figure 4-1. Sampling Location Arrangement.
4-2
-------
42"
'
47.3
1
75"
37
L
^
.75"
28;
I
75" T
18.75" ±
* ,
i 1 1 i9'375"
1
• • ' ••
• jfc A dk
• .A A A
&
A
WWW
• * • •
V
w
™
j
4
r
3"
l^ ^_
41/."
i
Point Probe Mark f
1 9.375
2 18.75
3 28.75
4 37.75
II
II
II
II
5 47.375"
Figure 4-2. Traverse Point Layout at Stack.
4-3
-------
5. SAMPLING AND ANALYTICAL PROCEDURES
The sampling and analytical procedures used for the asphalt plant test program
were the most recent revisions of the published EPA methods or proposed EPA
methods. In either case, state-of-the-art sampling and analytical methods were used.
This section describes the sampling and analytical method used for each compound
analyzed.
5,1 PARTICULATE MATTER AND METALS EMISSIONS TESTING
METHOD
Sampling for paniculate matter (PM) and metals was performed according to an
EPA EMB draft protocol entitled "Methodology for the Determination of Metals
Emissions in Exhaust Gases from Incineration Processes." The protocol is presented in
Appendix J.I. This method is applicable for the determination of PM emissions and Pb,
Ni, Zn, P, Cr, Cu, Mn, Se, Be, Tl, Ag, Sb, Ba, Cd, As, and Hg emissions from various
types of processes. The test samples were not analyzed for Hg because Hg was not
expected in the process stream. Paniculate emissions were based on the weight gain of
the filter and the front half acetone rinses of the probe, nozzle, and filter holder. After
the gravimetric analyses were completed, the sample fractions were analyzed for the
target metals as discussed in Section 5.2.5.
5.1.1 Sampling Equipment for Particulate Matter and Metals
This methodology used the sampling train shown in Figure 5-1. The sampling
train consisted of a quartz nozzle/probe liner followed by a heated filter assembly with a
Teflon® filter support, a series of five impingers, and the standard EPA Method 5
meterbox and vacuum pump. The sample was not exposed to any metal surfaces in this
train. Two of the sequential impingers contained a 5 percent nitric acid
(HNO3)/10 percent hydrogen peroxide (H2O2) solution and one contained silica gel.
The first and fourth impingers were empty knockout impingers not required by the
method, but added because of the high moisture content of the flue gas. The second
impinger containing HNO3/HZO2 was of the Greenburg-Smith design; the other
impingers had straight tubes. The impingers were connected together with clean glass
JBS336
-------
i Thermometer
Temperature /
Sensor y
Gooseneck / /
Nozzle / A
Thermometer
S-Type Pilot Tube
Is)
Implngere with Absorbing Solution
Stack
Wall Heat Traced
S.S. Probe
Glass Filter Holder
Empty Knockout
Silica Gel
Empty Knockout
Temperature
Sensorti
5% HNQ,/10% H2O2
vacuum
Gauge
Dry Gait
Meter
Vacuum
Une
Figure 5-1. Schematic of Multiple Metals Sampling Train
-------
U-tube connectors and were arranged in an impinger bucket. Sampling train
components were recovered and analyzed in separate front and back half fractions
according to the described method.
5.1.2 Equipment Preparation for Particulate Matter and Metals Sampling
5,1.2.1 Glassware Preparation. Glassware was washed in hot, soapy water, rinsed
three times with tap water and then rinsed three times with deionized distilled water.
The glassware was then subjected to the following series of soaks and rinses:
• Soaked in a 10 percent HNO3 solution for a minimum of 4 hours;
• Rinsed three times with deionized distilled water rinse; and
• Rinsed with acetone rinse.
The cleaned glassware was allowed to air dry in a contamination-free
environment. The ends were then covered with parafilm. All glass components of the
sampling train plus any other sample bottles, pipes, Erlenmeyer flasks, petri dishes,
graduated cylinders, and other laboratory glassware used during sample preparation,
recovery, and analysis were cleaned according to this procedure.
5,1.2.2 Reagent Preparation. The sample train filters were Pallflex
Tissuequartz 2500QAS filters. The acids and H2O2 were Baker "Instra-analyzed" grade
or equivalent. The H2O2 was purchased specifically for this test site.
The reagent water was Baker "Analyzed HPLC" grade or equivalent. The lot
number, manufacturer, and grade of each reagent that was used were recorded in the
laboratory notebook.
The HNO3/H2O2 absorbing solution was prepared fresh daily according to
Section 4.2.1 of the reference method. The analyst wore both safety glasses and
protective gloves when the reagents were mixed and handled. Each reagent had its own
designated transfer and dilution glassware. To avoid contamination, this glassware was
marked for identification with a felt tip glass-marking pen and used only for the reagent
for which it was designated.
5.1.2.3 Equipment Preparation. The remaining preparation included calibration and
leak checking of all the train equipment, which included meterboxes, thermocouples,
nozzles, pitot tubes, and umbilicals. Referenced calibration procedures were followed
JBS336 ^".3
-------
when available, and the results were properly documented and retained. A discussion of
the techniques used to calibrate this equipment is presented below.
Type-S Pilot Tube Calibration. The EPA has specified guidelines concerning the
construction and geometry of an acceptable Type-S pilot tube. A pitot tube coefficient
of 0.84 is used if the specified design and construction guidelines are met. Information
pertaining to the design and construction of the Type-S pitot tube is presented in detail
in Section 3.1.1 of EPA Document 600/4-77-027b. Only Type-S pitot tubes meeting the
required EPA specifications were used. Pitot tubes were inspected and documented as
meeting EPA specifications prior to field sampling.
Sampling Nozzle Calibration. Glass nozzles were used for isokinetic sampling.
Calculation of the isokinetic sampling rate required that the cross sectional area of the
sampling nozzle be accurately and precisely known. All nozzles were thoroughly
cleaned, visually inspected, and calibrated according to the procedure outlined in Section
3.4.2 of EPA Document 600/4-77-027b.
Temperature Measuring Device Calibration. Accurate temperature measurements
were required during source sampling. Thermocouple temperature sensors were
calibrated using the procedure described in Section 3.4.2 of EPA document
600/4-77-027b. Each temperature sensor was calibrated at a minimum of two points
over the anticipated range of use against an NBS-traceable mercury-in-glass
thermometer. All sensors were calibrated prior to field sampling,
Dry Gas Meter Calibration. Dry gas meters (DGMs) were used in the sample
trains to monitor the sampling rate and to measure the sample volume. All DGMs were
calibrated to document the volume correction factor just before the equipment was
shipped to the field. Post-test calibration checks were performed as soon as possible
after the equipment has been returned to Research Triangle Park, North Carolina
(RTF). Pre- and post-test calibrations agreed to within 5 percent. Prior to calibration, a
positive pressure leak check of the system was performed using the procedure outlined in
Section 3.3.2 of EPA document 600/4-77-237b. The system was placed under
approximately 10 inches of water pressure and a gauge oil manometer was used to
JBS336
5-4
-------
determine if a pressure decrease was detected over a 1-minute period. If leaks were
detected, they were eliminated before actual calibrations were performed.
After the sampling console was assembled and leak checked, the pump was
allowed to ran for 15 minutes. This allowed the pump and DGM to warm up. The
valve was then adjusted to obtain the desired flow rate. For the pretest calibrations,
data were collected at orifice manometer settings (AH) of 0.5, 1.0, 1.5, 2.0, 3.0 and 4.0
inches of H2O. Gas volumes of 5 ft3 were used for the two lower orifice settings, and
volumes of 10 ft3 were used for the higher settings. The individual gas meter correction
factors were calculated for each orifice setting and averaged. The method required that
each of the individual correction factors fall within ±2 percent of the average correction
factor or the meter was cleaned, adjusted, and recalibrated. In addition, Radian
required that the average correction factor be within 1.00 ± 1 percent. For the post-test
calibration, the meter was calibrated three times at the average orifice setting and
vacuum used during the actual test.
Rockwell Model 175 DGMs in Research Appliance Company (RAC) enclosures
were used for measuring gas sampling rates. The DGM calibrations were performed at
Radian's RTF laboratory using an American wet test meter as an intermediate standard.
The intermediate standard is calibrated every six months against the EPA spirometer at
EPA's Emissions Measurement Laboratory in RTF.
5.1.3 Particulate Matter/Metals Sampling Operations
5,1.3.1 Preliminary Measurements. Before sampling began, preliminary
measurements were required to ensure isokinetic sampling. These included determining
the traverse point locations and performing a preliminary velocity traverse, cyclonic flow
check, and moisture determination. These measurements were used to calculate a
"K factor." The K factor was used to determine an isokinetic sampling rate from stack
gas flow readings taken during sampling.
Measurements made during the pretest site survey were then checked for
accuracy. Measurements were made of the duct inside diameter, port nozzle length, and
the distances to the nearest upstream and downstream flow disturbances. These
measurements were used to verify sampling point locations by following EPA Reference
JBS336 -*~^
-------
Method 1 guidelines. The distances were then marked on the sampling probe using an
indelible marker.
5.1.3.2 Assembling the Train. Assembling the PM/metals sampling train
components was initiated in the recovery trailer and final train assembly was completed
at the stack location. First, the empty, clean impingers were assembled and laid out in
the proper order in the recovery trailer. Each ground-glass joint was carefully inspected
for hairline cracks. The first impinger was a knockout impinger with a short tip. The
purpose of this impinger was to collect condensate. The next two impingers were
modified tip impingers, which each contained 100 ml of 5 percent HNO2 and 10 percent
H2O2. The fourth impinger was empty, and the fifth impinger contained 200 to 300
grams of blue-indicating silica gel. After the impingers were loaded, each impinger was
weighed, and the initial weight and contents of each impinger were recorded on a
recovery data sheet. The impingers were connected together by clean glass U-tube
connectors and arranged in the impinger bucket. The height of all the impingers was
approximately the same to obtain a leak free seal. The open ends of the train were
sealed with parafilm or teflon tape.
The second step was to load the filter into the filter holder in the recovery trailer.
The filter holder was then capped off and placed into the impinger bucket. A supply of
parafilm and socket joints was also placed in the bucket in a clean plastic bag for use by
the samplers. To avoid contamination of the sample, sealing greases were not used.
The train components were transferred to the sampling location and assembled as
previously shown in Figure 5-1.
5.1.3.3 Sampling Procedures. After the train was assembled, the heaters for the
probe liner and heated filter box were turned on. When the system reached the
appropriate temperatures, the sampling train was ready for pretest leak checking. The
filter skin temperature was maintained at 120 ± 14°F (248 ±25°F). The probe
temperature was maintained above 100°C (212°F).
The sampling trains were leak checked at the start and finish of sampling. (EPA
Method 5 protocol required post-test leak checks and recommended pretest leak checks.)
Radian protocol also incorporated leak checks before and after every port change. An
JBS336 5-6
-------
acceptable pretest leak rate was less than 0.02 acfm (ft3/min) at approximately 15 inches
of mercury (in. Hg). If, during testing, a piece of glassware needed to be emptied or
replaced, a leak check was performed before the glassware piece was removed, and after
the train was reassembled,
To leak check the assembled train, the nozzle end was capped off and a vacuum
of 15 in. Hg was pulled in the system. When the system was evacuated, the volume of
gas flowing through the system was timed for 60 seconds. After the leak rate was
determined, the cap was slowly removed from the nozzle end until the vacuum dropped
off, and then the pump was turned off. If the leak rate requirement was not met, the
train was systematically checked by first capping the train at the filter, at the first
impinger, etc., until the leak was located and corrected.
After a successful pretest leak check had been conducted, all train components
were at their specified temperatures, and initial data were recorded (DGM reading), the
test was initiated. Sampling train data were recorded periodically on standard data
forms. A checklist for sampling is included in Table 5-1.
The leak rates and sampling start and stop times were recorded on the sampling
task log. Also, any other events that occurred during sampling were recorded on the
task log such as pilot cleaning, thermocouple malfunctions, heater malfunctions, or any
other unusual occurrences.
At the conclusion of the test run, the sample pump (or flow) was turned off, the
probe was removed from the duct, a final DGM reading was taken, and a post-test leak
check was completed. (The post-test leak check procedure is identical to the pretest
procedure; however, the vacuum should be at least 1 in. Hg higher than the highest
vacuum attained during sampling.) An acceptable leak rate was less than 4 percent of
the average sample rate, or 0.02 acfm (whichever was lower). If a final leak rate did not
meet the acceptable criterion, the test run could still have been accepted upon approval
of the test administrator.
5,1.4 Particulate Matter/Metals Sample Recovery
Recovery procedures began as soon as the probe was removed from the stack and
the post-test leak check was completed.
JBS336 *-/
-------
Table 5-1
Sampling Checklist
Before Test Starts:
1. Check impinger set for correct order and number. Verify probe markings,
and re-mark if necessary.
2. Verify that you have all the correct pieces of glassware.
3. Get data sheets and read barometric pressure.
4. Bag sampling equipment needs to be ready (with bags labeled and ready to
go) if applicable,
5. Examine meter box; level it and confirm that the pump is operational.
6. Assemble train to the filter and leak check at 15 in Hg. Attach probe to
train and do final leak check; record leak rate and pressure on sampling
log.
7. Check out thermocouples; make sure they are reading correctly.
8- Turn on all heaters and check to see that they are increasing.
9. Leak check pilots.
10. Check that cooling water is flowing and on. Add ice to impinger buckets.
11. Check isokinetic K-factor; make sure it is correct. (Refer to previous
results to confirm assumptions), (Two people should calculate this
independently to double check it.)
12. Have a spare probe liner, probe sheath, meter box and filter ready to go at
location.
JDS196
5-8
-------
Table 5-1
Continued
During Test:
1. Notify crew chief of any sampling problems immediately. Note problem on
sampling log.
2. Perform simultaneous/concurrent testing with other locations (if
applicable). Maintain filter temperature between 248°F _+ 25°F. Keep
temperature as steady as possible. Maintain XAD trap and impinger
temperatures below 68°F. Maintain probe temperature above 212°F.
3. Leak check between ports and record on sampling log,
4. Record sampling rate times and location for the fixed gas (CO, CO2, O2)
sample (if applicable).
5, Blow back pilot tubes at inlet location every 15 minutes.
6. Change filter if pressure drop exceeds 15 in. Hg.
7. Check impinger solutions every 1/2 hr; if bubbling into impinger prior to
silica gel, empty out first impinger into pre-weighed bottle and replace.
8. Check impinger silica gel every 1/2 hr; if indicator disappears request a
pre-filled impinger from van lab and replace.
9. Check manometer fluid levels and zero every hour.
After Test Is Completed:
1. Record final meter reading.
2. Check completeness of data jheet,
3. Do final leak check of sampling train at 1 in Hg greater than maximum
vacuum during test.
JB5296
5-9
-------
Table 5-1
Continued
4. Leak check each leg of pilot tubes.
5. Disassemble train. Cap sections. Take sections to recovery trailer,
6, Probe recovery (use 950 ml bottles)
a) Bring probes into recovery trailer (or other enclosed area),
b) For acetone rinses (all trains)
Attach flask to end of probe
Add about 50 mis of acetone
Put in brush down probe, and brush back and forth
Rinse back and forth in probe
Empty out acetone in sample jar
Do this 3 times
c) For MeCl2 rinses
Rinse 3 times with flask attached (no brushing)
7. Reattach nozzle and cap for next day, store in dry safe place.
8. Make sure data sheets are completely filled out and give to Location leader.
JBS296
5-10
-------
To facilitate its transfer from the sampling location to the recovery trailer, the
sampling train was disassembled into three sections: the nozzle/probe liner, filter
holder, and impingers in their bucket. Each of these sections was capped with Teflon®
tape or parafilm before being transported to the recovery trailer.
Once in the trailers, the sampling train was recovered as separate front and back
half fractions. Figure 5-2 is a diagram illustrating front half and back half sample
recovery procedures. No equipment with exposed metal surfaces was used in the sample
recovery procedures. The weight gain in each of the impingers was recorded to
determine the moisture content in the flue gas. Following weighing of the impingers, the
front half of the train was recovered, which included the filter and all sample-exposed
surfaces forward of the filter. The probe liner was rinsed with acetone by tilting and
rotating the probe while squirting acetone into its upper end so that all inside surfaces
were wetted. The acetone was quantitatively collected into the appropriate sample
bottle. This rinse was followed by additional brush/rinse procedures using a nonmetallic
brush; the probe was held in an inclined position and acetone was squirted into the
upper end as the brush was pushed through with a twisting action, All of the acetone
and paniculate was caught in the sample container. This procedure was repeated until
no visible particulate remained and was finished with a final acetone rinse of the probe
and brush. The front half of the filter was also rinsed with acetone until all visible
particulate was removed. After all front half acetone washes were collected, the cap was
tightened, the liquid level marked and the bottle weighed to determine the acetone rinse
volume. The method specifies that a total of 100 ml of acetone must be used for rinsing
these components. However, a thorough rinse usually requires more reagent. For blank
correction purposes, the exact weight or volume of acetone used was measured. An
acetone reagent blank of approximately the same volume as the acetone rinses was
analyzed with the samples.
The nozzle/probe liner, and front half of the filter holder was rinsed three times
with 0.1N HNO3 and the rinse was placed into a separate amber bottle. The container
wascapped tightly, the weight of the combined rinse was recorded, and the liquid level
JBS336
-------
Probe Uner
and Nozzle
Front Half ol
Filar Housing
Filer
Filer Support
and Bach KM
<* Finer
Housing
1st Impinger
(Empty at
beginning
of lest)
2nd,3rd & 4lh
fs
Last Impinger
Rinse with
Acetone fr*o
Tarad Container
Brush Unar
wNhNonmetalftc
Bruah and Rinse
w*h Acetone
at Least
3Tknee
Brush wilh
Nonmelalic
Bf usl) and
Rinse with
Acatooelnto
Tared Container
Caiaiutty
flemcveFllier
trom Supporl wflh
TeflonCaafed
Tweueriand
CheefcUnar
to»Ml
PMIcuWa
Ramowd:!
Stap
ftaMMl
Abow
0,1 N
Nitric Add
into Tared
ConiaJner
Brush Looa*
OMoFBar
I
Measure
bnpmger
Contorts
I
Calculate
Mo&ue
Qaki
I
Empty
Contents
Wo
Tared
Container
SeeJPslii
Obhwtth
TfOonTeiM
Rinse Three
TknaswMh
0.1 N
NblcAckl
I
necowerlnto
Rinse live*
0.1 N
NlricaddMo
TmdConMw
RlmeTtaee
Tbmtwtth
0.1 N
NlricaddMo
Tared Container
J
Weigh lo
CaiouMe
BtrtseVokno
I
APR
Corta^e/3
Weigh lo
Cdoutale
RkieeVokMne
I
PR
Container
Wetgh
lo Calculate
Rtoee Amount
Contahei
I
Weigh to
Cafculale
Unas Amount
Measure
Impinger
Contents
I
Calculate
Moisture
Gain
I
Empty
Contents
Into
Tarad
Container
Rinse Three
TbneswNh
01N
NttricAcU
I
Aacovai Into
Sampto
Container
I
Weigh to
Weigh lor
Motaluie
Calculate
Moisture
Gain
I
Discard
Hlnee Amount
Container I
Container 4
SG
I
l-'tgure 5-2, Metals Sample Recovery Scheme
-------
was marked on the bottle. The filter was placed in a clean, well-marked glass petri dish
and sealed with Teflon® tape.
Prior to recovering the back half impingers, the contents were weighed for
moisture content. Any unusual appearance of the filter or impinger contents was noted
in the logbook.
The contents in the knockout impinger was recovered into a preweighed,
prelabeled bottle with the contents from the HNO3/H2O2 impingers. These impingers
and connecting glassware were rinsed thoroughly with 0.1N HNO3, the rinse was
captured in the impinger contents bottle, and a final weight was taken. Again, the
method specifies a total of 100 ml of 0.1N HNO3 be used to rinse these components.
The weight of reagent used for rinsing was determined by weighing the impinger
contents bottle before and after rinsing the glassware. A nitric acid reagent blank of
approximately the same volume as the rinse volume was analyzed with the samples.
After final weighing, the silica gel from the train was saved for regeneration. The
ground-glass fittings on the silica gel impinger were wiped off after sample recovery to
ensure a leak tight fit for the next test.
A reagent blank was recovered in the field for each of the following reagents:
• Acetone blank-100-ml sample size;
• 0.1N HNO3 blank-1000-ml sample size;
• 5 percent HNO3/10 percent H2O2 blank--200-ml sample size;
• Dilution water--100-ml sample size; and
• Filter blank-one each.
Each reagent blank was from the same lot used during the sampling program. Each lot
number and reagent grade was recorded on the field blank label and in the logbook.
The liquid level of each sample container was marked on the bottle in order to
determine if any sample loss occurred during shipment. If sample loss had occurred, the
JBS336
-------
sample might have been voided or a method could have been used to incorporate a
correction factor to scale the final results depending on the volume of the loss.
Approximate detection limits for the various metals of interest are summarized in
Table 5-2.
5.1.5 Paniculate Analysis
The general gravimetric procedure described in EPA Method 5, Section 4.3, was
followed. Both filters and precleaned beakers were weighed to a constant weight before
use in the field. The same balance used for taring was used for weighing the samples.
The acetone rinses were evaporated under a clean hood at 70°F to dryness in a
tared beaker. The residue was desiccated for 24 hours in a desiccator containing fresh
room temperature silica gel. The filter was also desiccated to a constant weight under
the same conditions. Weight gain was reported to the nearest 0.1 mg. Each replicate
weighing agreed to within 0.5 mg or 1 percent of total weight less tare weight, whichever
was greater, between two consecutive weighings, and was at least 6 hours apart.
5.1.6 Metals Analytical Procedures
A diagram illustrating the sample preparation and analytical procedure for the
target metals is shown in Figure 5-3.
The front half acetone and filter fractions were digested with concentrated HNO,
and hydrofluoric acid (HF) in a microwave pressure vessel. The microwave digestion
took place over a period of approximately 10 to 12 minutes in intervals of 1 to 2 minutes
at 600 watts. The nitric probe rinse was digested by EPA SW 846 Method 3020. The
digested filters and the digested probe rinses were combined to yield the front half
sample fraction. The fraction was diluted to a specific volume with DI water and
analyzed by applicable instrumentation.
The absorbing solutions from the HNO3/H2O2 impingers were combined,
acidified, and reduced to near dryness. The sample was then digested by conventional
digestion, with 5 percent HNO3. After the fraction has cooled, it was filtered and diluted
to a specified volume with DI water.
Each sample fraction was analyzed by inductively coupled argon plasma
spectroscopy (ICAP) using EPA Method 200.7. Interelement corrections were applied to
JBS336 5-14
-------
TABLE 5-2. APPROXIMATE DETECTION LIMITS
Metal
Chromium
Cadmium
Arsenic6
Leacf
Nickel
Barium
Beryllium
Silver
Antimony
Thallium
Zinc
Copper
Manganese
Phosphorus
Selenium
Method'
ICAP
ICAP
GFAAS
GFAAS
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
Analytical
Detection
Limits
(pg/ml)
0.006
0.002
0.004
0.003
0.003
0.001
0.0001
0.006
0.015
0.100
0.015
0.004
0.003
0.300
0.005
Instack Method Detection Limits1*
Front Half
(300 ml sample
size)
0,g/m3)
1.4
0.5
1.0
0.7
0.7
0.2
0.2
- 1.4
3.6
24
3.6
1.0
0.7
72
1.2
Back Half
(150 ml sample
size)
<«?/m3)
0.7
0.2
0.5
0.4
0.4
0.1
0.1
0.7
1.8
12
1.8
0.5
0.4
36
0.6
TCAP = Inductively Coupled Argon Plasma
GFAAS = Graphite Furnace Atomic Absorption Spectroscopy
CVAAS = Cold Vapor Atomic Absorption Spectroscopy
"These detection limits are based on a stack gas sample volume of 1.25 m3. If 5 m3 are
collected, the instack detection method detection limits are 1/4 of the values indicated.
elf Fe and Al are present, samples will be diluted which may raise analytical detection
limits.
JBS336
5-15
-------
Containers
Acfd Probe Rinse
(Labeled APR)
Container 2
Acetone Probe Rinse
(Labeled PR)
Container 1
Filter
(Labeled F)
Reduce to Dryness
in a Tared Beaker
Desiccate to
Constant Weigh!
Determine Residue
Weight In Beaker
Container 4
HNQ /H,O2 Implngers
(labeled HN)
(include condensale
implnger. If used)
I
Aliquot Taken
Taken (or CVAAS
tor Hg Analysis
Fraction 2B
Determine Filler
Paniculate Weight
Solublllze Residue
with Cone. HNO3
Acidify to pH 2
with Cone. HNQ,
Os
Digest with Acid
and permanganate
at9S°Cfor2h
and Analyze
for Hg by CVVAS
Divide Into 0.5 g
Sections and Digest
Each Section with
Cone. HF and HNQ>
Reduce Volume to
Near Oryness and
Digest with
Cone. HNO,
Filter and Dilute
to Known Volume
Fraction 1
Remove SO to 100 ml
Aliquot for Hg
Analysis by CVAAS
Fraction IB
Digest with Acid and
Permanganate at 95°C In
a Water Bath for 2 h
Analyze by (CAP for
Taiget Metals
Fraction 1A
JL
Analyze for
Metals by GFASS
Fraction 1A
Analyze Aliquot tor
Hg Using CVAAS
Figure 5-3. Metals Sample Preparation and Analysis Scheme
-------
the analytes to remove the effects of unwanted emissions. If arsenic or lead levels were
less than 2 ppm, graphite furnace atomic absorption spectroscopy (GFAAS) was used to
analyze for these elements by EPA Methods 7060 and 7421. Matrix modifiers such as
specific buffering agents were added to these aliquots to make the matrix more volatile
and/or stabilize the analyte element. The total volumes of the absorbing solutions and
rinses for the various fractions were measured and recorded in the laboratory notebook.
5.1.7 Quality Control for Metals Analytical Procedures
All quality control (QC) procedures specified in the test method were followed.
All field reagent blanks were processed, digested and analyzed as specified in the test
method. To ensure optimum sensitivity in measurements, the concentrations of target
metals in the solutions were at least 10 times the analytical detection limits.
5.1.7.1 Inductively Coupled Argon Plasma Spectroscopy Standards andj^uality
Control Samples. The QC procedures used for ICAP analysis include running two QC
standards, and a calibration blank after every 10 samples. One interference check
standard was analyzed at the beginning and the end of the analytical run. One duplicate
analysis and one analytical spike were analyzed to check for precision and matrix effects.
Standards less than 1 /*g/ml of a metal were prepared daily; those with
concentrations greater than this were made monthly.
5.1.7.2 Graphite Furnace Standards and Quality Control Samples. Standards
used for GFAAS analysis were matrix matched with the samples analyzed and the matrix
modifiers added. Standards with less than 1 /*g/ml of a metal were prepared daily; those
with concentrations greater than this were made monthly. A minimum of five standards
composed the standard curve. Quality control samples were prepared from a separate
10 jUg/ml standard by diluting it into the range of the samples.
One analytical spike was analyzed for every 10 samples. If recoveries were below
80 percent of 100, the samples were analyzed by method of additions as explained in
EPA SW 846 Method 7000. One QC sample was analyzed to verify the standard curve
used to quanitate the samples.
JBS336
-------
5.2 EMISSIONS TESTING FOR PARTICULATE MATTER LESS THAN 10
MICRONS/CONDENSIBLE PARTICULATE MATTER
The sampling method for fine paniculate matter/condensible paniculate matter
(PM10/CPM) was a combination of the protocols outlined in EPA Method 201A [entitled
"Determination of PM10 Emissions (Constant Sampling Rate Procedure)"] and EPA
Method 202 (entitled "Determination of Condensible Emissions from Stationary
Sources"), These methods are presented in Appendix J.2, and are summarized below.
Method 201A is applicable to the measurement of PM emissions with aerodynamic
diameters less than or equal to 10 microns (PM10). Method 202 applies to the
determination of CPM from various types of combustion devices. Condensible PM
emissions are gaseous matter and aerosols that condense after passing through a filter
that captures liquid and solid particulates. Analyses of the test samples were performed
for total PM (including PM greater than 10 /im), PM10, and CPM. Total PM emission
rates were determined from the PM/metals train.
Particulate matter emissions larger than 10 microns were determined by
measuring the weight of the catch of an in-stack PM10 cyclone. The PM10 emissions were
determined from the weight gain of an in-stack backup filter that was downstream of the
cyclone. The CPM emissions were determined from the evaporated residue of the
impinger solution, as outlined in Section 5.2.5.2
5,2.1 Sampling Equipment for PM10/CPM
Figure 5-4 shows the sampling train for the PM10/CPM method, which combined
the in-stack cyclone, filter assembly, and probe from EPA Method 201A with the
impinger assembly from EPA Method 202. The sample train consisted of a tapered
stainless steel inlet nozzle, an in-stack PM10 cyclone, a backup filter holder and filter
behind the cyclone, a heated glass probe liner, a series of 4 impingers, and the standard
EPA Method 17 meterbox and vacuum pump.
The instrument used in PM10 determination was a Sierra Instruments Series 280
Cyclade™ cyclone. This device collected particulates larger than 10 microns and allowed
particulates smaller than 10 microns to pass through to a backup filter. The cyclone
JBS336
5-18
-------
Temper ad use
Saw*
Thermometer
Cyclone
£
Figure 5-4. PM/CPM Sampling Train
-------
caused the gas stream to swirl in a vortex; larger particulates contacted the cyclone wall
and fell into a collection cup.
The in-stack backup filter used after the cyclone had a demonstrated collection
efficiency of greater than 99.95 percent on diocytylphepthalate (DOP) smoke particles, as
required by ASTM Standard Method D 2986.
As outlined in EPA Method 202, the first two impingers each contained 100 ml of
deionized distilled H20, the third impinger was empty, and the fourth contained silica gel.
The first two impingers were of the Greenburg-Smith design with standard tips; the other
impingers had straight tubes. The impingers were connected together with clean glass U-
tube connectors.
5.2.2 PM10/CPM Sampling Equipment Preparation
5,2.2.1 Glassware Preparation. Glassware was washed as follows:
• Washed in hot soapy water;
• Rinsed with tap water;
• Rinsed with deionized distilled water;
• Rinsed with acetone; and
• Rinsed with methyiene chloride (MeCl2).
The cleaned glassware was allowed to air dry in a contamination-free environment.
After drying, the ends were covered with parafilm. All glass components of the sampling
train plus any sample bottles, pipets, Erlenmeyer flasks, petri dishes, graduated cylinders,
and other laboratory glassware used during sample preparation, recovery, and analysis
were cleaned according to this procedure.
The cyclone housing, nozzle, and interior surfaces were cleaned with hot, soapy
water, rinsed with hot tap water, rinsed with distilled deionized water, and finally rinsed
with acetone and dried.
JBS336
5-20
-------
5.2.2.2 Reagent Preparation. The deionized distilled reagent water used
conformed to the American Society for Testing and Materials Specification D 1193-74,
Type II.
5.2,2.3 Equipment Preparation. All measuring devices used during sampling were
calibrated prior to use, as specified in EPA Method 17. This equipment included top
loading scales, probe nozzles, pilot tubes, metering system, probe heater, temperature
gauges, dry gas metering system, and barometer. A laboratory field notebook was
maintained to record these calibration values.
Before they were used, all filters were desiccated and tared on a five-place
balance. Replicate weighings at least 6 hours apart must agree to within 0.5 mg to yield
an acceptable weight. Each filter was then stored in an individual petri dish with an
identification number, and all data were recorded in the logbook.
5.2.3 Sampling Operations for PMIO/CPM
The sampling procedure for the PM10/CPM method is similar to the procedure
for EPA Method 5, except that the PM10/CPM method includes a post-test nitrogen (N2)
purge to purge SO2 from the sample, if considerable amounts of SO2 are present in the
flue gas. Also, a different method was used for nozzle size selection and sampling time,
and no silicone grease was used in assembling the sample train in order to avoid
contamination.
Prior to sampling for PM]0, a preliminary velocity traverse was performed.
Moisture content, flue gas molecular weight, and temperature were determined using
EPA Methods 1 through 4. These data were used to determine the appropriate sampling
rate (as outlined in EPA Method 201A) through the cyclone and to select an appropriate
sampling nozzle or nozzles. Since a constant sampling rate was required throughout a
given run, more than one nozzle was required to maintain approximate isokinetic
sampling conditions. In preparation for sampling, the tester calculated an appropriate
nozzle size for each anticipated range of pitot readings (delta P), such that isokinetics
could be maintained within ±20 percent of the constant sampling rate.
In addition to the above mentioned preliminary data, particulate loading was also
known in order to calculate the required run duration to achieve a representative sample
JBS336 *"21
-------
in the cyclone. Because of the complexity of the PM10 method, only experienced
samplers performed the sample tests,
The impinger train was prepared according to EPA Method 5. Teflon tape was
used to provide leak-free connections between glassware. The impingers and impinger
contents were weighed and the weights recorded. The sample train components were
carefully assembled in the recovery trailer except for attachment of the cyclone, backup
filter, and probe, which was performed at the stack sampling location.
The train was assembled at the stack location by connecting the cyclone, filter,
and probe liner to the impinger train, which was connected to the meterbox. After the
probe and filter heaters were turned on, the train was leak checked at 15 in. Hg. The
leak rate must be below 0.02 cfm.
The samples were withdrawn at a constant flow rate from the stack at the traverse
points determined by EPA Method 1. The sampling time at each point was based on the
relative gas velocity at that point. A leak check was performed before and after each
sample test. Parafilm or Teflon tape was used to seal the train components at the end of
each test. As soon as possible after the post-test leak check, the probe was disconnected
from the impinger train.
5.2.4 Sample Recovery for PMie/CPM
Recovery procedures began as soon as the probe was removed from the stack at
the end of the sampling period. The recovery scheme is shown in Figure 5-5. To
facilitate transfer from the sampling location to the recovery trailer, the sampling train
was disassembled into four sections: the cyclone, the filter holder, the nozzle/probe liner,
and the impingers in their bucket. Each of these sections was capped with parafilm or
Teflon tape before being transported to the recovery trailer.
5.2.4.1 Cyclone Recovery. The cyclone was disassembled and the nozzle
removed. The PM was quantitatively recovered from the interior surfaces of the nozzle,
cyclone, and collection cup (excluding the exit tube) by brushing with a nylon bristle
brush and rinsing with acetone until the rinse showed no visible particles. After this
procedure, a final rinse of the cyclone surfaces and brush was performed. All paniculate
and acetone rinse was collected in a sample jar and sealed. The liquid level was marked,
JBS336 5-22
-------
Ul
fe
Nozzle/I
Dry br u
Cyclone / Front-half Back-half / /
Cyclone But / Filter Filler / Probe / Connecting Imi
' Holder Filler Holder ' Extension ' Glassware N
sh Into
tared aluminum foil
(excluding the
turn around" cup)
Rinse
brusl
WtttM
(Bnea
L ••> jj OmLJtWFVL
QAO RiflSt aiiu rvgiiN^i
H3X bnah3X ftterhol
alone wtth acetone place In
•ssary) petrl
efroni
derand
original
diah
Silic
^° !mP"
Wetghfor
moisture
ga
Emj
cont
Into Si
corrtf
In
a Gel
igere
Weigh for
*1 mouture
anla gain
wnple a
»lner
Inspect and
discard If
latlqued
Ariri riruJrvui Bowh loose Rinse 2 Rinse 2 times
to^umte any partteulale times wrth wtthwalerand
toaampw ^bteon walerand addlo
finer holder add to container
onto
fitter Implngare HjO
Rinae2Umes FUnseSttmee
with MeCl, wthMeOj
and add lo and add to
MeCljConubner MeC^ container
I
I
rv.r.lnno Dinao rur-inna Dlnaa FUtar FUnaa Filter M6Uj
H,
Figure 5-5. PM10/CPM Sample Recovery Scheme
-------
and the jar was identified. This information was logged into the field notebook.
The above procedure was repeated for all interior surfaces from the exit tube to
the front half of the in-stack filter. The acetone rinse was collected in a separate sample
jar, sealed, identified, the liquid level was marked, and the sample information was
logged into the field notebook.
5,2.4.2 In-stack Filter Recovery. The in-stack filter holder was opened and the
filter was removed with tweezers or rubber gloves. The filter was placed in a marked
petri dish sealed with Teflon tape, and the filter number was logged into the field
notebook.
5,2.4.3 Probe and Impingers Recovery. The weight or volume gain in each of the
impingers was recorded and used to determine the moisture content in the flue gas. The
liquid from the three impingers was transferred into a clean glass sample jar. The
impinger bottles, back half of the filter holders, and probe liner were rinsed twice with
water, the rinse water was added to the same sample bottle, and the liquid level was
marked on the bottle.
Following the water rinses, the impingers, filter holder, and probe were rinsed
twice with MeCl2. The MeCl2 rinse was saved in a clean glass sample jar and the liquid
level was marked. The sample information was logged into the field notebook.
All sample jars were fully identified and sealed. Pertinent information was logged
into the field notebook.
5.2.4.4 Field Blanks. Field blanks of water (500 ml), MeCl2 (a volume
approximately equal to the volume used for the MeCl2 rinses), and acetone (200 ml)
were taken. Each reagent blank was of the same lot as was used during the sampling
program. Each lot number and reagent grade were recorded on the field blank label
and recorded into the field notebook.
JBS336
5-24
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5.2.5 Analysis for PM10/CPM
The PM10/CPM gravimetric analyses were completed as shown in Figure 5-6.
Sample jars were checked to ascertain if leakage during shipment had occurred. If
sample loss occurred during shipment, the sample may have been voided or a method
may have been used to incorporate a correction factor to scale the final results
depending on the volume of the loss.
5,2.5.1 Cyclone Catch Analysis. The dry cyclone catch, stored in foil; the cyclone
rinse; and the front half filter rinses were analyzed gravimetrically according to EPA
Method 5. Each rinse was evaporated at 70°F in a tared beaker to dryness. The residue
was then desiccated at room temperature for 24 hours to a constant weight in a
desiccator containing anhydrous calcium sulfate. To be considered constant weight, each
replicate weighing must agree to within 0.5 mg and must be at least 6 hours apart.
Weight gain for each fraction was reported to the nearest 0.1 mg. This weight gain
constituted the PM greater than 10 microns in size.
5.2.5.2 Filter Catch Analysis. ,The in-stack filter catch was analyzed
gravimetrically according to EPA Method 5 requirements.
For each filter, the filter and loose particulates were transferred to a tared glass
weighing dish and dried for 24 hours in a desiccator containing silica gel. The sample
was weighed to a constant weight, with results reported to the nearest 0.1 mg. The
resulting weight gain from the filter and exit tube acetone rinses constituted the
noncondensible PM10 portion of the sample.
5.2.5.3 Impinger and Probe Sample Rinse Analysis. Data were recorded on the
data sheet shown in Figure 5-7. The water sample was measured volumetrically.
The MeCl2 sample was combined with the water sample in a 1000-mi separatory
funnel. After mixing, the aqueous and organic phases were allowed to separate; most of
the organic/MeCl2 phase was drained off and collected in a tared 350-ml weighing tin
(approximately 100 ml). Then 75 ml of MeCl2 was added and mixed; again most of the
organic MeCl2 was drained into the weighing tin. This procedure was repeated with
another 75 ml of MeCl2. A total of approximately 250 ml of organic extract was drained
into the weighing tin. No water was drained during this procedure.
JBS336 5-25
-------
Cyclone Cfflch
Cyclone Catch
(if used)
Determine
total sample
volume
Transfer contents
to tared
breaker
Acetone
Determine
total sample
volume
Transfer corrtente
to tared
breaker
Finei
Determine
tot el sample
volume
H20
Determine
total sample
volume
Dessteate and wetah
to a constant weight
Dessicate and weigh
lo a constant weight
Desstoste and weigh
to a constant wetghl
Desalcate and weigh
to a constant weight
' Combine contents '
in 1000 mt
Separatory runnel
Mix allow to
separate, drain, (save)
moslofMeCb
phase Into MeCI2
sample container
Add 75 mis of
MeCI jio sepa/atory
runnel and repeat
above procedure
Repeat above
I
Transfer MeOj
contents to tared
beaJw
I
Allow to evaporate
at room tamperadure
under, a hood
I
Place HjO In a
pre-cleaned
container and
evaporated to 50 ml
on a hot plate
or equMlenf
DasaJcate and weigh
lo a constant weight
Place In a tared
beaker and evaporate
to dryneaa In a
10S°Coven
Desaicale and weigh
to a constant weight
Figure 5-6. PM1Q/CPM Analytical Scheme
-------
Moisture Determination
Volume or weight of liquid In impingers_
Weight of moisture in silica gel "m
ml or g
g
Sample Preparation (Container No. 4)
Amount of liquid lost during transport
Final volume
pH of sample prior to analysis
Addition of NH,OH required?
Sample extracted 2X with 75 ml MeClz?
For Tltratlon of Sulfate
Normality of NH4OH
Volume of sample titrated
Volume of tUrant
ml
ml
N
ml
ml
Sample Analysis
Container
number
weight of Condensible Participate, mg
Final Weight Tare Weight Weight Gain
4 (Inorganic)
4 & 5 (Organic}
Total
Less Blank
Weight of Condensible Particulate
Figure 5-7. Analytical Data Sheet
5-27
-------
Organic Fraction Weight Determination
The organic extract was evaporated under a laboratory hood. Following
evaporation, it was dried for 24 hours in a desiccator containing silica gel. The resulting
sample was weighed to the nearest 0.1 rag.
Inorganic Fraction Weight Determination
The water sample was evaporated on a hot plate to approximately 50 ml, then
evaporated to dryness in a 105°C oven. Because no N2 recovery purge was used, the
sample was then desiccated and weighed to a constant weight.
5.2.5.3 Field Blank Analysis. The acetone field blank was measured
gravimetrically and transferred to a 250-ml beaker. The sample was evaporated to
dryness, desiccated for 24 hours, and weighed to a constant weight.
The MeCl2 and water field blanks were analyzed as described in Sections 1.2.5.2.1
and 1.2.5.2.2 of the test method, respectively. Blank correction was not required,
because the sum of the values for the water blank and the MeQ2 blank was less than
2 mg or 5 percent of the mass of the CPM, whichever is greater.
5.3 ALDEHYDES EMISSIONS TESTING
Sampling for aldehydes was performed according to EPA SW-846 Test
Method 0011, "Sampling for Aldehyde and Ketone Emissions from Stationary Sources."
5.3.1 Sampling Equipment for Aldehydes
This methodology used the sampling train shown in Figure 5-8. The
four-impinger train consisted of a quartz nozzle/probe liner followed by a series of
impingers and the standard EPA Method 5 meterbox and vacuum purnp. The contents
of the sequential impingers were: the first two impingers with 2,4-dinitrophenylhydrazine
(DNPH), the third impinger empty, and the fourth impinger with silica gel. The first,
third, and fourth impingers were of the Greenburg-Smith design; the second impinger
had a straight rube. The impingers were connected together with clean glass U-tube
connectors. Sampling train components were recovered and analyzed in several fractions
in accordance with the described method.
JBS336
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Temperature
Sensor
Thermometer
S-Type Pttrt Tube \
Modified Greenburg
Smith Implngers
(Mice
Manometer
Figure 5-8. Aldlehyde Sampling Train
-------
5.3.2 Sampling Equipment Preparation for Aldehydes
5,3.2.1 Glassware Preparation. Glassware was washed in hot, soapy water, rinsed
with tap water three times, and then rinsed with delonized distilled water three times.
The glassware was then rinsed with methylene chloride, drained, dried, and heated in a
laboratory oven at 130°C for several hours. Solvent rinses with methanol were
substituted for the oven heating. After drying and cooling, glassware was stored in a
clean environment to prevent any accumulation of dust or other contaminants.
5.3.2.2 Reagent Preparation. Reagent grade chemicals were used in all tests and
conformed to the specifications of the Committee on Analytical Reagents of the
American Chemical Society.
The reagent water was organic-free reagent water. The lot number, manufacturer,
and grade of each reagent that was used were recorded in the laboratory notebook.
The DNPH absorbing solution was prepared according to Section 3.5.5.4,2 of the
reference method. The analyst wore plastic gloves and safety glasses when handling
DNPH crystals or solutions. Reagent bottles for storage of cleaned DNPH derivatizing
solution were rinsed with acetonitrile and dried before use.
5.3.2.3 Equipment Preparation. The remaining preparation included calibration
and leak checking of all train equipment as specified in EPA Method 5. This equipment
included probe nozzles, pilot tubes, metering system, probe heater, temperature gauges,
leak check metering system, and barometer. A field laboratory notebook was maintained
to record these calibration values.
5.3.3 Aldehydes Sampling Operations
5,3.3.1 Preliminary Measurements. Prior to sampling, preliminary measurements
were required to ensure isokinetic sampling. These included determining the traverse
point locations, performing a preliminary velocity traverse, cyclonic flow check, and
moisture determination. These measurements were used to calculate a K factor. The
K-factor was used to determine an isokinetic sampling rate from stack gas flow readings
taken during sampling.
Measurements were then made to verify the duct inside diameter, port nozzle
length, and the distances to the nearest upstream and downstream flow disturbances.
JBS336 "0
-------
These measurements were then used to determine sampling point locations by following
EPA Reference Method 1 guidelines. The distances were then marked on the sampling
probe using an indelible marker.
5,3.3.2 Assembling the Train. Initial assembly of the aldehyde sampling train
components was completed at the recovery trailer. First, the empty, clean impingers
were assembled and laid out in the proper order in the recovery trailer. Each ground
glass joint was carefully inspected for hairline cracks. The first impinger was of the
Greenburg-Smith design and contained DNPH. The second impinger was a straight tube
and also contained DNPH. The third impinger, of the Greenburg-Smith design, was
empty, and served as a knockout to collect condensate. The fourth impinger contained
200 to 300 grams of blue indicating silica gel.
After the impingers were loaded, each impinger was weighed, and the initial
weight and contents of each impinger was recorded on a recovery data sheet. Final
assembly of the sampling train components was completed at the stack location. The
impingers were connected using clean, glass U-tube connectors. The height of all
impingers was approximately the same to obtain a leak-free seal. The open ends of the
train were sealed with ground-glass caps.
5.3.3.3 Sampling Procedures. After the train was assembled, the heaters for the
probe liner were turned on. When the system reached the appropriate temperature, the
sampling train was ready for pretest leak checking. The probe temperature was
maintained above 100°C (212°F). The sampling trains were leak checked at the start
and finish of sampling. An acceptable pretest leak rate was less than 0.02 acfm (ft3/min)
at approximately 15 in. Hg. If, during testing, a piece of glassware needed to be emptied
or replaced, a leak check was performed before the glassware piece was removed and
after the train was reassembled.
To leak check the assembled train, the nozzle end was capped off and a vacuum
of 15 in. Hg was pulled through the system. When the system was evacuated, the volume
of gas flowing through the system was timed for 60 seconds. After the leak rate was
determined, the cap was slowly removed from the nozzle end until the vacuum dropped
off, and then the pump was turned off. If the leak rate requirement was not met, the
JBS336 5-31
-------
train was systematically checked by first capping the train at the first impinger, the
second impinger, etc., until the leak was located and corrected.
After a successful pretest leak check had been conducted, all train components
were at their specified temperatures, and initial data were recorded (DGM reading), the
test was initiated. Sampling train data were recorded periodically on standard data
forms.
The leak rates and sampling start and stop times were recorded on the sampling
task log. Also, any other occurences during sampling were recorded on the task log,
such as pitot cleaning, thermocouple malfunctions, heater malfunctions, or any other
unusual occurrence.
At the conclusion of the test run, the sample pump (or flow) was turned off, the
probe was removed from the duct, a final DGM reading was taken, and a post-test leak
check was completed. The procedure was identical to the pretest procedure, but the
vacuum should have been at least one in. Hg higher than the highest vacuum attained
during sampling. An acceptable leak rate was less than 4 percent of the average sample
rate or 0.02 acfm (whichever is lower). If a final leak rate did not meet the acceptable
criterion, the test run may still have been accepted upon approval of the test
administrator.
5.3.4 Aidehydes Sample Recovery
Recovery procedures began as soon as the probe was removed from the stack and
the post-test leak check was completed.
To facilitate transfer from the sampling location to the recovery trailer, the
sampling train was disassembled into two sections: the nozzle/probe liner, and the
impingers in their bucket. Each of these sections was capped before being removed to
the recovery trailer.
Once in the trailer, the entire sampling train was recovered into one sample
container. The weight gain in each of the impingers was recorded to determine the
moisture content in the flue gas. Following weighing of the impingers, the nozzle/probe
was recovered. The probe liner was rinsed with methylene chloride by tilting and
rotating the probe while squirting methylene chloride into its upper end so that all inside
c-17
JBS336 J J£-
-------
surfaces were wetted. The methylene chloride was quantitatively collected into the
sample container. This rinse was followed by additional brush/rinse procedures; the
probe was held in an inclined position and methylene chloride was squirted into the
upper end as the brush was pushed through with a twisting action. The procedure was
performed three times. The brush was also rinsed with methylene chloride and the
washing liquid was quantitatively collected in the sample container.
The first three impingers were then rinsed three times with methylene chloride
and the washing was collected in the same sample container that was used for the probe.
There were at least two liquid phases in the impingers. This two-phase mixture did not
pour well and a significant amount of the impinger catch was left on the walls after the
methylene chloride rinse. The use of water as a final rinse helped make the recovery
quantitative.
After all methylene chloride and water washing and particulate matter had been
collected in the sample container, the lid was tightened so solvent, water, and DNPH
reagent did not leak out.
A sample blank was prepared by using an amber flint glass container and adding
a volume of DNPH reagent and methylene chloride equal to the total volume in the first
container.
The silica gel from the train was saved in a bag for regeneration after the job was
completed. The ground-glass fittings on the silica gel impinger were wiped off after
sample recovery to ensure a leak-tight fit for the next test.
The liquid level of each sample container was marked on the bottle in order to
determine if any sample loss occurred during shipment. If sample loss had occurred, the
sample would be voided or a method would have been used to incorporate a correction
factor to scale the final results depending on the volume of the loss.
JBS336
5-33
-------
5.3.5 Aldehydes Analysis
The methylene chloride extract was solvent exchanged into acetonitrile prior to
HPLC analysis. Liquid chromatographic conditions are described which permit the
separation and measurement of formaldehyde in the extract by absorbance detection at
360 nm.
5.3.6 Quality Assurance for Aldehydes
The quality assurance (QA) program required for this method included the
analysis of the field and method blanks, procedure validations, and analysis of field
spikes. The assessment of combustion data and positive identification and quantitation
of formaldehyde were dependent on the integrity of the samples received and the
precision and accuracy of the analytical methodology. The OA procedures for this
method were designed to monitor the performance of the analytical methodology and to
provide the required information to take corrective action if problems were observed in
laboratory operations or in field sampling activities.
Field blanks were submitted with the samples collected at each sampling site.
The field blanks included the sample bottles containing aliquots of sample recovery
solvents, methylene chloride and water, and unused DNPH reagent. At a minimum, one
complete sampling train was assembled in the field staging area, taken to the sampling
area, and leak checked at the beginning and end of testing. The probe of the blank train
was heated during the sample test. The train was recovered as if it were an actual test
sample. No gaseous sample was passed through the blank sampling train.
To evaluate contamination and artifacts that can be derived from glassware,
reagents, and sample handling in the laboratory, a method blank was prepared for each
set of analytical operations.
A field spike was performed by introducing 200 /*! of the field spike standard into
an impinger containing 200 ml of DNPH solution. Standard impinger recovery
procedures were followed and the spike was used as a check on field handling and
recovery procedures. An aliquot of the field spike standard was retained in the
laboratory for derivatization and comparative analysis.
JBS336 5-34
-------
5,4 NQNMETHANE HYDROCARBON ANALYSIS BY METHOD 25A AND
C1-C6 BY METHOD 18
Benzene, toluene, and xylene concentrations were determined according to EPA
Method 18. Total gaseous hydrocarbon (THC) concentrations were determined
according to EPA Method 25A. Methane concentrations were determined by subtracting
the results of EPA Method 18 from EPA Method 25A.
The instrument used to determine THC utilized a flame ionization detector
(FID). For FIDs, the flue gas entered the detector and hydrocarbons were combusted in
a hydrogen flame. The ions and electrons formed in the flame entered an electrode gap,
decreased the gas resistance, and permitted a current flow in an external circuit. The
resulting current was proportional to the instantaneous concentration of the total
hydrocarbons.
The flue gas was analyzed by a Ratfisch Model 55 analyzer. The analyzer utilized
a FID. The results are reported on a methane basis. Methane was used as the
calibration gas.
EPA Method 18 analysis was performed using gas chromatography (GC) to
separate the hydrocarbon (Q - C6) species present in the gas stream. Prior to sampling
of the source gas, the GC/FID system was calibrated with standard gas mixtures
containing each hydrocarbon (CH4, CjH^ C3H6, C4H10, C5H12, and C6HJ4) to establish
calibration curves and retention times. The calibration curves and retention times were
used to quantify the concentrations in the source samples.
A heat-traced slipstream from the stack was transferred to the Shimadzu Mini2
GC/FID to prevent any condensation of the sample gas. The gas sampling loop of the
GC/FID was also heated and was purged each time a sample was analyzed. A
schematic of the CEM and GC system is shown in Figure 5-9. Each analysis was
approximately 10 to 15 minutes in duration. Thus, this analysis was semicontinuous with
a result being generated approximately every 5 to 10 minutes during the sampling period.
The source sample was drawn into the GC sampling loop under conditions that
prevented any condensation of the sample gas. The sample was injected into the GC
and the hydrocarbon compounds were separated by absorbing them onto the column and
JBS336
5-35
-------
StBCKWBll
Noi.3Ci.ca
O,T>C.CO
CaVQC
Heal Trace
Unherted Qaa LJnag
Signal Wlr*
Figure 5-9. Schematic of CEM System
5-36
-------
desorbing them at different times. As each hydrocarbon compound was eluted, it was
combusted in the hydrogen flame of the FID. The ions and electrons formed in the
flame entered an electrode gas, decreased the gas resistance, and permitted a current
flow in an external circuit. The resultant current was proportional to the instantaneous
concentration of the hydrocarbon.
The response and retention times of the individual hydrocarbons were recorded
on a strip chart recorder. A built-in integrator measured the peak areas and printed out
the retention times and counts. The peaks were identified from the established retention
times and the concentration of each hydrocarbon was determined by referring to the
calibration curve.
The nonmethane hydrocarbon concentration was calculated by subtracting the
average methane concentration as measured by GC/FID (EPA Method 18) from the
average total hydrocarbon concentrations by EPA Method 25A.
5.5 EPA METHODS 1-4
5.5.1 Traverse Point Location Bv EPA Method 1
The number and location of sampling traverse points necessary for isokinetic and
flow sampling was dictated by EPA Method 1 protocol. These parameters were based
upon how much duct distance separated the sampling ports from the closest downstream
and upstream flow disturbances. The minimum number of traverse points for a square
duct of this size was 28. A set of perpendicular sampling ports was established in the
stack.
5.5.2 Volumetric Flow Rate Determination by EPA Method 2
Volumetric flow rate was measured according to EPA Method 2. A Type K
thermocouple and S-type pilot tube were used to measure flue gas temperature and
velocity, respectively. All of the isokinetically sampled methods that were used
incorporate EPA Method 2.
5.5.2.1 Sampling and Equipment Preparation. For EPA Method 2, the pilot
tubes were calibrated before use following the directions in the method. Also, the pilots
were leak checked before and after each run.
JBS336
5-37
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5.5.2.2 Sampling Operations. The parameters that were measured included the
pressure drop across the pilots, stack temperature, stack static and ambient pressure.
These parameters were measured at each traverse point, as applicable. A computer
program was used to calculate the average velocity during the sampling period.
5.5.3 O2 and CO, Concentrations by EPA Method 3A
The O2 and CO2 concentrations were determined by CEMs following EPA
Method 3A. Flue gas was extracted from the duct and delivered to the CEM system
through heated Teflon® tubing. The sample stream was then conditioned (particulate
and moisture removed) and was directed to the analyzers. The O2 and CO2
concentrations were, therefore, determined on a dry basis. Average concentrations were
calculated to coincide with each respective time period of interest. More information on
the CEM system will be given in Section 5.6.
5.5,4 Average Moisture Determination by EPA Method 4
The average flue gas moisture content was determined according to EPA
Method 4. Before sampling, the initial weight of the iiupingers was recorded. When
sampling was completed, the final weights of the impingers were recorded, and the
weight gain was calculated. The weight gain and the volume of gas sampled were used
to calculate the average moisture content (percent) of the flue gas. The calculations
were performed by computer. EPA Method 4 was incorporated in the techniques used
for all of the manual sampling methods that were used during the test.
5.6 CONTINUOUS EMISSIONS MONITORING METHODS
EPA Methods 3A, 7E, 6C, and 10 were the continuous monitoring methods used
for measuring CO2/O2, NOX, SO2, and CO concentrations, respectively. Total
hydrocarbons were .analyzed by EPA Method 25A. A diagram of the CEM system is
shown in Figure 5-9.
One extractive system was used to obtain flue gas samples for the CEM systems.
For the main CEM system, samples were withdrawn continuously at a single point from
the outlet duct and transferred to the CEM trailer through heat-traced Teflon® line.
The flue gas was conditioned (temperature lowered and moisture removed) before the
flue gas stream was split through a manifold to the various analyzers. Total hydrocarbon
5-38
JBS336
-------
measurements were made on an unconditioned, hot basis. Therefore, this sample stream
bypassed the gas conditioner.
5.6.1 GEM Sampling Equipment
5.6.1.1 Sample Probes. The main CEM probe consisted of a black iron pipe
mounted to a Swagelok® reducing union which was attached directly to the heat trace
tubing. The probe was placed approximately at a point of average velocity in the stack
determined by a prior velocity traverse by EPA Method 2,
5,6.1.2 Heated Lines. Heated sample lines were used to transfer the flue gas
samples to the instrument trailer for O2, CO2, NO^ SO2, CO, and THC analyses, These
lines were heated in order to prevent condensation. Condensate could clog sample lines
or provide a medium for the flue gas sample to react and change composition.
All heat trace lines contained three 3/8-inch Teflon® tubes. One tube carried the
sample, one tube was used for calibration and QC gases, and the other was available as
a backup. Calibration and QC gases were directed to the sampling probe through the
transfer tube and then back through the entire sampling/conditioning system.
5,6.1.3 Gas Conditioning. Special gas conditioners were used to reduce the
moisture content of the flue gas. A Radian designed gas conditioning system utilized a
chiller system to cool a series of glass cyclones. An antifreeze liquid system was used to
chill the glass cyclones. The hot flue gas was chilled by heat conduction through the
glass wall causing the moisture to condense into droplets. The droplets and any PM
were flung outward toward the glass walls by the centrifugal force. Particles impacted
the glass walls and fell to the bottom of the cyclone where they were drained from the
system. In this manner, both moisture and PM were effectively removed from the flue
gas sample stream. This system operated under positive pressure eliminating the
possibility of leakage which would dilute the gas samples. The gas conditioner was
located in the CEM trailer.
5.6.2 CEM Principles of Operation
5.6.2.1 Sulfur Dioxide Analysis. The Western 721A SO2 analyzer was essentially
a continuous spectrophotometer in the ultraviolet range. Sodium dioxide selectively
absorbed ultraviolet (UV) light at a wavelength of 202.5 nm. To take advantage of this
JBS336 5-39
-------
property of SO2, the analyzer emitted UV light at 202.5 run and measured the
absorbance (A) of the radiation through the sample cell by the decrease in intensity.
Beer's law, A = abc, was used to convert the absorbance into SO2 concentration
(A = absorbance, a = absorbitivity, b = path length, c = concentration). Sulfur dioxide
measurements were performed using EPA Method 6C.
5.6.2.2 Nitrogen Oxide Analysis. The principle of operation of the TECO Model
10AR was a chemiluminescent reaction in which ozone (O3) reacted with nitric oxide
(NO) to form O2 and nitrogen dioxide (NO2). During this reaction, a photon was
emitted which was detected by a photomultiplier tube. The instrument was capable of
analyzing total oxides of nitrogen (NO + NO2) by thermally converting NO2 to NO in a
separate reaction chamber prior to the photomultiplier tube. Nitrogen oxide
measurements were performed using EPA Method 7E.
5.6.2.3 Oxygen Analysis. The Thermox WDG IV measured O2 using an
electrochemical cell. Porous platinum electrodes were attached to the inside and outside
of the cell, which provided the Instrument voltage response. Zirconium oxide contained
in the cell conducted electrons when it was hot from the mobility of O2 ions in its crystal
structure. A difference in O2 concentration between the sample side of the cell and the
reference (outside) side of the cell produced a voltage. This response voltage was
proportional to the logarithm of the O2 concentration ratio. A linearizer circuit board
was used to make the response linear. The reference gas was ambient air at
20.9 percent O2 by volume.
5.6.2.4 Carbon Dioxide Analysis. Non-dispersive infrared (NDIR) CO2 analyzers
emitted a specific wavelength of infrared radiation which was selectively absorbed by
CO2 molecules through the sample cell. The intensity of radiation which reached the
end of the sample cell was compared to the intensity of radiation through a CO2-free
reference cell. A reference cell was used to determine background absorbance which was
subtracted from the sample absorbance. The detector used two chambers filled with
CO2 and connected by a deflective metallic diaphragm. One side received radiation
from the sample cell and the other side received radiation from the reference cell. Since
more radiation was absorbed in the sample cell than in the reference cell, less radiation
JBS336 5-40
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reached the sample side of the detector. This caused a deflection of the diaphragm due
to increased heat from radiation absorption on the reference side. Deflection of the
diaphragm created an electrical potential which was proportional to absorbance.
Absorbance was directly proportional to CO2 concentration in the gas. Carbon dioxide
measurements were performed according to EPA Method 3A using a Beckman
Model 880 NDIR anlayzer.
5.6.2.5 Carbon J/lonoxide Analysis. A TECO Model 48 analyzer was used to
monitor CO emissions. The TECO analyzer measured CO using the same principle of
operation as CO2 analysis. A wave length of 5 nm is selective for CO. Carbon
monoxide measurements were performed using EPA Method 10.
5.6.2.6 Total Hydrocarbon Analysis. A Ratfisch Model 55 was used to monitor
THC emissions. By allowing the THC sample stream to bypass the gas conditioner,
concentrations were determined on a wet basis. The analyzer employed an FID. As the
flue gas entered the detector, the hydrocarbons were combusted in a hydrogen flame.
The ions and electrons formed in the flame entered an electrode gap, decreased the gas
resistance, and permitted a current flow in an external circuit. The resulting current was
proportional to the instantaneous concentration of the total hydrocarbons. This method
was not selective between species. EPA Method 25A applies to the continuous
measurement of total gaseous organic concentrations of primarily alkanes, alkenes,
and/or arenes (aromatic hydrocarbons). The results were reported on a methane basis
and methane was used as the calibration gas.
5.6.3 CEM Calibration
All the CEM instruments were calibrated once during the test program (and
linearized, if necessary) using a minimum of three certified calibration gases (zero and
two upscale points). Radian performed the multipoint calibrations with four general
categories of certified gases: zero gas (generally N2), a low scale gas concentration, a
midrange concentration, and a high scale concentration (span gas). The criterion for
acceptable linearity was a correlation coefficient (R2) of greater than or equal to 0.998,
where the independent variable was cylinder gas concentration and the dependent
variable was instrument response. If an instrument did not meet these requirements, it
JBS336 5-41
-------
was linearized by adjusting potentiometers on the linearity card within the instrument or
by other adjustments, if necessary.
The CEM analyzers were calibrated before and after each test ran (test day) on a
two point basis: zero gas (generally N2), and a high-range span gas. These calibrations
were used to calculate response factors used for sample gas concentration
determinations. Instrument drift as a percent of span was also determined using these
calibrations for each test run.
After each initial calibration, midrange gases for all instruments were analyzed,
with no adjustment permitted, as a quality control (QC) check. If the QC midrange gas
concentration observed was within ±2 percent of full scale, the calibration was accepted
and the operator began sampling. If the QC check did not fulfill this requirement,
another calibration was performed and linearization was performed if deemed necessary.
Calibration procedures are further detailed in the daily operating procedure
(Section 5.6.5).
Table 5-3 lists the concentration of all calibration and QC gases used on this test
program.
5.6.4 Data Acquisition
The data acquisition system consisted of a Dianachart PC Acquisitor data logger,
a signal conditioner, and a 386 desktop computer. All instrument outputs were
connected in parallel to stripchart recorders and the data acquisition system. The
stripchart recorders were a back-up system to the data logger. The PC Acquisitor
scanned the instrument output and logged digitized voltages. A Radian computer
program translated the digitized voltages into relevant concentrations in engineering
units (ppmv, %V, etc.). The computer program had several modes of operation:
calibration, data acquisition, data reduction, data view, data edit, and data import. The
import function was used to combine other data files for comparison and correlation.
5.6.5 Daily Operating Procedure
The following is a detailed standard operating procedure for calibrating and
operating the CEM system:
JBS336
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Table 5-3
CEM Operating Ranges And Calibration Gases
Analyte
Gas Concentration
CO2
Instrument
Range
Span Gas Value
Zero Gas
Midrange QC Gas Value
Low Range QC Gas Value
Beckman 880
0 - 20%
18%
100% N2 (UHP)
10%
5%
CO-dry
Instrument
Range
Span Gas Value
Zero Gas
Midrange QC Gas Value
Low Range QC Gas Value
TECO 48H
0 - 100 ppmvd
98 ppm
100% N2 (UHP)
60 ppm
20 ppm
O,
Instrument
Range
Span Gas Value
Zero Gas
Midrange QC Gas Value
Low Range QC Gas Value
Thermox WDG III
0-25%
20%
0.2% O2
10%
5%
SO,
Instrument
Range
Span Gas Value
Zero Gas
Midrange QC Gas Value
Low Range QC Gas Value
Western 721A
0 - 200 ppmvd
180 ppm
100% N2 (UHP)
100 ppm
30 ppm
JBS296
5-43
-------
Table 5-3
Continued
Analyte
Gas Concentration
NO,
Instrument
Range
Span Gas Value
Zero Gas
Midrange QC Gas Value
Low Range QC Gas Value
TECO 10AR
0 - 250 ppmvd
200 ppm
100% N2 (UHP)
100 ppm
50 ppm
THC (EPA Method 25A)
Instrument
Range
Span Gas Value
Zero Gas
Midrange QC Gas Value
Low Range QC Gas Value
Ratfisch RS-55
0 - 100 ppmvd
90% as methane
100% N, (UHP)
45 ppm as methane
25 ppm as methane
IBS29A
5-44
-------
JBS336
1. Turn on computer and printer, put printer on-line, and load the CEM.EXE
program. Be sure that the CEM instruments have been on for at least 20
hours.
2. Synchronize DAS clock with sample location leaders and the test leader.
3, Turn on strip chart recorders (SCR) and make appropriate notes on charts
and in logbook (write down all procedures and observations in logbook and
on SCRs as the day progresses),
4, Turn on the gas conditioners and blow back compressor. Blow back the
system.
5. Open all calibration gas cylinders so that they may be introduced to the
instruments via control panel valves.
6. Perform daily pretest leak check on CEMs by introducing ultra high purity
nitrogen to the system. Zero all instruments except the Thermox O2
analyzers. Make adjustments to the zero potentiometers as required to
zero the instruments. Be sure to check and maintain all flows throughout
calibration and operation.
7. Record the zero values in the computer calibration routine.
8. Introduce 2.0 percent O2 to set the low scale response for the Thermox O2
analyzers and repeat Step 7 for these instruments.
9, Introduce the mixed span gases for O2, CO2, and CO. Make adjustments
as required to these instruments.
10. Enter these values in the computer calibration routine,
11. Introduce the NOX span gas.
12. Make adjustments to the NOX instruments as required and enter the value
into the computer calibration routine.
13. Introduce the SO2 span gas for the SO2 analyzer, repeat Step 12 for the
SO2 analyzer. (Note that all calibration gases are passed through the entire
sampling system.)
14. Switch the Western SO2 analyzer range to 0-500 ppm introduce the span
gas for this range and repeat Step 12 for this instrument.
5-45
-------
15. Check the calibration table on the computer, and make a hardcopy. Put
the computer in the standby mode.
16. Introduce QC gases to instruments in the same sequence as the calibration
gases. Record three minutes of data for each, once the responses have
stabilized. If the QC gas response is not within ± 2 percent of the
instrument range the operator should recalibrate the instrument, or
perform other corrective actions.
17. Begin sampling routine, with the computer on stand by.
18. Start the data acquisition system when signaled by radio that system is in
stack.
19. Carefully check all flows and pressures during the operation of the
instruments and watch for apparent problems in any of the instruments,
such as unusual readings or unreasonable fluctuations. Check the gas
conditioning system periodically and drain the traps.
20. Stop the data acquisition system at the end of the test when signaled.
21. Perform final leak check of system,
22. Perform the final calibration (Repeat steps 6-16) except make no
adjustments to the system.
23. Check for drift on each channel.
5.7 POLYNUCLEAR AROMATIC HYDROCARBON EMISSIONS
TESTING
The polynuclear aromatic hydrocarbon (PAH) sampling and analytical method is
a combination of EPA SW-846 Test Method 0010 and EPA SW-846 Test Method 8270.
5.7.1 Sampling Equipment
The PAH sampling method used the sampling train shown in Figure 5-10. Radian
modified the protocol configuration to include a horizontal condenser rather than a
vertical condenser. The horizontal condenser lowered the profile of the train and
reduced breakage. The XAD trap following the condenser was maintained in a vertical
position.
JB5336 5"46
-------
Slack
Wall
Temperature /
Sensor
Gooseneck /
Nozzte /
~\\
Temperaiure Sensor
. Filler Holder
Temperaiure Sensor
Temperature Sensor
S-Type Pttot Tube
Heal Traced
Quartz Probe
Uner
Water Knockout 100 ml HPLC Water Empty
bnptngef
Vacuum
Line
Figure 5-10. PAH Sampling Train Configuration
-------
5.7.2 Sampling Equipment Preparation
In addition to the standard EPA Method 5 requirements, the PAH sampling
method included several unique preparation steps which ensured that the sampling train
components were not contaminated with organics that may interfere with analysis. The
glassware, glass fiber filters, and XAD resins were cleaned and checked for residuals
before being packed.
5.7.2.1 Glassware Preparation. Glassware was washed in soapy water, rinsed with
distilled water, baked, and then rinsed with acetone followed by methylene chloride.
This included all the glass components of the sampling train including the glass nozzles
plus any sample bottles, Erlenmeyer flasks, petri dishes, graduated cylinders or stirring
rods that were used during recovery. Nonglass components (such as the teflon-coated
filter screens and seals, tweezers, teflon squeeze bottles, nylon probe brushes and nylon
nozzle brashes) were cleaned following the same procedure except that no baking was
performed. The specifics of the cleaning procedure are presented in Table 5-4.
5.7.2.2 XAD II and Filters Preparation. XAD resin and glass fiber filters were
placed together in a soxhlet and extracted in HPLC-grade water, methyl alcohol,
methylene chloride and hexane, sequentially. At the conclusion of the soxhlet
extractions, one filter and 30 grams of XAD resin were analyzed for background
contamination following the same procedure followed for the flue gas samples. The
XAD and filter blank were analyzed for PAH compounds. The pressure drop for the
XAD traps was checked before and after the resin was loaded to ensure that the
pressure drop across the XAD traps was less than seven inches of mercury.
5.7.2.3 Method 5 Equipment Preparation. The EPA Method 5 equipment was
prepared according to the protocol discussed in Section 5.1.2.3.
JBS336 5-48
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Table 5-4
Glassware Cleaning Procedure
(Train Components and Sample Containers)
NOTE: USE DISPOSABLE GLOVES AND ADEQUATE VENTILATION
1. Soak all glassware in hot soapy water (Alconox*).
2. Tap water rinse to remove soap.
3. Distilled/deionized H2O rinse (X3).1
4. Bake at 450°F for 2 hours."
5. Acetone rinse (X3), (pesticide grade).
6. Methylene Chloride (X3).
7. Cap glassware with clean glass plugs or methylene chloride rinsed
aluminum foil.
8. Mark cleaned glassware with color-coded identification sticker.
'(X3) a Three times,
bStep (4) is not used for probe liners and non-glass components of the train that cannot
withstand 450°F (i.e., Teflon-coated filter screen and seals, tweezers, Teflon squeeze
bottles, nylon probe and nozzle brushes). The probe liners are too large for the baking
ovens.
5-49
-------
5.7.3 Sampling Operations
5.7.3.1 PreliminaryJMgasurements. Prior to sampling, preliminary measurements
were made as described in Section 5.1.3.1.
5.7.3.2 Assembling the Train. Initial assembly of the PAH sampling train
components was performed in the recovery trailer. Final assembly of the train with the
probe, nozzle, and filter was performed at the stack location. First, the empty, clean
impingers were assembled and laid out in the proper order. The first impinger was a
knockout impinger which had a short tip. The purpose of this impinger was to collect
condensate which formed in the coil and XAD trap. However, the gas was not bubbled
through the condensate to prevent carry-over to the next impinger. The next two
impingers were modified tip impingers that contained 100 ml of HPLC grade water each.
The fourth impinger was empty, and the fifth impinger contained 200 to 300 grams of
silica gel. When the impingers were loaded, they were wrapped with teflon tape to
secure the two sections of the impinger. Then each impinger was weighed and the
weight recorded along with information on the contents of the impingers. The impingers
were connected together using cleaned glass U-tube connectors and arranged in the
impinger bucket. The height of all the impingers should be approximately the same to
obtain a leak-free seal. The open ends of the train were sealed with methylene
chloride-rinsed aluminum foil.
The second step was to load the filter into the filter holder. The filter holder was
then capped off and placed with the XAD trap and condenser coil (capped) into the
impinger bucket. A supply of precleaned foil and socket joints were also placed in the
bucket in a clean plastic bag. The train components were transferred to the sampling
location and assembled as previously shown in Figure 5-10. Sealing greases were not
used to avoid contamination or adsorption of the sample.
5.7.3.3 Sampling Procedures. After the train was assembled, the heaters were
turned on for the probe liner and heated filter box. When the system reached the
appropriate temperatures, the sampling train was ready for leak checking.
The PAH train was leak checked at the start and finish of sampling as required in
EPA Method 5 as well as before and after each port change. If a piece of glassware
JBS336 5-50
-------
needed to be emptied or replaced, a final leak check was performed before the
glassware piece was removed. After the train was reassembled, an initial leak check was
performed.
To leak check the assembled train, the nozzle end was capped off and a vacuum
of 15 in, Hg was pulled in the system. When the system was evacuated, the volume of
gas flowing through the system was timed for 60 seconds. The leak rate is required to be
less than 0.02 acfm (ft3/min). After the leak rate was determined, the cap was slowly
removed from the nozzle end until the vacuum dropped off, and then the pump was
turned off.
If the leak-rate requirement was not met, the train was systematically checked by
first capping the train at the filter, at the first impinger, etc., until the leak was located
and corrected.
In the event that a final leak rate was found to be above the minimum acceptable
rate (0,02 acfm) upon removal from a port, acceptance is subject to the approved of the
EPA administrator. Otherwise, the run was voided and repeated.
The leak rates and sampling start and stop times were recorded on the sampling
task log. Also, any other events that occurred during sampling were recorded on the
task log such as pilot cleaning, thermocouple malfunctions, heater malfunctions and any
unusual occurrences.
Sampling train data were recorded every five minutes on standard data forms. A
checklist for sampling was given previously in Table 5-2. The purpose of the checklist is
to remind samplers of the critical steps during sampling.
A sampling operation that was unique to PAH sampling was maintaining the gas
temperature entering the XAD trap below 68°F. The gas was cooled by the condenser
and the XAD trap, which both have a water jacket in which ice water was circulated.
JBS336
5-51
-------
5.7.4 Sample Recovery
To facilitate transfer from the sampling location to the recovery trailer, the
sampling train was disassembled into four sections; the probe liner, the XAD trap and
condenser, filter holder, and the impingers in their bucket. Each of these sections was
capped with methylene chloride-rinsed aluminum foil before removal to the recovery
trailer. Once in the trailer, field recovery personnel followed the scheme shown in
Figure 5-11. The samples were placed in cleaned amber glass bottles to prevent light
degradation.
The solvents used for train recovery were acetone (pesticide grade) followed by
methylene chloride. The use of the highest grade acetone for train recovery was
essential to prevent the introduction of chemical impurities which interfere with the
quantitative analytical determinations.
Field recovery resulted in the sample components listed in Table 5-5. The
samples were shipped to the analytical laboratory as expediently and carefully as
possible.
5.7.5 Analytical Procedures
The analytical procedure used to determine PAH concentrations from the
Modified Method 5 sample followed EPA SW-846 Test Method 8270 protocol. The
detection limit for PAH was about 1 /ig per train. The compounds/isomers of interest in
the analysis are shown in Table 5-6.
5.7.5.1 Preparation of Samples for Extraction. Upon receiving the sample
shipment, the samples were checked against the chain-of-custody forms and then
assigned an analytical laboratory sample number. Each sample component was
reweighed to determine if leakage occurred during travel. Color, appearance, and other
particulars of the samples were noted. Samples were extracted within 21 days of
collection.
Glassware used in the analytical procedures (including soxhlet apparatus and
disposable bottles) was cleaned by washing twice with detergent, rinsing with distilled
water, and then rinsing with acetone, methanol, and methylene chloride. The glassware
was allowed to air dry.
JBS336 *-52
-------
Probe Liner
Cyclone
Front Han
Filter House
Filler Support
and Back Half
of Finer
Filter Housing
Condennet
isllmpingef Shlmplnger
XAD Trap (knockout) 2nd Imping*! 3rd Impinger 4ih Implnger (aillca gel)
* I * * i (•
I
I
Attach
2SOmL flask
to bafl joint
Rinse wtth
ftMhanoi
empty flask
ttofeOmL
U)
Brush Hner
and rinse
vRh3
elqueilsof
acetone
Check Knar
toaeeir
partJcuMe
Brush and
rinse with
methanol
untt
particulate
(•removed
Then rinse
3 times with
methylene
chloride
Brush and
rinse with
methanol
PX)
Rime wth
methylene
chloride
P*)
• not repeal
3
Htneewth
3aHqoutB
of methylene
chloride
Carefully Rinse with
remove fmer methanol
from support (3x)
wtth tweezers
Rinse wth
Brush
parttculate chloride
ontolttar pW
SeeJpetrl
db
sh
Rinse with Secure XAD Weigh Weigh
melhanol trap Implnger Impinger
PX) openings
wbh glass Empty Empty
Rlrue with balb and contents Into contents Into
methyteiie clamps bottle bottle
chlorida
PX) Place in
cooler (or
storage
Rinse
iwfth Rinse
iwflh
methanol methanol
P*) . PX)
Rinse wtth Rinse wtth
methi
chto
P
Iftene methyl*rw
ride chloride
x) P
")
Weigh Weigh
Implnger Implnger
Empty Empty
contents Into contents Into
bottle bottle
Rinse
with FUnsc
iwtth
methanol methanol
PX) P»)
Rinse wtth Rinse wtth
methylene methylene
chloride chloride
P
x) P
x)
Weigh
Implnger
Discard
elllcagtri
PR
CR
SM
IR
Figure 5-11. PAH Field Recovery Scheme
-------
Table 5-5
Polynuclear Aromatic Hydrocarbon Sample Components
Shipped to Analytical Laboratory
IBiimliBsiptriii
i
2
3
4
5
F
PR
CR
IR
SM
Filter(s)
Rinses3 of nozzle, probe, and front
of filter holder
Rinses* of back half of filter holder
filter support, and condenser
half
*
First, second, third, and fourth
impinger contents and rinses*
XAD-2 resin
aRinses include acetone and methylene chloride recovered into the same sample bottle.
JBS336
5-54
-------
Table 5-6
Polynuclear Aromatic Hydrocarbon Compounds To Be Analyzed
Naphthalene
Acenapthylene
Acenapthene
Fluorene
Phenathrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(a)pyrene
2-Methylnapthalene
2-Chloronapthalene
Benzo(k)fluoranthene
Benzo(e)pyrene
Perylene
Indeno(l,2,3-cd)pyrene
Dibenz(a,h)anthracene
Dibenzofuran
7, i2-Dimethyibenz(a)anthracenc
Benzo(g,h,i)perylene
JBS336
5-55
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5.7.5.2 Calibration of GC/MS System. An initial calibration of the GC/MS
system was performed to demonstrate instrument linearity over the concentration range
of interest. Analyses for PAH was performed using low resolution mass spectrometry. A
typical calibration range consisted of points at 4:100, 40:100, and 400:100 for the ratio of
analytes to isotopically labeled internal standards. Relative response factors were
calculated for each compound of interest. The response factors were verified on a daily
basis using a continuing calibration standard consisting of mid-level standard (typically
the 40:100 standard).
5,7.5.3 Sample Extraction. For PAH analyses, isotopically labeled surrogate
compounds were added to the samples before the extraction process was initiated.
These surrogates were used to monitor the efficiency of the extraction/clean-up. The
internal standards used in the quantitative analysis of these analytes were added to the
samples immediately prior to analysis, and used to perform the quantitative calculations.
5.7.5.4 Analysis by GC/MS. The PAH analyses were performed by
high-resolution GC followed by low resolution mass spectrometry.
Data from the MS were recorded and stored on a computer file as well as printed
on paper. A duplicate analysis was performed on every tenth sample in the sample
batch. A method blank which was carried through the complete extraction procedure
was also analyzed. Results such as amount detected, detection limit, retention time, and
internal standard and surrogate standard recoveries were calculated by computer. The
chromatograms were retained by the analytical laboratory and also included in the
analytical report.
5.7.6 Analytical QA/QC Procedures
This section discusses the general quality control procedures that were followed
for the analytical methods. Method-specific analytical QA/QC procedures are also
presented,
5,7.6.1 Quality Control. This section presents the PAH quality control
requirements.
Blanks. Two different blanks were collected for the PAH analyses: a laboratory
proof blank and a field blank. Proof blanks were obtained from a complete set of
JBS336 5-56
-------
Modified Method 5 sample train glassware that had been cleaned according to the
procedure presented in Section 5.1,2. The precleaned glassware, which consisted of a
probe liner, filter holder, condenser coil, and impinger set, was loaded and then
recovered by rinsing with acetone and methylene chloride three times each. All sets of
glassware were blanked.
A field blank was collected from a set of PAH glassware that was used to collect
at least one sample and had been recovered. The train was reloaded and left at the
sampling location during a test run. The train was then recovered. The field blank was
used to measure the level of contamination that occurred from handling, loading,
recovering, and transporting the sample train. The field blank was analyzed concurrently
with the flue gas samples. If the field blank results were acceptable, the laboratory proof
blank and reagent blanks were archived but not analyzed.
Analytical method (reagent) blanks were also analyzed as part of the QC
program. The QC criteria for method blanks was concentrations less than or equal to
the detection limit (in the noise range).
Standards Duplicates. Isotopically labelled internal standards and surrogate
compounds were added to the sample before the extraction process began. Once added
to the samples, the internal standards went through the entire extraction process and
were measured on the GC/MS. The recoveries of the internal standards were
determined and the results of the native species were adjusted according to the internal
standard recoveries. The results contained in the analytical report were adjusted for
internal standard recoveries. The surrogate compounds were added in a similar manner,
but the surrogate recoveries were not used to adjust the results of the native species.
Surrogate recoveries provided additional data on the efficiency of the extraction
procedure and the performance of the instruments. The QC objective for internal
standards and surrogate recoveries was 100 .±.50% recovery.
JBS336
5-57
-------
The purpose of duplicate analyses was to evaluate the reproductibility (precision)
of the combined sample preparation and analytical methodology. The QC criterion for
analysis of duplicates was agreement to within .+.50% (for each PAH species). Analytical
duplicates (two injections of the same sample) were also analyzed to assess the precision
of the analytical methodology. For PAH flue gas samples, only analytical duplicates
were performed. For every 10 samples, one duplicate analysis was performed.
5.8 ASTM METHODS
Standard ASTM methods were used to assess heat of combustion, ultimate
analysis (ash, O2, carbon, hydrogen, sulfur, and nitrogen), and chlorine content of the
waste oil fuel. Aggregate moisture and ambient humidity were also analyzed.
Descriptions of applicable ASTM methods follow.
5.8.1 Relative Humidity
Sampling for relative humidity was performed using ASTM Method E337-62,
"Standard Test Method for Relative Humidity by Wet- and Dry-Bulb Psychrometer."
This method covers the determination of the relative humidity of atmospheric air by
means of wet- and dry-bulb temperature readings.
5.8.1.1 Sampling Equipment and Method. A sling psychrometer was used for
measuring relative humidity. Two thermometers, one with a wet-bulb covering were
mounted on the psychrometer. The wet-bulb covering was moistened and the
psychrometer slung through the air for several minutes. The thermometers were read
and the psychrometric chart was used to calculate the relative humidity.
5.8.2 Heat of Combustion Test Method
Heat of combustion of the fuel sample was determined according to ASTM
Method D240-87, "Standard Test Method for Heat of Combustion of Liquid
Hydrocarbon Fuels by Bomb Calorimeter." This test method covered the determination
of the heat of combustion of liquid hydrocarbon fuels ranging in volatility from that of
light distillates to that of residual fuels.
5.8.2.1 Sampling Equipment and Method. Heat of combustion was determined
using an O2 bomb, calorimeter, stirred water jacket, and a thermometer. A weighed
sample was burned in an O2 bomb calorimeter under controlled conditions. The heat of
JBS336 5-58
-------
combustion was computed from temperature observations before, during, and after
combustion with proper allowance for thermochemical and heat transfer corrections.
Adiabatic calorimeter jackets were used.
5.8.3 Total Moisture Content Test Method
Total moisture content of the aggregate sample was determined according to
ASTM Method C566-89, "Standard Test Method for Total Moisture Content of
Aggregate by Drying." This test method covered the determination of the percentage of
evaporative moisture in a sample. The plant routinely performed this test at least
several times per day. This information was provided by the plant personnel and is
included in the process data section of the test report.
5.8.3.1 Sampling. Equipment and Method. Total moisture content was
determined using a balance or scale accurately readable and sensitive to within
0.1 percent of the test load, a source of heat such as a ventilated oven capable of
maintaining the temperature surrounding the sample at 110 ±5°C (230 ±9°F); and a
sample container not affected by the heat and of sufficient volume to contain the sample
without danger of spilling.
The sample was weighed to the nearest 0.1 percent and then dried in the sample
container. The temperature was controlled when excessive heat may alter the character
of the aggregate or where more precise measurement was needed, The dried sample
was weighed to the nearest 0.1 percent after it had cooled sufficiently to prevent damage
to the balance. Total moisture was calculated using the formulas presented in
Section 7.1 of the reference method.
5-8.4 Sulfur Test Method
Sulfur concentrations in the sample were determined according to ASTM
Method D1552-90, "Standard Test Method for Sulfur in Petroleum Products (High
Temperature Method)," This test method covered the procedures for the determination
of total sulfur in petroleum products including lubricating oils containing additives and in
additive concentrates.
5,8.4.1 Sampling Equipment and Method. Sulfur content of a sample was
determined using a furnace, an absorber, a buret, and other miscellaneous apparatus.
JBS336 5-59
-------
The IR detection system was used for the determination of sulfur. The sample was
weighed into a special ceramic boat which was then placed into a combustion furnace in
an O2 atmosphere. Any sulfur was combusted to SO2 which was then measured with an
IR detector after moisture and dust were removed by traps. A microprocessor calculated
the mass percent sulfur from the sample weight, the integrated detector signal and a
predetermined calibration factor. Both the sample identification number and mass
percent sulfur were then printed out. The calibration factor was determined using
standards approximating the material to be analyzed.
5.8.5 Nitrogen Test Method
Nitrogen concentration in the sample was determined according to ASTM
Method D3179-84, "Standard Test Methods for Nitrogen in the Analysis of Coal and
Coke." This test method covered the determination of total nitrogen in samples of coal
and coke.
5.8.5.1 Sampling Equipment and Method. Total nitrogen was determined using a
digestion unit, digestion flasks, distillate unit, buret, Erlenmeyer flasks, rubber tubing,
and pipets. Reagents included an alkali solution, ethyl alcohol, and sulfuric acid.
Nitrogen in the sample was converted into ammonium salts by destructive digestion of
the sample with a hot, catalyzed mixture of concentrated sulfuric acid and potassium
sulfate. These salts were subsequently decomposed in a hot alkaline solution from which
the ammonia was recovered by distillation and finally determined by alkalimetric or
acidimetric titration.
5.8.6 Carbon and Hydrogen Test Method
Carbon and hydrogen concentrations in the sample were determined according to
ASTM Method D3178-84, "Standard Test Method for Carbon and Hydrogen in the
Analysis Sample of Coal and Coke."
5.8.6.1 Sampling Equipment and Method. Carbon and hydrogen content were
determined using an O2 purifying train that consisted of two water absorbers and a CO2
absorber, a flow meter, a combustion unit, and reagents. A quantity of the sample was
burned in a closed system. The products of combustion were fixed in an absorption train
after complete oxidation and purification from interfering substances. This test method
JBS336 5-60
-------
gave the total percentages of carbon and hydrogen and included the carbon in
carbonates and the hydrogen in the moisture and in the water of hydration of silicates.
JBS336
5-61
-------
6. QUALITY ASSURANCE AND QUALITY CONTROL
To ensure the production of useful and valid data, specific QA/QC procedures
were strictly adhered to during this test program. A detailed presentation of QC
procedures for all manual flue gas sampling, process sample collection, GC operations,
and CEM operations can be found in the Mathy Test Plan. This section will report the
test program QA parameters so that the degree of data quality can be shown.
Two days of testing were conducted at Mathy Construction Company, Plant 6.
Three runs were completed successfully at near-design operating conditions while the
plant was operating on natural gas. No sampling related problems were encountered
during testing that would affect data quality.
In summary, a high degree of data quality was maintained throughout the project.
Post-test leak checks for all sampling trains were within acceptable limits and all
post-test calibration checks for the dry gas meters were within acceptable limits. All
PM/metals, aldehydes, and PAH manual sampling trains met the isokinetic criterion of -
± 10 percent out of 100 percent, and the PM10/CPM manual sampling trains met the
isokinetic criterion of ±20 percent out of 100 percent, which is acceptable for this test
method.
Method blank and field blank results for the manual sampling trains showed some
contamination. Also, several method spike recovery values for the metals, aldehydes,
and PAH analyses were not within the QA allowance. Method blank, field blank, and
method spike results are further discussed in Section 6.2.
The CEM results showed acceptable calibration drift values and QC gas
responses. All CEM QC procedures and objectives were followed as described in the
Mathy Test Plan.
The GC used for EPA Method 18 analysis was calibrated each test day before
and after flue gas sampling. Quality assurance/quality control results showed allowable
response factor drift values for the calibration gases.
Section 6.1 presents the QA/QC definitions and data quality objectives.
Section 6.2 presents manual flue gas sampling and recovery parameters and Section 6.3
JBS336 6-1
-------
presents method-specific analytical QA parameters. Section 6.4 discusses the CEM QA
parameters and Section 6.5 presents the GC QA parameters.
6.1 QUALITY ASSURANCE/QUALITY CONTROL DEFINITIONS AND
OBJECTIVES
The overall QA/QC objective is to ensure precision, accuracy, completeness,
comparability, and representativeness for each major measurement parameter called for
in this test program. For this test program, quality control and quality assurance can be
defined as follows:
• Quajity. .Control: The overall system of activities whose purpose is to
provide a quality product or service. QC procedures are routinely followed
to ensure high data quality.
» Quality Assurance: A system of activities whose purpose is to provide
assurance that the overall quality control is being done effectively.
Assessments can be made from QA parameters on what degree of data
quality was achieved.
• Data Quality: The characteristics of a product (measurement data) that
bear on its ability to satisfy a given purpose. These characteristics are
defined as follows:
Precision - A measure of mutual agreement among individual
measurements of the same property, usually under prescribed
similar conditions. Precision is best expressed in terms of the
standard deviation and in this report will be expressed as the
relative standard deviation or coefficient of variation.
Accuracy - The degree of agreement of a measurement (or an
average of measurements of the same thing), X, with an accepted
reference or true value, T, can be expressed as the difference
between two values, X-T, the ratio X/T, or the difference as a
percentage of the reference or true value, 100 (X-T)/T.
Completeness - A measure of the amount of valid data obtained
from a measurement system compared with the amount that was
expected to be obtained under prescribed test conditions.
* •
Comparability - A measure of the confidence with which one data
set can be compared with another.
JBS336
-------
Representativeness - The degree to which data accurately and
precisely represent a characteristic of a population, variations of a
parameter at a sampling point, or an environmental condition,
A summary of the estimated precision, accuracy, and completeness objectives is
presented in Table 6-1.
6.2 MANUAL FLUE GAS SAMPLING QUALITY ASSURANCE
The following section will report manual sampling QA parameters so that insight
can be gained into the quality of the emissions test data produced from manual tests
during the test program.
6.2.1 Particulate Matter/Metals Sampling Quality Assurance
Table 6-2 presents post-test leak check results for all of the manual sample trains.
The acceptance criterion is that all post-test leak checks must be less than 0.02 cfm. All
PM/metals post-test leak checks met the acceptance criterion and, therefore, no leak
corrections were applied.
The isokinetic sampling rates for all of the manual sampling runs are presented in
Table 6-3. The acceptance criterion for the PM/metals, aldehydes, and PAH sampling
runs is that the average sampling rate must be within 10 percent of 100 percent
isokinetic. Acceptance criterion for the PMto runs allows sampling rates to be within
20 percent of 100 percent isokinetic. All FM/metals runs deviated by no more than
4 percent of 100 percent, thereby meeting the isokinetic criterion.
All dry gas meters used for manual sampling were fully calibrated within the last
six months against an EPA approved intermediate standard. The full calibration factor
or meter Y was used to correct actual metered volume to true sample volume. To verify
the full calibration, a post-test calibration was performed. The full and post-test
calibration coefficients must be within five percent to meet Radian's internal QA/QC
acceptance criterion. The results of the full and post-test calibration check of the meter
boxes used for manual sampling are presented in Table 6-4. The post-test calibration
factor for the meter box used for PM/metals test runs was within the five percent
criterion of the full calibration factor.
JBS336
6-3
-------
Table 6-1
Summary of Precision, Accuracy, and Completeness Objectives"
Parameter
Flue Gas Formaldehyde
Flue Gas Metals
Polynuclear Aromatic Hydrocarbons
Flue Gas Total Particulate Matter
Continuous Monitoring System
Velocity/Volumetric Flow Rate
Fixed Gases/Molecular Weight
Moisture
Flue Gas Temperature
Precision"
• (%)
±15
±15d
±15
±11
±2e
±6
±03%V
±20
±2°F
Accuracy8
(%)
±20
±30C
±20
±10
±2d
±10
±0.5%V
±10
±5°F
Completeness6
(%)
100
100
100
100
95
95
100
95
100
"Precision and accuracy estimated based on results of EPA collaborative tests. All values
stated represent worst case values. All values are absolute percentages unless otherwise
stated.
bMinimum valid data as a percentage of total tests conducted.
""Relative error (%) derived from audit analyses, where:
Percent Error =
Measured Value - Theoretical Value
Theoretical Value
x 100
dPercent difference for duplicate anlayses, where;
„ _..„ First Value - Second Value 1A_
Percent Difference = x 100
0-5 (First + Second Values)
'Minimum requirements of EPA method 6C, based on percent of full scale.
JBS336
-------
Table 6-2
LEAK CHECK RESULTS FOR MANUAL SAMPLE TRAINS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
PM/Metals
PM/Metals
PM/Metals
PM10/CPM
PM10/CPM
PM10/CPM
Aldehydes
Aldehydes
Aldehydes
PAH
PAH
PAH
09/19/91
09/19/91
09/20/91
09/19/91
09/20/91
09/20/91
09/19/91
09/20/91
09/20/91
09/19/91
09/19/91
09/20/91
1
2
3
1
2
3
1
2
3
1
2
3
2
2
2
NA
NA
NA
3
2.5
4
7
7
8
0.50
0.48
0.47
0.78
0.79
0.74
0.49
0.46
0.48
0.51
0.49
0.47
0.010
0.008
0.014
0.003
0.003
0.004
0.014
0.004
0.005
0.012
0.012
0.006
10
3.5
8
3
3
3
10
8
10
10
11
11
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
NA = Not Available
-------
Table 6-3
ISOKINETIC SAMPLING RATES FOR MANUAL SAMPLING TEST RUN
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
PM/Metals
PM/Metals
PM/Metals
PM10/CPM
PM10/CPM
PM10/CPM
Aldehydes
Aldehydes
Aldehydes
PAH
PAH
PAH
09/19/91
09/19/91
09/20/91
09/19/91
09/20/91
09/20/91
09/19/91
09/20/91
09/20/91
09/19/91
09/19/91
09/20/91
1
2
3
1
2
3
1
2
3
1
2
3
104
104
104
87.0
89.5
80.4
105
101
102
107
106
105
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
PM/Metals, Aldehydes and PAH test metals specify isokineuc sampling
rates must be within 10 percent of TOO percent isokinelic. The PM10
Lest method allows isokinelic sampling rales 10 be within 20 percent
of 100 percent isoldnetic
6-6
-------
Table 6-4
DRY GAS METER POST-TEST CALIBRATION RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
N-30
N-32
N-33
PAH
Aldehydes
PM/Metals -
PM10/CPM
1.0006
0.9875
1.0218
1.0051
0.9788
2.20
0.45
-0.88
yes
yes
yes
* = ((Post-Tesl)-(FuH)]/(FuIl)*100
-------
6.2.2 PM10/CPM Sampling Quality Assurance
Post-test leak checks, isokinetic rates, and dry gas meter post-test calibrations for
the PM10/CPM test runs were with QA allowances and are presented in Tables 6-2
through 6-4, respectively. Note that the isokinetic acceptance criterion for PM10/CPM
runs is more lenient than other methods allowing the average sampling rate to be within
20 percent of 100 percent isokinetic.
6.2.3 Aldehydes Sampling Quality Assurance
The post-test leak checks for the aldehydes sample trains met the QA acceptance
criterion. The isokinetic rates for the aldehydes test runs deviated by no more than
5 percent of 100 percent, meeting the QA acceptance criterion. The post-test calibration
factor for the meter box used for aldehydes'.jest runs was within the 5 percent criterion
of the full calibration factor. Post-test leak check results, isokinetic values, and dry gas
meter calibration results for the aldehydes runs are presented in Tables 6-2 through 6-4,
respectively.
6.2.4 Pojynuclear Aromatic Hydrocarbon Sampling Quality Assurance
The post-test leak check results for tb.e PAH trains are presented in Table 6-2,
and all trains met the QA acceptance criterion. Isokinetic rates, presented in Table 6-3,
varied no more than 7 percent of 100 percent, meeting the acceptance criterion. The
post-test calibration results of the dry gas meter used for PAH sampling are presented in
Table 6-4 and show that the calibration factor is within the QA allowance.
6.3 ANALYTICAL QUALITY ASSURANCE
The following sections briefly report QA parameters for the metals, PM10/CPM,
aldehydes, and PAH analytical results. The analytical methods used for the flue gas
samples are discussed fully in Section 5.
6.3.1 Metals Analytical Quality Assurance
Field blanks were collected for the PM/metals, PM10/CPM, aldehydes, and PAH
sampling trains. A train of each sample type was fully prepared, taken to the sample
location, leak checked, and then recovered. Table 6-5 presents the results of the metals
field blank analysis compared to the test ran results. There was a noticeable
contamination of certain metals in the field blank. The front half fraction was
JBS336 "~°
-------
Table 6-5
METALS FIELD BLANK RESULTS COMPARED TO TEST RUN RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
'-:y^:^z
*'' i j \r *'' '•>•*'•>'
^ '*te*t» '
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
*"*M*t|*;
*.*. ,**X3
atpiftte
14,1
[1.00]
9.15
(0.250]
2.93
7.75
[1.00]
1.92
58.0
45.0
(75.0]
[4.00]
7.00
[25-0]
23,8
\.;\.K«t:.
- •*#$*#£ '
'>vl^/
... .Miiift .
[1.57]
[0,418]
0.815
[0.104]
0.282
1-87
6.23
0.886
2.81
2,17
59.0
[1.67]
[0,627]
[10,4]
16.1
Vs^"';,-;1?
! - KM* ' *
1' ' **
14.1
[1.42]
10.0
[0,354]
3.21
9-62
6-23
2.81
60.8
47.2
59.0
[5.67]
7.00
[25,4]
39.9
' -S*B3
ffWP» ,
.' „ mi
(total tag)
12.1
[1.00]
7.48
[0.250J
(1.830
3.20
[1,00]
0.750
29.0
2.43
[75.0]
[4.00]
5.35
[25.0]
15.4
""5.^. O , 3 "> O O
U** ,. •? J^ *>>«?<: •*
' ft&ffi
'fat.
- ftotola^
12,1
[1-00]
9.50
[0.250]
1.43
3.38
[1.00]
6,35
41.5
3.50
[75.0]
[4.00]
[1.50]
[25,0]
35.0
-^Vxipipj.^,.,,
' iq$Bi$^
! i*>
^fa^wit
[158]
[0.421]
1,42
[0.105]
0.700
L28
5.92
1.66
3,34
1.72
73.3
[1,68]
[0.631]
[10.5]
13.4
S , .,r
" f<^* j
, -"** :^'
12.1
[1,42]
10.9
(0.355]
2.13
4.66
5,92
8.01
44.8
5.22
73.3
[5.68]
[2.13]
[35.5]
48.4
•L .?.. .:, ,'....!..
ftWjt/'v.
•v-air-xj
vf o ,..>
'f^lV
', :*« >,'
13.6
[1.44]
5.81
[0.361]
1.58
4.59
[L44]
2.11
6,18
4.26
77.5
[5.78]
4.75
[36.1]
23.8
s
NOTE: Run 2impinger sample bollle broke during shipmenl Therefore, only Ilie frcni
half is recorded. The average is based on Runs I and 3.
[ ] = Minimum Detection Limit
-------
contaminated with Sb, Ba, Cd, Cr, Pb, Mn, Ni, Ag, and Zn. The back half fraction was
contaminated with Ba, Cr, Pb, Mn, Ni, phosphorus (P), and Zn. The appropriate blank
corrections were applied to the metals where contamination was found in the field blank.
This resulted in 9 of the 15 metals exhibiting significant amounts detected in the flue gas
samples. These metals are Ba, Cd, Cr, Cu, Pg, Mn, Ni, Ag, and Zn. Table 6-6 presents
the metals method blank results for the flue gas samples. Lead, Mn and Ni were
detected in the flue gas method blank at low levels. These amounts were negligible in
comparison to the amounts found in the field blanks and, therefore, no blank corrections
were applied based on these results.
Table 6-7 presents the method spike results for the metals analysis. All spiked
recoveries for the front half fraction (except for Ag) were within the QA allowance of
±20 percent of 100 percent. Barium, Cu, and P were slightly below the 20 percent
acceptance in the back half fraction, with 78.4 percent, 79.3 percent, and 78,2 percent,
respectively. No spike corrections were applied.
6.3.2 PM10/CPM Analytical Assurance
Table 6-8 presents the results of the PM10/CPM field blank analysis compared to
the test run results. Methylene chloride and acetone were detected in the field blank
and were 0.8 percent and 3.1 percent, respectively, of the average run amount. The
PM10/CPM samples were gravimetrically analyzed according to EPA Method 5
requirements. Sample jars were checked to determine if leakage occurred during
shipment. The residue for the cyclone catch, filter catch, organic fraction, and inorganic
fraction were weighed to within 0.5 ing. The weight determinations were conducted at
least six hours apart. Weight gain for each fraction was reported to the nearest 0.1 mg.
Water and methylene chloride blanks were analyzed with the samples. Blank correction
was not required because the sum of the values for the water blank and the methylene
chloride blank was less than 2 mg.
6.3.3 Aldehydes Analytical Quality Assurance
Aldehydes field blank results are compared to the test run results in Table 6-9.
Acetone was detected in the field blank at a noticeable level and formaldehyde was
detected at a low level. The aldehydes method blank results for the flue gas samples are
JBS336 6-10
-------
Table 6-6
METALS AMOUNT IN FLUE GAS METHOD BLANK RESULT
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorous
Selenium
Silver
Thallium
Zinc
[1.50]
[0.400]
[0.100]
[0.100]
[0.200]
[0.600]
[0.400]
[0.300]
(0.330)
[0.300]
[30.0]
[1.60]
[0.600]
[10.0]
(2.41)
[1.59]
[0.424]
[0.106]
[0.106]
[0.212]
[0.636]
[0.424]
(0.744)
2.37
(0.572)
[31.8]
[1.70]
[0.636]
[10.6]
[1.59]
[ J = Minimum Detection Limit.
( ) = Estimated Vahie
6-11
-------
Table 6-7
METALS METHOD SPIKE RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorous
Selenium
Silver
Thallium
Zinc
100%
87.4%
91.4%
95.0%
100%
99.6%
93-5%
97.8%
96.1%
99.9%
89-2%
99.0%
74.5%
103%
103%
86.8%
86.0%
88.2%
83.4%
98.5%
97.0%
90.1%
88.6%
94,0%
88.1%
78.2%
85.3%
41.0%
94,7%
90.7%
100%
95.4%
91.0%
95.2%
99.9%
99.4%
93.9%
102%
96.2%
100%
92.1%
99.6%
24.7%
100%
104%
96.8%
97.8%
78.4%
93.4%
88.5%
86.5%
79.3%
98.8%
84.9%
98.5%
86.5%
95.8%
30.4%
97-5%
101%
6-12
-------
Table 6-8
PM10/CPM FIELD BLANK RESULTS COMPARED
TO TEST RUN RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
H20
MeCl
Acetone
41.7
5.03
26.1
0.000 b
0.040
0.800
a = Runs 1,2,3
b = Showed a slightly negative weight gain, assumed to be zero
6-13
-------
TABLE 6-9
ALDEHYDES FIELD BLANK RESULTS COMPARED TO TEST RUN RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Acetaldehyde
Acetone
Acetophenone/o-Tolualdehyde
Acrolein
Benzaldehyde
Butyraldehyde/Isobutyraldehyde
Crotonaldehyde
2,5-Dimethylbenzaldehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehyde
MffiK/p-Tolualdehyde
Methyl Ethyl Ketone
Propionaldehyde
Quinone
m-Tolualdehyde
Valeraldehyde
822
23700
[23-0]
[13.0]
199
47.0
37.1
[24.0]
2950
40.7
[18.0]
[18.0]
[23.0]
[18.0]
[14.0]
48.8
[23.0]
[18.0]
1040
11200
[23.0]
[13.0]
198
[18.0]
29.5
[24.0]
4470
62.5
[18.0]
[18.0]
[23.0]
[18.0]
[14.0]
27.0
[23.0]
[18.0]
1170
2570
[23.0]
26.7
211
75.4
65.0
[24.0]
2770
20.0
[18.0]
[18.0]
[23.0]
93.5
94.6
1040
[23.0]
56.9
[5.80]
6640
[12.0]
[7.10]
[11.0]
[9.40]
[9,40]
[13.0]
10.7
[11.0]
[9.40]
[9.80]
[12.0]
[9,40]
[7.30]
[9.40]
[12.0]
[9.80]
[ ] = Minimum Detection Limit
6-14
-------
presented in Table 6-10. Acetaldehyde, acetone, formaldehyde, and isovaleraldehyde
were detected in the flue gas method blank at low levels. However, no corrections were
made to the flue gas samples based on these results,
Table 6-11 presents the method spike results for the aldehyde analysis. All spike
recoveries, except for acetophenone/o-tolualdehyde at 70 percent recovery, acrolein at
23 percent recovery, crotonaldehyde at 25 percent recovery, and quinone at 64 percent,
are within the QA ±20 percent of the 100 percent. No spike corrections were applied.
6.3.4 Polvnuclear Aromatic Hydrocarbon Results
Table 6-12 presents the PAH field blank results compared to the test run results.
Naphthalene was detected in the field blank at a noticeable level, while
methylnaphthalene and phenanthrene were detected at low levels. Blank corrections
were applied based on these results. The PAH method blank results for the flue gas
samples are presented in Table 6-13. Fluorene, 2-methylnaphthalene, naphthalene, and
pyrene were detected in the flue gas method blank at low levels. No method blank
corrections were applied.
Table 6-14 presents the method spike results for the PAH analysis. All spike
recoveries, except for nitrophenol, pentachlorophenol, and di-n-butylphthalate, are within
the QA ±20 percent of the 100 percent. No spike corrections were applied. Table 6-15
presents the PAH surrogate recovery results. 2-fluorobiphenyl was out of the lab control
limits, but nitrobenzene-d5 and terphenyl-d!4 were within control limits for all sample
runs.
6.4 CONTINUOUS EMISSION MONITORING QUALITY ASSURANCES
Flue gas was analyzed continuously for O2/C02, CO, SO2, NOX, and THC using
EPA Reference Methods 3A, 10, 6C, 7E, and 25A, respectively. Daily QA/QC
procedures were performed in accordance with QA/QC guidelines in the reference
methods and Radian standard operating procedures. These procedures are fully detailed
JBS336
6-15
-------
Table 6-10
ALDEHYDES FLUE GAS METHOD BLANK RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Acetaldehyde
Acetone
Aceiophenone/o-Tolualdehyde
Acrolein
Benzaldehyde
Butyraldehyde/Isobutyraldehyde
Crotonaldehyde
2,5-Dimethylbenzaldehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehydc
MIBK/p-Tolualdehyde
Methyl Ethyl Ketone
Propionaldehyde
Quinone
m-Tolualdehyde
Valeraldehyde
0,660
1.74
[1.20]
[0.710]
[1.10]
[0.940]
[0.940]
[1.30]
1,06
[1.10]
[0.940]
3.68
[1.20]
[0.940]
[0.730]
[0.940]
[1.20]
[0.980]
[5.80]
6640
[12.0]
[7.10]
[11.0]
[9.40]
[9.40]
[13,0]
10.7
[11.0]
[9.40]
[9.80]
[12.0]
[9.40]
[7.30]
(9.40]
[12.0]
[9.80]
[ ] = Minimum Detection Limit.
6-16
-------
Table 6-11
ALDEHYDES METHOD SPIKE RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Acetaldehyde
Acetone
Acetophenone/o-Tolualdehyde
Acrolein
Benzaldehyde
Butyraldehyde/Isobutyraldehyde
Crotonaldehyde
2,5-Dimethylbenzaldehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehyde
MIBK/p-Tolualdehyde
Methyl Ethyl Ketone
Propionaldehyde
Quinone
m-Tolualdehyde
Valeraldehyde
90.0%
83.0%
70.0%
23.0%
119%
NA
25.0%
85.0%
87.0%
117%
91.0%
NS
106%
NA
107%
64.0%
93.0%
82.0%
NA = Not Analyzed
NS = Not Spiked
6-17
-------
TABLE 6-12
PAH FIELD BLANK RESULTS COMPARED TO TEST RUN RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Aeenaphthylene
Acenoaphihene
Anthracene
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
2-Chloronapthalene
Chrysene
Dibenz(a,h) anthracene
Dibenzofuran
7,12-DimethyIbenz(a)anthracene
Fluoranthene
Fluorene
Indeno(l,2,3-cd)pyrene
2-Methylnaph thalene
Naphthalene
Perylene
Phenanthrene
Pyrene
(41.8)
(14.9)
(10.2)
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[100]
[50.0]
[50.0]
[50.0]
408
416
[50.0]
(9.04)
(1.26)
(37.7)
[50.0]
(8.99)
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[100]
[50.0]
[50.0]
[50.0]
348
776
[50.0]
(7.94)
(0.625)
(48.1)
[50.0]
(9.62)
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[100]
[50.0]
[50.0]
[50.0]
417
1470
[50.0]
(8.49)
(0.805)
[50.0]
[50.0]
[50.0]
[50-0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[100]
[50.0]
[50.0]
[50.0]
(2.36)
751
[50.0]
(0.275)
[50.0]
[ ] = Minimum Detection Limit
( ) = Estimated Value
6-18
-------
Table 6-13
PAH FLUE GAS METHOD BLANK RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Acenaphthylene
Acenaphthene
Anthracene
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
2-Chloronapthalene
Chrysene
Dibenz(a, h )an thracene
Dibenzofuran
7,12-Dimethylbenz(a)anthracene
Fluoranthene
Fuorene
lndeno(l,2,3-cd)pyrene
2-Methylnaphthalene
Naphthalene
Perylene
Phenanthrene
Pyrene
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[50.0]
[100]
[50.0]
(0.375)
[50.0]
(0,680)
260
[50.0]
[50.0]
(0.805)
[ | = Minimum Detection Limit.
( ) = Estimated Value
6-19
-------
Table 6-14
PAH METHOD SPIKE RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
Phenol
2-Chlorophenol
1,4-Dichlorobenzene
N-Nitroso-di-n-propylamine
1,2,4-Trichlorobenzene
4-Chloro-3-methylphenol
4-Nitrophenol
2,4-Dinitrotoluene
Pentachlorophenol
Di-n-butlyphthalate
84.8%
94.2%
95.6%
104%
109%
99.9%
53.0%
94.6%
26.6%
2.15%
6-20
-------
Table 6-15
PAH SURROGATE RECOVERY RESULTS
MATHY CONSTRUCTION COMPANY PLANT 6 (1991)
v
2-Fluorobiphenyl
Nitrobenzene-d5
Terphenyl-dl4
146%
113%
112%
124%
93.9%
111%
153%
113%
121%
141%
96.4%
112%
130%
87.4%
111%
143%
105%
127%
30% lo 11.5%
23% to 120%
18% to 137%
-------
in the site-specific test plan prepared by Radian Corporation.1 A summary of the
QA/QC parameters and results is provided in this section. Deviations from the test plan
and/or problems encountered during the test program are also discussed,
6.4.1 Calibration and Drift Assessments
Continuous monitoring instruments were calibrated at the beginning of the test
period on a two-point basis using a zero gas (N2) and a high-range span gas, A
mid-range gas was analyzed with no adjustment permitted as a QC check at least once
on site. The observed mid-range QC gas concentration was within ±2 percent of full
scale for the linearity check to be considered acceptable. The results of this check are
presented in Tables 6-16 through 6-21.
In addition to conducting the linearity check, the instrument drift was also
determined for each analyzer on a daily basis. Typically, the mid-range gas was analyzed
at mid-day and/or at the end of each test day to determine an "inter-run" drift; however,
the span gas was used in some cases to conserve gases that were available in more
limited quantities. A drift check was not determined between every manual run to allow
completion of as many manual method tests as possible while the batch operated plant
was actually on-line. The inter-run instrument drift value was calculated as a difference
on a percent scale basis by comparing the current observed response to the previous
response. The instrument drift over the entire test program was calculated similarly,
except that the final mid-gas observed response was compared to the initial mid-gas
observed response. These inter-run and overall drift values are also provided in
Tables 6-16 through 6-21. The allowable drift of ±3 percent of full scale which was met
in all cases except for one inter-run check of the NOX analyzer; however, the overall drift
for this analyzer over the entire test period was determined as 0,6 percent, which is
within ±3 percent limit.
lnEmission Testing for Asphalt Concrete Industry, Site-Specific Test Plan and Quality
Assurance Project Plan, Mathy Construction Company Plant #6," Radian Corporation,
September 1991.
JBS336 6-22
-------
Table 6-16
Method 3A Oxygen Analyzer and Drift Summary
Mathy Construction Company-Plant 6
Multipoint linearity*
9/19/91
08:34
Zero:
0.0
0.0
0.0
0.0
9/19/91
08:35
Mid;
7.99
7,7
-0.29
-1.16
9/19/91
08:34
Span:
18.0
18.0
0.0
0.0
Inter-run Drift Summary1'
9/19/91
12:55
Mid:
7.99
7.6
-0,1
-0.4
9/19/91
15:53
Mid:
7.99
7.6
0.0
0.0
9/20/91
6:51
Mid:
7.99
7.2
-0.4
-1.6
9/20/91 | 15:40
Mid:
7.99
7.4
0.2
0.8
Test Period Drift Summary*
9/20/91
15:40
Mid:
7.99
7.4
-0.3
-1.2
Difference Percent Scale = (observed cone. - certified conc.)/span value * 100%.
(current observed cone. - previous observed conc.)/span
"Difference Percent Scale
value * 100%.
Difference Percent Scale
100%.
= (final observed cone. - initial observed conc.)/span value *
JBS336
6-23
-------
Table 6-17
Method 3A Carbon Dioxide Analyzer and Drift Summary
Mathy Construction Company, Plant 6
Multipoint Linearity*
9/19/91
08:34
Zero;
0.0
0.0
0.0
0.0
9/19/91
08:35
Mid:
9.91
10.3
0.4
2.0
9/19/91
08:34
Span:
17.0
17.0
0.0
0.0
Inter-run Drift Summary11
9/19/91
12:55
Mid:
9.91
10.3
0.0
0.0
9/19/91
15:53
Mid:
9.91
10.6
0.3
1.5
9/20/91 15:40
Mid:
9.91
•10.2
-0.4
-2.0
Test Period Drift Summary6
9/20/91
15:40
Mid:
9.91
10.2
-0.1
0.5
Difference Percent Scale = (observed cone. - certified conc.)/span value * 100%.
(current observed cone. - previous observed conc.)/span
bDifference Percent Scale
value * 100%.
'Difference Percent Scale
100%.
= (final observed cone, - initial observed conc.)/span value *
JBS336
6-24
-------
Table 6-18
Method 10 Carbon Monoxide Analyzer and Drift Summary
Mathy Construction Company, Plant 6
Multipoint linearity*
9/19/91
08:34
Zero:
0.0
0.0
0.0
0.0
9/19/91
08:35
Mid:
92.1
-3.8
-0.76
9/19/91
08:34
Span:
474
474
0.0
0.0
Inter-run Drift Summary1*
9/19/91
12:55
Mid:
92.1
89.9
1.6
0.3
9/19/91
15:53
Mid:
92.1
93.7
3.8
0.8
9/20/91 06:51
Mid:
92.1
82.2
-11.5
-2.3
Test Period Drift Summary*
9/20/91
06:51
Mid:
92.1
82.2
-6.1
-1.2
Difference Percent Scale = (observed cone. - certified conc.)/span value * 100%.
(current observed cone. - previous observed cone.)/span
bDifference Percent Scale
value • 100%,
TDifference Percent Scale
100%.
= (final observed cone. - initial observed conc.)/span value
JBS336
6-25
-------
Table 6-19
Method 6C Sulfur Dioxide Analyzer and Drift Summary
Mathy Construction Company, Plant 6
Multipoint Linearity*
9/19/91
08:34
Zero:
0.0
0,0
0.0
0.0
9/20/91
06:51
Mid:
98.0
95.8
-2.2
-0.4
9/19/91 08:34
Span:
295
295
0.0
0.0
Inter-run Drift Summary**
9/19/91
12:55
Span:
295
299
0.8
9/19/91
15:53
Span:
295
300
0.2
9/20/91 12:38
Span:
295
287
-8
-1.6
Test Period Drift Summary*
9/20/91
15:40
Low:
98.0
97.7
1.9
0.4
aDifference Percent Scale = (observed cone, - certified conc.)/span value * 100%.
(current observed cone. - previous observed conc.)/span
bDifference Percent Scale
value * 100%.
^Difference Percent Scale
100%.
= (final observed cone, - initial observed conc.)/span value *
JBS336
6-26
-------
Table 6-20
Method 7E Nitrogen Oxides Analyzer and Drift Summary
Mathy Construction Company, Plant 6
Multipoint Linearity*
9/19/91
08:34
Zero:
0.0
0.0
0.0
0.0
9/20/91
06:51
Low:
44.0
44.0
0.0
0.0
9/19/91 08:34
Span:
201
201
0.0
0.0
Inter-run Drift Summary1'
9/19/91
12:55
Span:
201
202
0.4
9/19/91
15:53
Span:
201
206
1.6
9/20/91
06:48
Span:
201
201
-5
-2.0
9/20/91
12:38
Span:
201
212
11
4.4
Test Period Drift Summary*
9/20/91
15:40
Low:
44.0
45.5
1.5
0.6
Difference Percent Scale = (observed cone. - certified conc.)/span value * 100%.
(current observed cone. - previous observed conc,)/span
bDifference Percent Scale
value • 100%.
Difference Percent Scale
100%.
= (final observed cone. - initial observed conc.)/span value *
JBS336
6-27
-------
Table 6-21
Method 25A Total Hydrocarbon Analyzer and Drift Summary
Mathy Construction Company, Plant 6
Multipoint linearity*
9/19/91
08:34
Zero:
0.0
0.0
0.0
0.0
9/20/91
06:51
Low:
10.1
9.9
-0.2
-0.2
9/19/91 08:34
Span:
41.4
41.4
0.0
0.0
Inter-run Drift Summary11
9/19/91
12:55
Span:
41.4
40.6
-0.8
-0.8
9/19/91
15:53
Span:
41.4
41.2
0.6
0.6
9/20/91
06:48
Span:
41.4
41.4
0.2
0.2
9/20/91
12:38
Span:
41.4
41.6
-0.2
-0.2
9/20/91 15:02
Span:
41.4
41.3
-0.3
-0.3
Test Period Drift Summary'
9/20/91
15:02
Low:
10.1
9.4
-0.5
-0.5
Difference Percent Scale = (observed cone. - certified conc,)/span value * 100%.
(current observed cone. - previous observed conc.)/span
bDifference Percent Scale
value * 100%.
^Difference Percent Scale
100%.
= (final observed cone. - initial observed conc.)/span value •
JBS336
6-28
-------
6.4.2 Line Bias Checks
Radian performed all multi-point and OC calibrations through the entire sampling
system. A three-way valve was located between the reference method CEM probe and
the heat-traced line. This valve was shut during calibration and QC drift checks, and the
standard gases were directed from the gas cylinder through the heat-traced line to the
analyzer probe and back before the gas was directed to the CEM analyzers. This
procedure eliminated the need for performing line bias checks described in Methods 3A,
7E, and the test plan.
6.4.3 Leak Checks
Since Radian performed all calibrations through the entire sampling system, leak
checks were incorporated in each calibration. The criterion used for this test was an O2
response to a zero gas of less than 0.5 percent O2. All leak checks performed at this test
site met this criterion.
6.5 GAS CHROMATOGRAPHY QUALITY ASSURANCE
EPA Method 18 analysis of the flue gas was performed using a GC to separate
the hydrocarbon (Cj-Cg) species in the gas stream. At the beginning of each test day
prior to sampling the flue gas, the GC was calibrated with standard gas mixtures
containing each hydrocarbon (methane, ethane, propane, butane, pentane, hexane) and
an instrument response factor for each hydrocarbon was determined. Response factors
for each hydrocarbon were determined again at the end of each test day after sampling
was completed. In this way, a daily calibration drift was determined for these
compounds. Additional calibrations were completed for benzene, toluene, and xylene
(BTX). Only a single calibration was completed daily for BTX compounds. The
calibration drift values are shown in Table 6-22. The drift values for Cj through C6 were
determined to be less than 7 percent, which is within the QA allowance criterion of
10 percent. Based on these low drift values, the BTX drift values would not be expected
to higher than the 10 percent criterion.
JBS336 6-29
-------
Table 6-22
GC Response Factor Drift Values
Mathjr Construction Company-Plant 6
(1991)
Methane
2.823 x
2.788 x 10'5
-1,26
3.0855 x 10"5
3.3123 x NT5
6.85
Ethane
1.371 x Iff5
1.355 x 10'5
-1.18
1.3928 x IQT5
1.4493 x 10'5
3.90
Propane
9.264 x 1CT6
9.123 x Iff6
-1.55
9,4026 x Iff*
9.7336 x Iff*
3.40
Butane
6.710 x 10"6
6.783 x
1.0
6.4131 x Iff6
6.7103 x Iff*
4.43
Peniane
5.401 x Iff6
5.414 x Iff6
0.24
5.4065 x Iff6
5.6770 x 10-6
4.76
Hexane
4.522 x KT6
ND
4.6559 x 10"6
4.8493 x Iff6
3.99
Benzene
ND
4.413 x
3.9334 x 10"6
ND
Toluene
ND
3.632 x
4.1761 x
ND
Ethylbenzene
ND
2.838 x Iff*
23932 x Iff6
ND
Xylene
ND
2,500 x
2.2779 x
ND
ND = Not Determined
"Response Factor =
Calibration Gas Concentratjon (ppm)
Peak Area Count
bDrift Percent =
(Post-Test Response Factor - Ptc-Test Response Factor)
Post-Test Response Factor
JBS336
6-30
-------
APPENDIX A
EMISSIONS TESTING FIELD DATA SHEETS
A.I PM/Metals
A.2 PM]0,CPM
A3 Aldenydes
A.4 PAH
-------
APPENDIX A.I
PM/METALS
-------
PLANT
SAMPLING LOCAMON
SAMPLE 1TPE i
RUN NUMBER
OPERATOR
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE .
STATIC PRESSURE IP I _
FILTER NUMBER Hi
PROBE LENGIH AND IYPE
NDZ/LE I.D ,J.fll
ASSUMED MOISTURE, *, _J?l
SAMPLE BOX NUMBER
METER BOX NUMflEH,
METER SHa
/I/-
PROBE HEATER SETT ING
HEAIERBOISCTIINC_
fltftHtMLl &t_ K-
«-
= Li
ICHEMAIICOF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA tVERY JLS— MINUTES
TRAVERSE
POUT
NUMBER
CAS KIER READING
|VI. II-
-1
VELOCIIY
HEAD
flPjl m. H?0
ORIFICE PRtSStlRE
DIFFERENTIAL
(AH), in, HjOl
DESIRED ACTUAL
SIACK
TEMPERATUNL
DRTCA1KTER
IEHPERATURE
INLET OUTLET
PUMP
VACULN
in. H|
SAiPLC B01
IEMPERAIJRE
IIPINCER
TERPERATURE
"f
A±
/
Jtl
J1L
/V.
U
X
^L.
M
7IL
el
3LL
2^.
£L
4.
JC
JSL
XL
J/l
\
tn
Jl
,64
Ji
11
ra~
*SL
2£
M.
COMMENTS;
EPA (Dm) MS
r?
-------
[HAVE USE
POINI
NUMBER
~TvV\ 0 I !C
CAS M1ILH READING
" "
VEIOCMY
HEAD
in Hn
ORiriCE PREiSJHf
i&Hi in
•DEimco
ACTUAL
SIACK
IEMPERATUHE
• I...T
DRVCMMHER
lEMPEFIAIURt
INK I
OUIlEI
PU«P
VACUUM
ID M|
SAMPLE BOI
ItMPERATURE
"F
IMPINCt R
UMPERAIuni
£±
fefcr
f/1
-it
f/r
6
r 6
-O-
1
zr.-|
-------
COnPOBOTIO*
MOISTURE AND IMPINCER CATCH DATA SHEET
v\
v •
Impinger
Number
Solution Solution (mL)
Conf Iuraclon
Weight (R)
'Z'
^OD 6-5
MOD 6"
MT —
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain tCi A'
Final
Inital
Wt. Gain «fpi
Final q?<7.(
Initial
Wt. Gain
Final
Initial
Wt. Gain i».^
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Total laplngers Weight Cain (We), grams
Vf - Final Meter Volume • ft3
Vt - Initial Meter Volume - ft3
DFMCF - Dry Gas Meter Correction Factor - _
Vffl - Metered Gas Volume • (Vf - V1)(DGMCF)
T - Average Meter Temperature • °F + 460 •
P • Meter Pressure (Barometric Pressure) •
„ m (17.6ft)(Vm)(Pn) (17.64)(__
vm(std) -
Analyst
3
ft3
°R
in.Hg
ft»)( In
Hg.)
Vw(atd) " Voluna o£ M«ter
• Moisture Fraction -
*)
- .0472(
vw(ctd)
Jt«
ft>
ft
It1
-------
PLANT.
DAIE_
SAMPLING LOCAII
SAMPLE TYPE .
RUN NUMBER J!
OPERATOR 36?^
MBIERT TEMPERATURE _
BAROMETRIC PRESSURE _
STATIC PRESSURE. IP,|_
FILTER RUMBER HI
PflOBt LENGTH AND frPL__
NOZZLE 1.0. L3J-
SSSUHED MOISTURE ' ,2
SAMPLE BOX NUMBER
ME TEH BOX NUMBER
METER AH
JLco
y " MINUTES
TRAVERSE
POINT
NUMBER
GAS MEIER READING
VELOCITY
HEAD
ApjI. in, HjO
ORIFICE PRESSURE
DIFFERENTIAL
liHI. in. H^Ol
DESIRED ACTUAL
STACK
TEMPERATURE
(1,1. "F
DRTGA1 METER
TEMPERATURE
INLET OUTLE1
PUMP
VACUUM
m H|
SAMPLE BOX
TEMPERATURE
IMPIMGEN
TEMPERATURE
"f
tt>
JLl
_£lL
JM
^2
yr
J7S
&-
//y-o
u*
m.
120-0
n
7O
J72
JTA
Jj-
J-tl
SO
£_I
f>
S£
371
^L
ML
Hit
2D.
JJ±
1
IL
1k
32_
Jl
IS.
^
M.
^1
15
~H5
0
a
A3
M-
li.
n
im
wo
/rp
//I
COMKNIS
EPA (Dot 21i
-------
-------
MOISTURE AND OfPINGER CATCH DATA SHEET
Irapinger
Number Solution Solution (mL)
k* "I-" -
i r\T
**HX>.W*», *03
^^ ^
Configuration Weight
l^OD G~~S Final ""]
Initial <-
Wt. Gain j
Mot) 6"~S Final ^4
Initial £
Ut. Gain j
l/U^b £**~'i Final *"
Inital £
Vt. Gain
(a)
M7
i7(,5_
tfrm$\...:fr.-f\
m
q3,%
[ **f 1 , 3
ir?»2^
04 ,v-
Final 41^,3
Initial ^f?^,3
Wt. Gain t
NoO
Final
Initial
Ut. Gain iii-T
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Total Imoinge re Wei ah t Gala (He),'grams
Vf • Final Meter Volume - ft3
Vi • Initial Meter Volume - ft1
DFMCF • Dry Gas Meter Correction Factor -
VB - Metered Gaa Volume - (Vf - V^DCMCD •
T « Average Meter Temperature • °F + 460 «
P - Meter Pressure (Barometric Pressure) -
n
Analyst
eR
In.Hg.
v«(itd)
m (17.
B)
fci
Vw(8td) " VolufflB ol
• Moisture Fraction *
.0«72
-------
DATE
SAMPLING LOCATION tV^L
SAMPLE TTPE
RUII NUMBER
OPERATOR
AMBIENT TEMPERA TUBE
BAROMETRIC PRESSURE .
STATIC PRESSURE. |P,I_
FILTER RUBBER III
PflUBt LENGTH AND HPL
NOZ/Lf ID
ASSUMED MOISTURE.',
SAMPLE DDK NUMBER
METER BOX NUMBER
b (j L ±)
HI'
n %
4,'- 33
METER AHp J <.'£-'
/.CTACIOB " , fr
1 PROBE HEATER SETTING
;s
Jii-
HEATER BOX SET TING >•> *
REFERENCE A. <
t ^ ^*4 7t.»
r>
SCHEWTICOF TRAVERSE POINT IATOUI
READ AND RECORD ALL DATA EVERT.
MINUTES
FRAVERit
POM I
NUMBER
CAS IETER READING
VELOCITY
HEAD
ORIFICE PRESSURE
DIFFERENTIAL
(aH|, In. HO|
DESIRED ACTUAL
STACK
IEMPERATURL
IT...-F
DRTGMHTER
TEHPERAIURC
INLET
IT. ^."
OUILEI
PUMP
VACUUM
in. Hf
SAMPLE BOK
TEMPERATURE
"F
WINGER
IERPERATURE
"F
: 6
_£S_
JJL
Jl
H
MO
70, 5
J_l
'JJL
Jo
MIL
77T
Jl
LM
jm.
i±
js
MS
^3_
t/2
5?
IQJ3
31
S2_
/D
Hi
C 5
JT7
fftf)
Jo ft
13-
71
/to?
s-
Ml
JLtUL
ns
JOL
f>
.M
21
j IM
COmENTS.
EPA (DM) IK
JtUiL
/01/77
7-3
i
-------
n;
IHAVERSE
POINT
NUMBlfl
SWUNG
TIKE. KB
CLOCK I Ml
hi
ClOCRi
CAS ME. I LN HEADING
•v »J
IIHftNGlR
lEWEHilURI
•r
-------
s
RADIAN
: O M
Impinger
Number
MOISTURE AKP DiPIHCER CATCH DATA SHEET
Solution Solution (ml)
Configuration
*teifi"i: to),,,,
NT
/MOD 6 '5
MT
mon 6 "
Final
Initial
Wt. Cain
Final
Initial
Wt. Cain
Final
Inital
».'t. Gain
Final
Initial
Wt. Gain
Final
Initial feV5.Z-
Wt. Gain -
Final
Initial
Wt. Cain
Final
Initial
Wt. Gain
Total Impingers UeighC Gain (He),'grans
Vf « Final Meter Volume » ft3
Vt - Initial Meter Volune - ft3
DFMCF - Dry Gaa Meter Correction Factor *
Vn • Metered Gas Volume - (V| - V1)(DGMCF) -
T - Average Meter Temperature - °F 4- 460 «
p « Meter Pressure (Barometric Pressure) -
Vstd) "
fa
" VoluBie o
Bw8 - Moisture Fraction -
ft')
" .0472(WC) - ,0472(
Vtf(ctd)
g)
ft
ft1
ft
ft1 -
-------
APPENDIX A.2
PM]0/CPM
-------
•>
a
*
\\>'
Run
Code
ID
crgD
fllCAC
IP
OrUntation
«•-*<.
Sampling
v
Dian«t«r-ID * (in)
,.. ,
f/
start
End
Sanpling
Due at ion
(mini
D9€
(final)
Saaple
(ft3)
Dual Hanonatttt
and
M*qnah«lic3 Zeroed?
V33-,
Conpoaition
ICO
Moiatuct Content
Pi tot I«sJc Check
(P05)
Stack
ft«p«t»tur«
^i u .-
'
Oil£«r*ntial Stack
(in.
T»«p«rature
Cf)
Aabient
Pe***ui«
(In. Hq)
velocity
System Leak Check
., O l_ &, lo "
Moees
Kin
Tine
H
Port Mo
Ttav.Pt.
A) «}
PI tot
.(pf
i.r
Sample
• s
DO*
Vbltaoa
T
Stack
T
Ptob«
t
DGM
Dwell
at
*Dwell Tine, t.
ff- f. CSfl
I/lMt
-------
V1*
Run
Ced«
SMpitC
ID
Filcar
IB
Ori«P«t«tion
1-octtion
Nozzle
Di«»«t«r-ID (In)
Op«titor
0«t«
Start
Time
Bnd
Tia*
SBJpLincj
Due at ion
(«in)
Stack
Diffectntitl Stack
?ceeaat« (in.
Aabient
Aafiient
Pte»»ure
(in. Hq)
Velocity
OGH
(final)
S«npl«
Volume
(£tj)
Dual
L«v«l«d and £«te*d?
Naqnehtlics I«ro«0 If
Pitot Leak Ci«cn
(Po«)
ttote*
Run
Tine
Pert No
Trtv.?t.
c 7
Pi tot
o
AH
Sample
-n-
D01
ri.l
~ ft. ^
T
Stack
T
Probe
T
ox
'
-ft
ii. r
•5-r
Time
"15
LC
-^ I
*0w«ll Tine, t. •
'6 P.
-------
5-- ti
IrT-H
jj^ifc
Hi
3
Run
Code
Sampler
niter
ID
Orientation
Sampling
Location
NOZZle
Di*n«t*r-rD
(in)
Op«ratoc (i)
Data
Stut
Tia«
find
Stapling
Ou tat ion (mini
OQ(
(initial)
DQf
(final!
Saapla
7olUB« (ft3)
Dual Manonetar L«v«l*d and Zeroed?
Magneh«lics Zeroed?
Gaa Composition
tea, tOj %co
Moisture Content
ten
Tim*
gjQ
fort So
Tt iv . Pt .
£ |
^L,
O
IT"
P r
Pitot Laak Ch«ck
(Poa) (Neg)
AP
Pitot
el-U
2 ^
i-ir
,(•0
,M|
FlKH
AH
SanpLa
L LVii
OGH
«r^>
v. ^_
%.ir
r?7i
n.^3
r
Stack
Ttapxfitura ('n
Differential Stack
Pteaaure (in. R^O)
Aabi«nt
?eap«ratuf« (*p)
Aobient
Pressure . (in. H"-/
;^r
;^/-
"*! ' ^ >
T
;> 3"
T
OCM
^/i?
^
3-y.f
>J/4/.
7«
Dwell
f •••!
7 >_ J
/6 /
/-1 L
?'/
F/jurt 5- f. CSR fold dta
43
-------
io
MOISTURE AND IMPINGER CATCH DATA SHEET
Implnger
Number Solution
Solution (ml)
Configuration
Weight (g)
PI
I o o
Final
Initial ^
Wt, Gain ~
. 7
oo
Final owit'-
Initial STJZ.
Wt. Cain ;- -
Final
Inital '
V't. Cain
Final
Initial**
Wt. Cain
Final
Initial
Wt, Gain
Final
Initial
Wt. Cain
Final
Initial
We. Gain
2n ~. €
Total Impingers Weight Gain (We), grans
Vf - Final Meter Volume - ft3
Vi - Initial Meter Volume - ft3
DFMCF • Dry Gas Meter Correction Factor •
Vn - Metered Gas Volume - (Vf - Vt)(DGMCF) -
Tffl • Average Meter Temperature - °F + 460 •
Pn • Meter Pressure (Barometric Pressure) •
) (17.64)( ft!)<
Analyst
Fi\Ur ^o,
_ ft3
-°R
in.Hg.
in.Hg.)
-R)
Tn C
V«(atd) " Volu»e of Water Vapor - .0472(WC) • .0472(_
- Moisture Fraction •
g) -
ft1
ft1
Vw(std>
ft
ft1 -
-------
11
UM'
V-lf
2: 3?
:$i O
Code
Saaplec
ID
nicer
IB
Saaplcr
Orientation
Sanpling
Location
Di«iB«ttr-lD '
(in)
Op«tttoc (i)
Date
Start
Tifl*
End
Sanplinf ,
Duration
Cain)
(initial)
ocat
(final)
Saaple
VoilUM
Ut1)
Dual Hanoneter Leveled and Zeroed?
HagneheliCJ Zeroed?
G«a Composition
*COj 1C, ICO
Moisture Concent
Pi tot LeaJc Qteck
(Pea) (N*g)
Stack
Ttap«rmtute
(*?)
Diittrtntial Stack
Preeauct f ^ f (in. RjO)
Xabient
(in. Hg]
SAC
velocity
SyiteJi Leak Check
ttotea
Run
Tine
7-Yo
I/.
1 >
Poet Ho
Tt«v.?t.
£3
D i
03
DT
AP
Pi tot
Mf
AH
Sanple
O./fc
Volume
3t.
T
Stock
ore
StHl
T
DOf
41-
-zi,
Tinwu
n
$• 1. CSR fiatd din X/IML
63
-------
J-7-/
U
f: H
O'.JM
l1 -.3 ca
Run ^*.o - 2- ' ~
Code ft* 1 *f ^J
ID
Filter
ID
Saaplec
Orientation
Sampling
Location
Nozzle
Diameter -ID (in)
Operator (t)
Data
Stazt
Tiae
bid
Tiae
Sampling
Due at ion (»i>f
DO .X'
(initial) ^X^
DQt s*'
'^arlune (ft1)
Dual Manometer Leveled" and Zeroed?
Haqnehelics ZeroejW
Gas Composition
%Ci*% %o_ ^X|CO
MoiatuHT Content
Tiae
I«*r i(a
l*:*4
32." •*
3H--M
3t:at
U'.sf
7t;rs,
ff:iK
•**«
*/?' 2*
fk'.^Y
^ :^
Poet Ho
Tr av.Pt.
d.flT
A2-
6.H3
a.«^
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Sample
|
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71 T-
21 »-
jr/
^
T
EQ1
7^fe
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<4>
V-t
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%
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^ V V-
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j-y
5;.
•D-.U Time. t -
*'yur» 6- f. CSfl ^ff/fl1 tfan
45
-------
-3f
Run M.-T- .
Cod.' " <*3*F?>)
Samplat
ID
niter
10
SaBplar
Orientation
Saaplin?
Location
Nozzle
DiaiB*t«r-ID (in)
Op«catocli)
Data
Staxt
Tia«
2nd
TiM
Sanpl ing
Duration Cain)
DQ» .
(initial) ^X^
DM .x"
(final! ^X*^
SaapUx"
voljirfi (ft1)
Dual Manomater L«v«led >erfcl Iaro«d?
Hagnehalies Itcoed?/'
Gas Corepo«itm*r>l
iCOj lOj ^x*^
HoistuitxCSntent
Run
w?
5"3.%
n.it
Jl:^1
fil'.tfr
43:o5
POCt HO
Tiav.Pt.
A/
A-^
^3
Avf
^r
Pi tot L«ak Oiecft
(Pos) (N*;)
ap '
PI tot
3,*r
j.>
h^
o.'k*
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, n
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6-J. CSR fiftd dm
65
-------
COncOBATIOM
MOISTURE AND mPINGER CA" ,,i DATA SHEET
Impinier
Numb e r
Solution Solution (mL)
Configuration
"eight (s)
loo
MT"
Final
Initial
Wt. Gain
Final
Initial
Wt. Cain
Final
Inital
Wt. Gain
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Total Impingera Height, Gain (We), grams 7- *-H
Vf » Final Meter Volume - ft3
Vi • Initial Meter Volume - ft3
DFMCF » Dry Gas Keter Correction Factor -
V0 • Metered Gaa Volume - (Vf - Vt)(DGHCF) -
TB • Average Meter Temperature - °F + 460 - __.,_
fm - Meter Pressure (BarOMtrie Pressure) »
_ (17.6ft)(?a,)(FD) (17.64)( ft>)(_
Analyst
D
vm(std)
in.Ug.
In.Hg.)
ft
Vvr(std) - Volume of Water Vapor - .0472(«c) - .0472( g) - ftj
B^g • Moiiture Fraction • ^(ctd) {c^
-------
\ ^
I'r
^
I 1'13
H ' ^ •' 3l
•55
Code
ID dJif
niter
ID
Orientation """
Stapling (ir^^k.. L
Location s hx^k.
Nozzle ,^v
Dianeter-ID (in)
Operator {•) ^^
°"' 9f^JM
Start
Tiae ^ /-'/,>
find
Saapling ^ L, j *,,'-,
Duration (ain)
DOI y^-
(initiall ^ ^ cnj
SOI
(final)
Saaple
Volume (£t3)
Dual Manometer Leveled and Zeroed? J""""
Hagnehelics Secoed?
G*aa Campos i"tion
Moisture Content
Run
Tine
c,:10
7'Hr
io :o -
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. 3
r,
Fiffurt 6- 7. CS/? /7«/tf dan j/ie*t
-------
J 5 0 * ; ,
Run
CoAm
-; 3
(a. >•=
ID
rilttr
ID
sanpitr
Orientation
Sapling
Location
NOZZi*
Diaa«t«r-ID (in)
Op*t«toc
St*rt
Tia«
Bnd
TiM
X TeatMcatur*
Duration
»»in)
(initial
D» /
(fifva)
(Jt3)
Dual Manoreettt
and I«co«d7
Gaa Conpoion
%CO
Hoistup-ri*i Stack
Di£f»r«r>ri
Vt*Mdc«
(in.
(*?)
Amiiant
Pt«»«ur«
(In. Hq]
Systan Laak Ch«ck
Run
Tin*
or
3 a '.
30
37:
*: O
POCt No
Tf tv.Pt.
£1
5 f
Df
4P
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0 .
3
43
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DQ4
73
T
Stack
1
CCM
Tin
,
n
TJ. ^
a'
/TFJ~
/jji/rt 6- 7. CSfl ffe/tf rfara
45
-------
Run Md - 3 "
Code { I of 1
ZD
rilter
10
Stapler
Orientation
Sanpling
Location
Nozzle
Diaseter-ID (in)
Operator (•)
0«te
Start
Tlae
End
TiM
Sampling
Duration (ain)
DW .X
(initial) ^
DW v^
(final) ^/
?"5iJ^ ""(ft*)
Dual Nanoneter Leveled JK& Zeroed?
Magnehelics ZeroedT^X^
Gaa Compos ft ip*i"
%C02 103 ^x«CO
Moistu^jr'tontent
ten
Tine,
vf.jX
5-30?
5-C,:J>
V^-'ST
_
Port Ho
ttav.pt.
tj |
C.I'
C7
c^
csT
Pi tot LeaK Check
(Pos) (N«r,
*JT>
jn
;ro
Dr,
T
r-rnha*
m 1> VMum
^r
>T3
T.70
i>?
^Z
T
001
-^f
%••
V>r
'V
%
Dwell
r&^ (
pcr
H?..
lz_
*/,
Time, tn -
Figurt 6- 1. CSA
45
-------
RADIAN
COBPOHATIOM
10
MOISTURE AND IMPINGER CATCH DATA SHEET
Impinger
Number
Solution
Solution (mL)
Configuration
Weight (i)
Joo
I no
O'S
(VIOQ G--S
6-lS
Final
Initial
Wt. Gain
Final
Initial 43-T. 3
Wt. Gain .£"? -
Final
Inlta
'.'t. Gain
Final
Initial
Wt. Gain £ -
Final
Initial
Wt. Gain
Final
AH.!* h» -feS,*.
Wt. Gain
Final
Initial
Wt, Gain
Total Imninaera Weight Gain (We), grams
V£ - Final Meter Volume - ft3
Analyst
V - Initial Meter Volume -
ft3
DFMCF • Dry Gas Meter Correction Factor -
V^ - Metered Gaa Volume - (V£ - V1)(DGMCF) •
T • Average Meter Temperature - °F + 460 •
PO • Meter Pressure (Barometric treasure) •
m(8td)
(17.64M
fe«)(
. ft3
In.Hg
in,
Hg.)
ft1
- Volume of Hater Vapor - .Q472(«c) - .0472(_
• Moisture Fraction •
|) •
vu(atd>
ft
ft
ft3
-------
APPENDIX A.3
ALDEHYDES
-------
PI AMI
oA 11
SAMPLING LOCATION fl»^
SAMPLE TTPE /luOfh^
RUN NUMBER I
OPERATOR £
AMBIENT 1EHPERAIUBE _
BAROMETRIC PRESSURE _
STATIC PRESSURE, |PJ
FILTER NUMBER It)
5"t)
t
z.
)
J
V
s
C
\ 1
PHOBl LENGTH AND TVPL_
NOZZLE 1,0 £
ASSUMED MOISTURE.',
SAMPLE BOX NUMBER t
MEIER BOX NUMBER
MEIER ftHg
t FACTOR_
A/'- > "2.
tufe
PROBE HEATER SETTING
HEATER BOX SETTING
REFERENCE ap _
_?_JiB
__
•> t'Q
iCHCMATIC OF TRAVERSE POINT LAYOUT
HEAD AND RECORD ALL DAIA EVEH»_JLl_ MINUTES
/
COMIEHIS
-------
IMPING! R I
TIMPERA1URE
"F
-------
RADIAN
A
MOISTURE AND EHPINCER CATCH DATA SHEET
\ '
Impinger
Number Solution Solution (ml)
i bUPU Oao
2 DWPU 2^0
Configuration
faao &-£•
&-<>
Weltht (l)
Final SOI. 2-
Initial bJ.5,(i
Wt. Gain f?-f.l-
Final 7/06,-T
Initial 63^
Wt. Gain F*.. i-
Si
Final
Inital
'.'t. Gain £../
Final 613,b
Initial k(aS. Q
Wt, Gain £,£,
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Final
Initial
Ut. Gain
Total Impinge re Weight Gala (We),'grams <3J
V£ • Final Meter Volume - ft3
VA • Initial Meter Volume - ft3
DFMCF • Dry Gaa Meter Correction Factor •
V0 - Mecered Gaa Volume - (Vf - V1)(DGMCF) •
TO • Average Meter Temperature • °F + 460 •
P - Meter Pressure (Baroi
n
m (17.64)(7,n)(Pm)
vm(etd)
T.
w(atd) " Volume of Water
U- • Molature Fraction •
Analyst
etrlc Pressure) -
(17.64)( f
(_
Vapor - .0472(WC)
MctJ)
vw(std> + vm(Btd)
In.Hg.
t«)( In.Hg.)
_-R)
- -0472( g) - ,
•••••PMNMMNMP
ft1 +
^^^••••••••P
ft1
ft1
IMP
ft* -
•Mi *••••
-------
PLAIH
DATE
SAMPLING LOCATION /J..H*
SAMPLE 1TPE I (tL
RUN RUMBtR 3.
OPERATOR I
AM8IENT TEMPERATURE
BAROMETRIC PRESSURE _
STATIC PRESSURE. iP I _
fILTER NUMBER fit
ji
.if.)
PRODI IENCIH AND UPt.
NOZZLE I.D. ./'1(
ASSUMED MOISTURE,'.
SAMPLE BOX NUMBER .
METER BOX NUMBER _
•ETERaH.
I,
0 C.JL.,*- fc
— PROBE HEATER SETTING.
— HEATER BOX SETT INC
— REFERENCE ftp L--
SCHEJUTIC OF TRAVERSE POINT LAYOUT
HEAD AND RECORD ALL DAIA tVFHK A- 5 MINUTES
TRAVERSE
POBII
NlfllBER
CLOCK TPtt
CASttlERRtADIHG
I ^
VIIOCIIT
HEAD
IAP,I , m. HjO
ORIFICE PRESSURE
DirrERERTIAL
I4H) in HOi
DESIRED ACIUAL
SIACK
TEIPERATURL
n.i.-r
DRTGA1KTER
TEVCRATURE
INLET
II, J.«
^
OUTLET
PUMP
VACUUM
in. HI
SAMPLE BOX
TEMPERATURE
"F
INPMCER
1EMPERAIURE.
75
/?
11
/S"
/Pit
u
30
¥7
n
&I
S3
^75
Jb
£-L
.HI
HL
tit, Iti
XLJ^
II
*±
Ul
li
/j
COIMKHIS .
rPA iDuil 7)4
_LL
-------
DRTCASHMffi
IIBPERATURE
r
-------
MOISTURE AND rMPINGER CATCH DATA SHEET
"zL
Impinger
Number
Solution Solution (mL)
Configuration
Weight W
D/UPH-
Final
Initlalt*
Wt. Cain
Initial
Wt. Cain d 1- fl
Final
Inital
We. Gain ,1, g"
Final
Initial
Wt. Gain
Final
Initial
Wt, Cain
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Total Impingera Weight Gain (We), grams _
Vf • Final Meter Volume - £t3
Vi • Initial Meter Volume - ft3
DFMCF • Dry Gas Meter Correction Factor • ___
VQ - Metered Gas Volume - (Vf - Vi)(DGMCF) •
TD - Average Meter Temperature • 8F + 460 •
PO - Meter Pressure (Barometric Pressure) -
„ (17.64)(7m)(P0) (17.64)(
vm(aed) ' 1- . =
Analyst
. ft3
in.Ug.
In.Hg.;
ft1
V«(atd) " VoluBIB of Water
- Moisture Fraction -
" .0472(UC) - .0472(_
ft
ft1
ft -
-------
PLANT.
SAMPLING LOC AT ION _
SAMPLE T IPS __fl
RUM NUMBER ^_ 3
OPERATOR
AMBIENT TCKPERA1UBE
BAROUTRIC PRESSURE .
STATIC PRESSURE, IP,).
FlllEft NUMBER|s| ^
C* ^ ^
PROBE LENGIH AND
NOZZLE I.D. _
/. '
ASSUMED MOISTURE.'.
SAMPLE BOX NUMBER
•ETER 601 NUMBER A) - Bp
•ElEH 4Ht
'ft FACT OR :
PROBE HEAIER SETTING
HEA1ERB01SET1ING
SCHEMATIC OF TRAVERSE POINT LftTOUT
HEAD AND RtCOHD ALL DATA tVEHt
MINUTES
THAVEBU
POM I
NMBEN
ClOCR T
IK.-io
CAS ttTEfl READING
|¥I, II3
VELOCIIV
HEAD
(up,!, in H;0
ORIFICE PRESSURE
DIFFERENTIAL
(4 HI. in. «:0l
DESIRED ACTUAL
STACK
TtiPERAIURC
II/-F
DfllTCASKTER
lEBPERATMRt
INLET OUTLET
VACUUM
in H|
SAMPLE BOX
IEIPERAIURE,
°F
IMPINGEH
lEMPEfiAIURC
PRocess
71
JIO/J
cta_
5
/
5/0
.5
,5"
41
Inf.*
M.
SfbP
JLL
n
£_
foTi
• & §
l
70
7.5
70
l/Q-6
70
yn.too
JL
ZL
K
JLL
ia_
3L
3&2_
Hto*
2L
U.
7A
COMMEMIS:
FP» (Dun m
t
*'
-------
-------
oaPOQOTIOH
MOISTURE AND IMPINCER CATCH DATA SHEET
lopinger
Number Solution Solution (mL)
Configuration
"eiiht («>
Ht
Final
Initial
We. Gain
Final
Initial
Wt. Gain
Final
Inltal
'.'t. Cain
Final
Initial
Wt. Gain
Final
Initial
Wt. Cain
Final
Initial
Wt. Gain
Final
Initial
Wt. Cain
36. I
Total Implngers Weight Gain (We),'grams __
Vf - Final Meter Volume - ft3
Vt - Initial Meter Volume - ft3
DFMCF • Dry Gas Meter Correction Factor -
Vm - Hetered Gaa Volume • (Vf -
3 3 2 . (o
T • Average Meter Temperature - °F + 460 •
P_ • Meter Pressure (Barooetrlc Pressure) -
n
Analyst
„ _
vm(std)
(17.64)(
ft>)(
In.Hg.
In.Hg.)
" Volune of Water
By8 • Moisture Fraction •
• -0472(WC) - ,0472( _ g) -
ft1
vo(atd)
ft
ft -
-------
APPENDIX A.4
PAH
-------
MODIFIED METHOD 5
FIELD DATA
HUN I
A
PAGE^OF
PI ANT
DATE
SAUPLINO LOCATION
SAMPLE TYPE
RUN NUMBER
OPERATOR
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
STATIC PRESSURE (Pi)
INITIAL LEAKCHECK
/H^M-, ±<~
•I'&w
CUrfe*
i*')
MOISTURE METHOD
MOISTURE OAT A
O2JCOZ METHOD
02
coa
FINAL LEAKCHECK
READ AND RECORD ALL DATA EVERY J> MINUTES
TltMfM
Point
Numb*
0
£1
-^
IT
Sampling
Tim*
-------
MODIFIED METHOD 5
FIELD DATA
PLANT
DATE .
SAMPLING LOCATION
SAMPLi TYPE
RUN NUUBER
OPERATOR
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
STATIC PRESSURE |P»)
INITIAL LEAKCHECK
tn^L.L
J^-^T
ijfaT^ft1 I'fjrii
I
UP
mj
si. 7
o.on t
READ AND RECORD ALL DATA EVERY
MINUTES
-------
QBPORATIi
PAN Ru, 1
MOISTURE AND DJPINGER CATCH DATA SHEET
Irapinger
Number
Solution
Solution (ml)
Configuration
Weight (g)
MT
6-S
IMOD
(£?-" S
100
(V\OD
ft1
ft
ft
fts -
-------
MODIFIED METHOD 5
FIELD DATA.
HUN x
PAGE I OF
PLANT
DATE
SAMPLING LOCATION
SAMPLE TVPE
RUN NUMBER
OPERATOR
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
STATIC PRESSURE (Pi)
INITIAL LEAKCHECK
/%M.j £t_
Tj5
'Vki,
Mi*
~L-
J^__
so
m
.J^Ib^ifl"1
PROBE LENGTH AND TVPE
N02ZLE 1 0 (in)
ME TEH BOX NUMBER
METER * H0
Yd
K FACTOR
PROBE HEATER SETTING
HEATER BOX SETTINQ
XADTRAP
HEIGHT OF LOCATION (H)
.J- .OWLi
i
.J^l. _._
fj-3o
f -*4
111%
,L5
Ko
150
V
DUCT DIMENSIONS
FILTER TYPE
FILTER NUMBER
ASSUMED MOISTURE (t*>)
MOISTURE METHOD
MOISTURE DATA
021C02 METHOD
O2
C02
FINAL LEAKCHECK
H?"x
READ AND RECORD ALL DATA EVERY _j MINUTES
PaiM
Nujnbw
A\
SAmpttng
Tim*
(rnbl)
_£2_
Clock
Tlma
/31?
131%
^5-3
(Vm), cu 1
jf^l.
VeJocMy
HMtf
J^L
.25-
Flue
Gil
Tampaiuuic
Onhca
PIBMUI*
DtftaentUI
JJ-
^10
IL
Fdiar
TcmpMilur*
Ab MM twill
Tltp
VY -
Tampaialuie |'F)
Dty Qaa UMM
mm
*<*
OUIMI
3T"
bnpingai
Pump
Vacuum
A.
,_iA
__J_
.J^l^
Oo
T5
Ul£L
-JJ-
£5
~Jl
_^^L_
.-TQ
_J^u_
7ci_.
-------
TJ*VHIM>
Pi Mil
Numbai
VL
-A.
3
-V
5"
Tim «
(tniii)
"
Jo5.
tt±
J25L-
Cl.--k
Tuna
_!?-—'!
-M7-
//IS
two
Gao UtHttl
Huarting
(Vm| cu n
JU
^5
jtf«3
HUM
mm
*
Vfliucily
Head
( • ?•).
m.H2O
W.
^1_
Fluo
Gai
rn
Onlico
Dittaianti*!
(» H, In H2O)
•t
FlIlBI
Tampaialuia
t'F)
Alituxljflnl
I rap
Inlui
HT-
r.^t"."
tju
(*F)
bikri
[Tmin)
Diy QaiUelai
Oullal
.^.
-ff-
-^4-
linp'iigui
PUIIIJI
Vacvuni
_O"_HB»_
-------
MOISTURE AND DiPINGER CATCH DATA SHEET
Lmpinger
Number
Solution
Solution (ml)
Confiuration
Weight (R)
HT
loo
Final g 17. 2.
Initial ifTy.C*
Wt. Gain \qt.L
Final
Initial
Wt. Gain i gf-.
100
MT
moo >-
Final
Inital
Wt.
,((,?
%J
6 -
Final
Initial
Wt. Gain
Final
Initial
Wt. Gain
Final
Initial
Wt. Cain
Final
Initial
Wt. Gain
i^
Total Impinger8 Weight Gain (He), grans
Vf - Final Meter Volume - ft3
Vt • Initial Meter Volume • ft3
DFMCF - Dry Gas Meter Correction Factor - _
Vffl - Metered Gas Volume • (Vf - Vi)(OGMCF)
T « Average Meter Temperature • °F + 460 •
P • Meter Pressure (Barometric Pressure) •
(17.64)(
Analyst
ft3
Vstd)
In.Hg.)
ft1
Vw(std) " Volume of
BW- • Moisture Fraction •
• .0472(WC)
Vtf(etJ)
.0472( _ g)
ft*
vm(Btd)
ft1 + ft1
-------
MODIFIED METHOD 5
FIELD DATA "
IIIIN
CAGE i or
Pi ANT
DATE
SAMPLING LOCATION
SAMPLE TVPE
RUN NUMBER
OPERATOR
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
STATIC PRESSURE (P«)
INITIAL LEAKCHECK
ftACH^ fa
°lnJlfLi
•>rp-^w
fti/'>
^
1^
>u
W?
.oifriSH*11
PROBE LENGTH AND TYPE
NOZZLE 10 (Hi)
METER BOX NUMBER
METER * H<9
Yd
K FACTOR
PROBE HEATER SETTING
HEATER BOK SETTING
XAOTRAP
HEIGHT OF. LOCATION (h)
6 'yky _
.^/
.& &
/ /.si
, TlJJf
rfrA'JL
^>o
f>0
DUCT DIMENSIONS
FILTER TYPE
FILTER NUMBER
ASSUMED MOISTURE ()
MOISTURE METHOD
MOISTURE DATA
O2/CO2 METHOD
O2
CO2
FINAL LEAKCHECK
Hf * / HL
HEAD AND RECORD ALL DATA EVERY 5 MINUTES
Mm
Numtw
_^2
Sampling
Tim*
(ffllfl)
Jf
_.fff.O
-^—
Cluck
Tlm«
«<-*">
2£/_.
_Z^
/oo
I
/o
]i
././flLL
(toadlng
(Vml. cu B
. 5"
55.
7T
Velocity
/, 1
ho
JL .
Flue
Gat
Onlice
PiiMUia
/f
11
^1.
___
Filial
T0mpa(«ui*
H> tut beiil
Ti»p
_iO_
_33_
j^_
T*mpeialuie(*F)
Inm
JT
r7
OulMl
.ro
61
JO
lmpttifl«i
Pump
Vacuum
j^_
_-i
j5:"
-------
c e
IWIL. I I lV_/L-» il
FIELD DATA
HUN
PAGE J' OF
PUNT
DATE
SAMPUNQ LOCATION
SAMPLE TYPE
RUN NUMBER
OPERATOR
/H*rL ^C
1-Jo'll
fto
3
Jtf
Trm
Prtnt
Numb*
Sampling
Tim*
(mta)
Ckwh
Tim*
<24-llf)
Qmhtotor
RMding
(Vm), ou.ft
Vrtoctly
Flue
Q*t
T MR pw cture
(•F)
Orlftca
Prmura
CNIfaiaMM
(* H, in. H2O)
Fitter
TamperMuni
DryQatMMW
Inkrt
(Tmln)
Outfel
(Tmootj
Implnger
Erf!
Pump
Vacuum
1-6
11
-7S
rftf
76
£
M-
s1
SI
M3I
,
-.40
Zf.
ICO
56
(itl
17
we
S
1
l/ll
1,0
71
llo
,32
r
jr
I'U,
COMMENTS;
-------
RAOIJUi
MOISTURE AND EMPINGER CATCH DATA SHEET
Impinger
Number
Solution Solution (ml)
Configuration
(R)
Final
Initial
ME. Gain 3-1 9- 7
&-S
mebb-
Initial
ME. Gain 7*/.
Final
Inital
We. Gain
IHT
s-s
Final *yf:V
Initial
Wt. Gain
J"
Final
Initial
Wt. Gain /2.7
Final
Initial
Wt. Gain -r-jTb.
Final
Initial
We. Gain
Total lmpiQR.ers Weight Gain (We), grams
Vf • Final Meter Volume • ft3
Vi - Initial Meter Volume - ft3
DFHCF • Dry Gaa Meter Correction Factor -
Vm - Metered G&a Volume • (Vf - Vt)(DGMCF) •
T • Average Meter Temperature - °F + 460 • _
Analyst
ft*
m
vm(etd)
Meter Pressure (Barometric Pressure)
. U7.64)(Vm)(Pm) (17.64)(
• in.Hg.
ft*)( in.Hg.)
ft
•R)
V«(etd) " Volua* of Mater Vapor - .0472(WC) - .0472(_
- Moisture Fraction • • V
ft3
Vw(atd) + VB(8t(J)
ft1
ft1 -
-------
APPENDIX B
PROCESS DATA SHEETS
-------
For* RECf04
100
J <
*3-
J
7PM
TPK
°F ,
N
e
ti
1
i
GM
iMfL
°F
FRHUMB
to
11
MumUiiy
12
Jr
o
,¥,
n
©
SX5
.35"
f -«*t
•1
0
2&D/23D
fi
3L
3io
ia
.3?
335
O
MT
Ll
^4
O
^•s*
3fO
-2,0
II
rzz.
o
•ft-
c?.'37
'. Mi
_0_1.
c»
3.0
5*7655
(9
.33-
57^73
0
5-0, C
Jt
H
S.fl'
3^10.
50,0
JLL
31
jl
IV
51.
-------
Farm REC*Q4
\CO
FHGE EL OF
JC.U
TPH
Drop
CXft
10
is
12
Ovmpar
4*
o
&fc
US'
51,6
31
42
.3}
/5"
21
'SHa
i,
o
11
SL
U_
za
-D
u
-------
RECfQ4
P»Ce I OF
•fvtfCN
tot<
Corf
ytaing
l
t^P
TPH
TPH
Asph*
Tt
C
3(0
,4-
31
19-
3DO
DO
C
O
073
O
ND
jflL
3',
103
O
lij
0
02
O
ill
13&
21
XI
j/r
^07
-------
Cf04
z
35
2
Fvtflfc*
Co-
c
c
W..-V
WH
RAP
bo*.
e
SdUbtMT
Ctap
Ojt
10
u
2
2-10
o
a. 3
350
An
G
w
HI
0-40
O
310
a.35
Hi
O
£7?
fT
LM
HI
a,1/!
Ti
c
-------
APPENDIX C
SAMPLE PARAMETER CALCULATION SHEETS
C.I PM/Metals
C.2 PM10/CPM
C.3 Aldehydes
C.4 PAH
-------
APPENDIX C.I
PM/METALS
-------
FACILITY : Mathy 06
[DATE: 9/20/91
(LOCATION: Outlet
(RUN NUMBER: 3.00
(SAMPLING PARAMETER TN
I
[Total Sampling Time (min.)
| Corrected Barometric Pressure (In. Hg)
(Absolute Stack Pressure, Ps( in. Hg}
(Stack Static Pressure (in. H20)
(Average Stack Temperature (deg. F)
(Stack Area (sq.in. )
| Meter ed Volume, Via (cu.ft.)
| Average Meter Pressure (in.K20)
(Average Meter Tenperature (deg, F)
(Moisture Collected (g)
(Carbon Dioxide Concentration (XV)
| Oxygen Concentration (XV)
(Nitrogen Concentration (%V)
jDry Gas Meter Factor
| Pi tot Constant
(Paniculate Catch (g)
i
1
(Average Sampling Rate Cdscfm)
(Standard Metered Volume, Vm(std) (dscf J
(Standard Metered Volune.VmCatd) (da on)
(Standard Volume Water Vapor, Vw (sef)
[Standard Volume Water Vapor, VH (son)
(Stack Moisture (XV)
(Mole Fraction Dry Stack Gas
(Dry Molecular Weight
(Wet Molecular Weight
(Stack Gas Velocity, Va (fpnO
(Stack Gas Velocity, Va (gpa)
(Volumetric Flow Rate (aefrn)
(Volumetric Flow Rate (aenxD)
(Volumetric flow Rate (dscfn)
(Volumetric Flow Rate Cdsom)
(Percent laokinen'c
(Percent Excess Air
(Fuel Factor, Fo
(Ultimate C02
(Concentration of Particulate (graina/acf)
[Concent rat ion of Paniculate (g/acm>
(Concentration of Pertfculate (graina/dscf)
(Concentration of Particulate (g/dscm)
(Concentration of Particulate (grains /dscf 3121 CO2)
1
125.00
29.68
29.74
0.80
245.08
2016.00
58.38
0.86
65.46
506.70
5.40
14.27
80.33
0.98750
0.84
0.01550
0.46
57.57
1.631
23.89
0.677
29.33
0.707
29.43
26.08
4222.90
1287.14
59120.55
1674.294
31085.51
880.342
104,21
205.23
1.228
17.02
0.00218
0.00500
0.00415
0.00951
0.00923
-------
FACILITY : Mflthy «6
(DATE: 7/19/91
[LOCATION: STACK
[RUN NUMBER; 1.00
(SAMPLING PARAMETER .TH
1
(Total Sampling Time (min.)
[Corrected Barometric Pressure (in. Hg)
[Absolute Stack Pressure, Ps( in, Hg)
[Stack Static Pressure (in. H20)
(Average Stack Temperature (deg. F)
(Stack Area fsq.in.)
[Metered Volume.Vm (cu.ft.)
[Average Meter Pressure (in.HZO)
[Average Meter Temperature (deg. F)
(Moisture Collected (g)
(Carbon Dioxide Concentration (XV)
(Oxygen Concentration (XV)
(Nitrogen Concentration (XV)
(Dry Gas Meter Factor
(Pi tot Constant
(Paniculate Catch (g)
1
(Average Sampling Rate (dscfm)
(Standard Metered Volume, Vm(std) (dscO
(Standard Hetered Volune, Vm(std) (dson)
(Standard Volume Water Vapor, Vw (scf)
(Standard Volume Water Vapor, Vw (son)
(Stack Moisture (XV)
[Hole Fraction Dry Stack Gas
(Dry Molecular Weight
[Wet Molecular Weight
[Stack Gas Velocity, Vs (fpm)
{Stack Gas Velocity, Vs (mpn)
(Volumetric Flow Rate (acfm)
[Volumetric Flow Rate (aeon)
(Volumetric Flow Rate (dscfn)
(Volumetric Ftow Rate (dsam)
(Percent Isokinecic
[Percent Excess Air
[Fuel Factor, Fo
[Ultimate CQ2
| Concent rat ion of Paniculate (grains/ocf)
(Concentration of Paniculate (g/actn)
[Concentration of Particulate (grains/dscf)
| Concentration of Particulate (g/dscra)
(Concentration of Particulate (grains/dscf 312X
1
125.00
29.68
29.74
0.80
240.60
2016.00
62.44
0.96
63.28
553.50
5.62
14.15
80.23
0.98750
0.84
0.02360
0.49
61.87
1.752
26.10
0.739
29.67
0.703
29.47
26.06
4540.05
1383.81
63560.69
1800.039
33472.05
947.928
104.01
200.80
1.201
17.40
0.00310
0.00709
0.00589
0.01347
C02) 0.01257
-------
JfiN 2il '92 13:09 RCDIflN CORP PPiC NC
P.2
tacky
|OUI; B/19/01
ILQUTIDMI cur Lit
IBUH tiuuEBi J.flO
|u0uac PAjuaanift r«
1
[fetot Boiling Tta» (•in.)
|Corrco(rd to rout Ha Prveaur*
-------
APPENDIX C.2
PM10/CPM
-------
JPTi 2B '92 IS: 25 RREIflN CORP PPK NC
P. 15
SAMPLE PARAMETERS FOR PM10/CPM RUNS
MATHY CONSTRUCTION COMPANY - PLANT tf (1991)
Corrected Barometric Pressure (in Hg)
Stack Static Pressure (in. H2O)
Average Stack Teraperature (deg. F)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (36 V)
Stack Moisture (%V)
Stack Gas Velocity, Vs (fps)
Volumetric Ftow Rate (acfm)
Volumetric Flow Rate (dscfm)
Stack viscosity (micropoJse)
.
Total sampling lime (min)
Average Meter Temperature (deg. F)
Average Meter Pressure (in.H2O)
Average Sampling Rate (dscfm)
Avftrag* Sampling Rate (acfm - cyclone cond)
Standard Metered VoIume,Vm(sul) (dscf)
Percent Isoldnetic
Paniculate Emissions < Cut Size (Its/hi)
Paniculate Emiwioni > Cut Size (Ibs/hr)
Paniculate Emissions Total (Ibi/hr)
M9
m
-
29.68
0£0
241.42
5.10
14.12
ea7B
2S.53
74.6'
62705"
33530'
198.32
m
70^2
65.18
056
0.41
0.78
29.36
95.8
2.04
1.68
3.72
29.68
O.SO
254 J5
5.40
14,24
8a36
2E52
72.9*
61261'
32656*
202.01
64.07
69.68
0.56
0.41
0.79
26.56
100
1.32
1.66
198
29.68
0.80
241.84
5.62
13.61
80,77
27.6S
70.2*
38967*
32105*
199.01
61.00
7160
OJ6
0.40
0.74
24.55
97.7
1.28
l.2fl
2.56
29.68
0.80
246,07
537
13,99
80.64
2R22
72.59
60,978
32,764
199.85
NA
69.15
0.56
0.41
0.77
26.82
NA
1.55
1.54
3.08
' Value taken Front lite average of all other tnuu as the PM10 flow raid (She 6) were
kiKpca (20 - SO higher).
NA =• Not Appticnble
-------
APPENDIX C.3
ALDEHYDES
-------
FACILITY : Mathy #6
DATE: 9/20/91
LOCATION: STACK
RUN NUMBER:!
SAMPLING PARAMETER
ALDEHYDES
Total Sampling Tine (min.)
Corrected Barometric Pressure (in. Hg)
Absolute Stack Pressure,Ps(in. Hg)
Stack Static Pressure (in. H20)
Average Stack Temperature (deg. F)
Stack Area (sq.in.)
Metered Volume,Vm (cu.ft.)
Average Meter Pressure (in.H2O)
Average Meter Temperature (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration (%v)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Pitot Constant
62.50
29.68
29.74
0.80
239.80
2016.00
30.87
0.91
61.54
265.40
6.17
12.85
80.98
1.00060
0.84
Average sampling Rate (dscfm)
Standard Metered Volume,Vm(std) (dscf)
Standard Metered Volume,Vm(std) (dscm)
Standard Volume Water Vapor,Vw (scf)
Standard Volume Water Vapor,Vw (scm)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity,Vs (fpm)
Stack Gas Velocity,Vs (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate C02
0.50
31.09
0.880
12.51
0.354
28.70
0.713
29.50
26.20
4435.20
1351.85
62092.73
1758.466
33187.04
939.857
105.42
150.38
1.305
16.02
-------
FACILITY : Mathy #6
DATE: 9-20-91
LOCATION: STACK
RUN NUMBER: 2.00
SAMPLING PARAMETER
ALDEHYDE
Total Sampling Tine (min.)
Corrected Barometric Pressure (in. Hg)
Absolute Stack Pressure,Ps(in. Hg)
Stack Static Pressure (in. H2O)
Average Stack Temperature (deg. F)
Stack Area (sg.in.)
Metered Volume,Vm (cu.ft.)
Average Meter Pressure (in.H20)
Average Meter Temperature (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Pitot Constant
62.50
29.68
29.74
0.80
237.52
2016.00
28.98
0.86
51.74
264.50
6.63
12,36
81.01
1.00060
0.84
Average Sampling Rate (dscfm)
Standard Metered Volume»Vm(std) (dscf)
Standard Metered Volume,Vm(std) (dscm)
Standard Volume Water Vapor,Vw (scf)
standard Volume Water Vapor,Vw (son)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
wet Molecular Weight
Stack Gas Velocity,Vs (fpm)
Stack Gas Velocity,Vs (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acum)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
0.48
29.75
0.843
12.47
0.353
29.54
0.705
29.56
26.14
4446.63
1355.33
62252.76
1762.998
32987.84
934.216
101.48
136.68
1.288
16.23
-------
FACILITY : Mathy #6
DATE: 9-20-91
LOCATION: STACK
RUN NUMBER: 3.00
SAMPLING PARAMETER
ALDEHYDE
Total Sampling Time (min.)
Corrected Barometric Pressure (in. Hg)
Absolute Stack Pressure,Ps(in. Hg)
Stack Static Pressure (in. H2O)
Average Stack Temperature (deg. F)
Stack Area (sq.in.)
Metered Volume,Vm (cu.ft.)
Average Meter Pressure (in.H2O)
Average Meter Temperature (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Pitot Constant
62.50
29.68
29.74
0.80
233.74
2016.00
29.95
0.83
72.76
232.60
5.63
13.43
80.94
0.99980
0.84
Average Sampling Rate (dscfm)
Standard Metered Volume,Vm(std) (dscf)
Standard Metered Volume,Vm(std) (dscm)
Standard Volume Water Vapor,Vw (scf)
Standard Volume Water Vapor,Vw (scm)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Height
Wet Molecular Weight
Stack Gas Velocity,Vs (fpm)
Stack Gas Velocity,Vs (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
0.47
29.50
0.836
10.97
0.311
27.10
0.729
29.44
26.34
4208.00
1282.60
58912.05
1668.389
32474.95
919.691
102.23
168.84
1.327
15.75
-------
APPENDIX C.4
PAH
-------
FACILITY : Mathy #6
DATE: 9-19-91
LOCATION: STACK
RUN NUMBER: 1.00
SAMPLING PARAMETER
PAH
Total Sampling Time (min.)
Corrected Barometric Pressure (in. Hg)
Absolute Stack Pressure,PS(in. Hg)
Stack Static Pressure (in. H2O)
Average Stack Temperature (deg. F)
Stack Area (sq.in.)
Metered Volume,Vm (cu.ft.)
Average Meter Pressure (in.H2O)
Average Meter Temperature (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Pitot Constant
125.00
29.68
29.74
0.80
239.68
2016.00
63.59
0.96
53.86
523,
5,
14.,15.
80.23
0.99980
0.84
10
62
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Standard Metered Volume,Vm(std) (dscf)
Standard Metered Volume,Vm(std) (dscm)
Standard Volume Water Vap'or,Vw (scf)
Standard Volume Water Vapor,Vw (sen)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity,Vs (fpm)
Stack Gas Velocity,Vs (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
0.52
64.96
1.840
24.66
0.698
27.52
0.725
29.47
26.31
4505.27
1373.21
63073.77
1786.249
34274.71
970.660
106.64
200.80
1.201
17.40
-------
FACILITY :.Mathy #6
DATE: 9-19-91
LOCATION: STACK
RUN NUMBER: 2.00
SAMPLING PARAMETER PAH
Total Sampling Time (min.)
Corrected Barometric Pressure (in. Hg)
Absolute Stack Pressure,Ps(in. Hg)
Stack Static Pressure (in. H20)
Average stack Temperature (deg. F)
Stack Area (sq.in.)
Metered Volume,Vm (cu.ft.)
Average Meter Pressure (in.H2O)
Average Meter Temperature (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Pitot Constant
125.00
29.68
29.74
0.80
236.04
2016.00
61.61
0.86
64.84
518.80
5.78
12.53
81.69
0.99980
0.84
Average Sampling Rate (dscfm)
Standard Metered Volume,Vm(std) (dscf)
Standard Metered Volume,Vm(std) (dscm)
Standard Volume Water Vapor,Vw (scf)
Standard Volume Water Vapor,Vw (scm)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity,Vs (fpm)
Stack Gas Velocity,Vs (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate C02
0.49
61.61
1.745
24.46
0.693
28.42
0.716
29.43
26.18
4323.73
1317.87
60532.27
1714.274
32654.51
924.776
106.15
138.41
1.448
14.43
-------
FACILITY : Mathy #6
DATE: 9-20-91
LOCATION: STACK
RUN NUMBER: 3.00
SAMPLING PARAMETER
PAH
Total Sampling Tine (min.)
Corrected Barometric Pressure (in. Hg)
Absolute Stack Pressure,Ps(in. Hg)
Stack Static Pressure (in. H2O)
Average Stack Temperature (deg. F)
Stack Area (sq.in.)
Metered Volume,Vm (cu.ft.)
Average Meter Pressure (in.H2O)
Average Meter Temperature (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Pitot Constant
125.00
29.68
29.74
0.80
244.28
2016.00
58.63
0.82
63.40
486.50
5.40
14.27
80.33
0.99980
0.84
Average Sampling Rate (dscfm)
Standard Metered Volume,Vm(std) (dscf)
Standard Metered Volume,Vm(std) (dscm)
Standard volume Water Vapor,Vw (scf)
Standard Volume Water Vapor,Vv (scm)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity,Vs (fpm)
Stack Gas Velocity,Vs (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
0.47
58.79
1.665
22.94
0.650
28.07
0.719
29.43
26.23
4208.90
1282.87
58924.63
1668.746
31570.07
894.065
104.77
205.23
1.228
17.02
-------
APPENDIX D
GEM DATA
D.I CEM DAS Printouts
D.2 Stripchart Tracings
-------
APPENDIX D.I
CEM DAS PRINTOUTS
-------
W-19-1991
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RAD I AW CORPORATION
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CALIBRATION
09-20-1991 10:07:27
CAllSftftTICN FiLE NAIE =0:\CEHOATA\0920CALA.CAL
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-------
SADJftN CORPORATION
0920RUNI
Field Testing and Process EnffGtrring Dept.
Continuous ciissions Roniteri^ Diti
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Sate Printed = 09-20-1991 Current Tin = 10iOfl:59
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RADIAN CORPORATION 0920QCCX
Field Testing and Process En^Dtcnnq Dept.
Continuous Emissions
HflHTY 14
F'er'oried for: JtflTHY
Date Printed = 09-20-1991 Current Tii* = 12:3B:28
= D:\CENDflTA\09i091.?SN Calibration File:D:\CE!HWA\092CCAL.A.CAL
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-------
RADIAN CORPORATION
0920RUN3
Field Testing and Process Ejiginttfipg Dept,
Continuous Eiissions Honitorijif* Dvta
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09-20-1991 D2 THC
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Bt TYPE
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UiOTH
799963 .363
H€ICHT CAL* COHC, M4ME
32027 z lae.aaa ETHANE
TOTftL
786963
K RUN *
STHRT
1 sTop
IF
SEP 28. 1991 Q6i31i«9
RUN* 41 SEP 2Q, 1991 aS1 3 I '. 43
NO RUN PEAKS STORED
* ZERO BREAK
* LIST: ZERO - 8 , -'3.642
* PLOT
STOP
« LIST: ZERO = a. - 1.463
*flTT 2 "• BREflK
* LIST! ZERO = 8, -1.279
•* LISTi ZERO = 9, -1.067
» ZERO 1Q Q
* PLOT
STOP
" LlSTi ZERO • 19. -0.706
> PLOT
ZE= 10, -2.343
2E' 18. -8.t35
0, -1.651
" 5. -2.238
2E= 5, -3.494
5, -7.338
B, -7.997
STOP
* LISTi ZERO
e. -e.384
-------
PLOT
-rr*~
+P BREAK
»P
INVALID SYSTE«~COH«flND
STOP
-------
OP •' 5
POST-RUN LIST OPTIONS
Star* pott-run rtioori CY'N*]!
External pott~r«n rtPori
List run p«ri»«t»rt CV^K
Lift (intiabla (Y^H*3i N
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L i * i r«iion n • t h o a
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Skin p»r r or a i i on» in r-»pori
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STflRT
ivvt om
ZE» 5, -6,267
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1 .
3.178
3.
7.884
7.
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TIMETflBLE STOP
12.688
15, 148
16. B2-*
ID.963
1-'. 566
17.951
19.Q56
28.990
28.614
22.409
23.369
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428
656
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409
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TYPE
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BB
aa
BB
BB
BB
BB
VB
ea
PB
BB
BB
BB
BB
BB
PB
BB
BB
PB
PB
VB
PB
BB
AREA
1 676
1 41 244
263813
170303
4426
36497
8504
34667
34192
3876
3226
1004 I 3
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21934
2613
56B6I
27054
1 489
11710
386 J
13034
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11911
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1 43
13749
63267 Z
15931 3
2323
4695
1 392 4
4533
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373
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1763 6
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1 1 1
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381
392
1 90
234
247
057
469
042
263
934
NAME
ETHANE
PROPANE
BUTANE
PENTANE
BENZENE
HEXANE
TOLUENE
ETH-BENZENE
XYLENE
TOTftL flfiE*=1164256
CIUL FRCTQR= i.eaaeE
RUN PARAMETERS
ZESO = 5
ft T T 2 '-
CHT SP
H R ft E J
THRSH
PK UO
- 1
1 . u
e
i
t>. U8
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AV
* RUN N 43
STftRT
SEP 20, 1991
0.633
—a,
10.asa
STOP
16.345
16,966
RUN*
43
SEP 20. 1991 89130106
NORM-AREA
RT TfPE
.637 BB
.835 BB
2.113 BB
AREA U10TH
28339 .83?
131776 .2B?
1332 .026
HEIGHT CftLt COHC. -NftNE
603S 1R .688 METHflHE
76** 2 1.969 ETHANE
96S 3 .019 PROPANE
-------
TOTAL WRES-2.3239E+07
MUL FflCTOR=i,
RUN PflRflHETERS
2ERO
ftTT 2' =
C H T S P -
ft R R E J =
THRSH
PK UD =
-------
* USTt 2IRO - 3. -19.875
'ZERO ia a
+ LIST! ZERO - 10, -10.676
* RUN *
STflRt
SEP 28» 1991 09:52120
ZE- 18. 4,968
a.544
i. 766
1.638
2. 129
10.
11 . 1 3«
I I .
15.092
S3.93t
16.45?
16.932
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TinETflBLE STOP
22.813
23.993
24.238
24 . 9 18
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SEP aa.
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544
766
119
331
630
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156
386
620
924
136
936
930
332
01 3
983
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310
TYPE
BB
BB
BB
BB
Be
BB
ee
BB
Be
BB
BB
PB
B6
ve
PB
VB
PB
I BP
AREA
3964 1 3
937423
29945
225377
49394
342
46154
14482
106376
922 1 7
27930
17912
59229
17464
1219
52476
630
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. 265
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25069
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2113 &
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27. 365
NAME
ETHflHE
PROPANE
BUTANE
PEHTANE
BENZENE
HEXRNE
TOLUENE
ETH-BEN2ENE
XYLENE
TOTflL MREA=2537798
MUL FflCTOR-i.aeeeE+ee
RUN PARAMETERS
£ E R 0 • 18.-
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0
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SEP 28 , 199 1 I 8:25:8i
1 . due
1.839
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3. 59Q
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1 1 , i E 5
11 . 3 7 5
ID. 1 4iS
16. ii 3
17.315
19.934
-------
TIMETABLE STOP
RUN
SEP 20. 1991 1B«25'32
MORM-flREft
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763
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294
393
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6E
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BB
PB
PB
PB
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rtRE A
412519
186393
197526
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4426
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65906
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15-582
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36.967
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2 7.986
26.974
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5.325
4 .266
7 .466
1.425
6 .163
9 . 826
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1.164
1.963
10 .063
NAME
METHANE
ETHANE
PRDPMNE
BUTANE
BENZENE
HEXfiNE
TOLUENE
ETH-BEHZEHE
X ¥ L E N E
TOTnL HKtM=li874?6
M U L F HI C T 0 p. = 1 . B U @ a E *• U »
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-------
• RUN • 46
START
SEP 28. 1991 18:55:34
"tf-
0 , 5 i ?
a . ? 5 e
1 . S8 6
2: . •» 9 B
i.S?^
3 . a 5 6
3. 5?0
11.063
11.955
15. > i e
ID. 3 i o
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T I Hk T HB i* i
46
AREA
ft T TYPE
517 66
756 BB
655 BB
273 BB
33S BB
45i 66
375 BB
69 1 66
5 7 & V B
979 BB
£1 6 -3- B B
955 B B
323 VB
& 4 2 V B
522 I BP
AFcEM = 2 18J3i
HCTOR=l.lieSk
ft P. H METERS
10
" = - 1
P - 1.0
J = y
= 1
= y . aa
t s i y t^
SEP 23, 1591 13:55:34
AREA UIDTH HEIGHT CAL» COHC. NflHE
657183 ,£62 4435" 46.953
85796" .655 157369 £ 27.285 ETHANE
4 •'•} 5 1 B .123 * 6 3 7 3.335
55296 .037 24557 3.724
20424 .124 2751 3 .419 P R 0 P fl H E
1464 .152 154 . 595
i&576 .177 ! * -4 1 1.386
3 5 9 5 B .131 4530 2.422
55444 .213 44 & 5 4 .776 BUTANE
5654 .632 2951 ~ .643 BENZENE
5491 .115 799 6 .656 HEXANE
5 S 0 3 .134 493 .391
14, '2 55 1.138 2156 3 1.344 TOLUENE
11596 . 2 1 9 3 i I 1 13 .858 X V L E H E
173688 .198 14593 i 1.6 93
13,
-------
* RUNS 47 SEP 20. 1991
STrtRT
~tf-
3. 335
STGP
u
6, 633
RUN*
SEP 2
I 5 9 1 1 1 s 5 9 I 3 6
N U F: M - H R E H
RT TYPE
.633 B B
3.325 El 6
i a e 17 3
UIDTH HEIGHT CAL* CONC. NAME
.155 8505 1R 73.9£8
. U7 14247 4 26.832 BUTANE
TOTHL MK£.H= 17Z015
WUL
f:UN PARAMETERS
Z E F, 0 • 1 0
ATT i'- = - 1
C K T i P = 1 . e
HF; REJ - a
T H R S H = 1
pK UD = e.ee
-------
RUN i
START
48
SEP 20. 1991 11:43:45
STOP
0,656
RUN*
48
SEP aa, i99i 11143:45
N G ft M - M R E A
fi T T Y P E
.658 P B
UHOTH HEIGHT Cftl» CONC,
.94'S ?555 IK 1
NftME
METHANE
TOTAL ftftEH= 22»354
MUL FMCTOR»I.eeeee+ee
r UN P H ft H M E T E P. S
ZERO = 1 6
C H T S P = 1.0
H S: r, E .1 • d
T H P s H = 1
P K LJ 0 = 8.8
-------
* RUN *
STwRT
49
SEP 28, 1991 I 1 M7s 14
-ff-
STOP
RUN* 43
EP 2%r 1991
ft T T V P E
,649 P B
,792 BB
\ . 26£l I BP
iREA UIDTH HE14HT CH!_» CONC. NftflE
j *? 2 7 .093 35IS 1R o3.63e METHftNE
94'? .061 196 2 .546 ETHANE
il82 .730 i I 8 2 3 35.774 PP. OPrtNE
TuTnL MRE«= 142378
MUL FH
F, U H P M F H M E T E R S
Z E r, 0 = I U
HIT 2'- = - 1
CHT SP = 1.8
H R R E J = 0
T H P. S H = 1
F K U 0 * 9 . 0 3
-------
*• RUN • 56
'-. T in R T
SEP 20, 1991 M:5l!t8
1 , S5Q
i. 2.3 a
i. a 6 >
3 , 1 o 0
.3,
3 . j
1 1 .882
U . 9 b 8
15.335
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1 1 .
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15.
1 6.
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1 t piE 1 HBI.E a i\>r
50 S E P 2 8 F 1 9 9 1
i 1 : 5 1 : 1 8
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fiT
665
744
650
69?
865
188
325
568
-5>9e
958
832
963
-335
773
79'*
T V P E
P6
BB
BB
BB
BB
BB
BB
BB
PB
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PB
PB
BB
BB
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AREfi
241318
269 S 52
2 1 '1 3 6 7
[ £ 9 6
1 1 7 3 1
3 £i 3 1 9
7211
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PlETHHNE
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BUTflHE
PENTfiNE
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ZERO
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10
= - 1
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* EDIT CHL1B 8
i = C-ALIB PROCEDURE
i = RETENTION TIME UIMDOU:
3 = TABLE ENTRIES
<» = PEAK GROUPS
•5 = C A L I B OPTIONS,
SECTION TO BE EDITED: 1
E = EXTERNAL STANDARD
i = INTEP.NHL STANDARD
H =• H 0 P. M fl L I u H T I 0 N
CALIB PftClCEDURE CE • I -- H * ] I E
SECTION TO BE EDITED:
<• RUN
START
51
SEP 20, 1991
1-p
.,-c,
l . 3 •>
6 . ')• 8 2
11. a 7 o
-------
16.
RUN*
5 I
SEP a Q , 1391 1 £:2 kiS6
ESTO-HREft
R T TYPE
,
,
1 .
2 .
2 _
3.
6.
1 1 .
S37
365
346
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643
325
9S3
a 76
PB
BB
BB
BB
SB
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ftPErt
492896
1 6Q444 2
1461865
5e0"3
14638
2877436
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2996469
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. 933
. 833
. 392
3.769
. 333
, 158
. 2-ei
, 222
HEIGHT (
S6622
196966
263483
243
•9 1 5
21-5717
£ 1 3 6 .' 3
2247-39
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2
3
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15.
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13.
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» RUN II
START
52 SEP 20 .
12! 46i 00
•~fP-
1.865
2E= 13, 2.767
16. 185
It, . 483
I 6 . '3 £ 3
-------
TIMETABLE STOP
R U H *
SEP 20, 1991 12:46:08
E'iTD-MREA
RT
, 523
. 658
.r~e
. "iZi
16.488
16.923
TYPE
PB
BB
Bi
BB
BB
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34638
41376
42942
1 "488
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3655
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8632
28563
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i R
2
3
3
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RUN F-MRrtPlETERS
ZERO
ATT 2" -
C H T S P =
ft F. ft £ J =
T H R S H =
P K y D =
-------
* RUN N
START
SEP 28. 1991 I 3: 14:55
-1-p-
-3.654
.-7.66!
1 t) . 0 j-*
1 i; .
1 5 . 3 1 i
15. -ta^t
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TIMETABLE STOP
aa.tta
RUN«
SEP 20. 1991 13114:33
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3,
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1 i .
fTsT
15,
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17 .
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23.
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956
061
034
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321
366
344
S23
332 I
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86
BB
PB
BB
BB
PB
PS
VB
PB
VP
«RErt WIDTH HEIGHT CfiL» COMC. SAME
22245264 4.617 88388 4 142.6^2 BUTANE
626136 .891 114878 3 3.383 PENTANE
2192330 .£11 166412 7 8, £73 BEH2EHE
Id23 . e/9 213 6 ,083 HEXfiNE
l 1 1 Z 6 1 J . ! B 3 r""l"7 5642 ;
12786 .324 634
•?383 .2o5 585 3
3 8 1 '? 1 •» 2 .371 171433 '?
23V 6 .142 272
545-J792 .839 183(873 13
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M F F E J
T H ft -;, h
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LIST: CnL I B
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F; E f "•; F, T U :
5 ,
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« EDIT C M L1 & 3
1 = LMLlEf PROCEDURE
2 = RETENTION TIME UINDOUS
3 = TMBLE ENTRIES
4 = PEAK GROUPS
5 • CALIB OPT 1 ONS
SECTION TO BE EDITED'- 3
C H L * : 3
R T: 5113.812
-------
H ^ rt E : TOLUENE
L rt L. » !
SECTION TO BE EDITED: :
+ RUN 9 54 SEP 29. 1991 13:46:54
> T M R 7
I. 3 j ?
RUH» 54 'iEP 23, 1991 13: *tl!54
ESTO-HP, EH
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.8 2-5 6£ 2"2? .323 197b .384
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T 0 T M L R R E M- 35^461
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T H F, i ri = 1
F K Ul 0 = 0 . f) "1
<^ r
-------
* PUN * 55
S 7 ft r: T
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SEP 20, 1991 1 3 s52:
Ifl .nil
RUN* 55
•.-; E P a a . i * 9 i 13152130
R T T V P E
. •» £ 1 6 B
H F; E A ID 1 D T H
3 H = 1
F• K y D = a. w 3
-------
<• EDIT CALIB @
1 = CALIB PROCEDURE
i = RETENTION TIME UINOOU3
3 « TABLE ENTRIES
-t = PEAK CROUPS
5 = CALIB OPTIONS
SECTION TO BE E&ITEQ: 1
E = EXTERNAL STANDARD
I « INTERNAL STANDARD
N = NORMALIZATION
C ft L I B PROCEDURE [ E » / I /• N ] : N
SECTION TO BE EDITED:
«- RUN » 5c SEP 2fl. I'SSl 13!33'.45
START
•» i g f
RUM* 5 i 3 E P 2 0 , 1 Si 9 1 1 j : 5 3 ; 4 5
N 0 R M - M R E M
RTT'r'PE AREA UIDTH HEIGHT CftLDCOHC. NAME
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. B4'ei BB 352075 .088 66563 1R 7j.3£6 NETHANI
1 BP _22ai99 .'330 9751 2 2 I . 8 I .' ETHANE
0 . i
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HUL FACTOR^i,ae00E«ae
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ZERO =• lu
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ftft REJ = 0
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-------
« EDIT CHL 16 il
1 = C AL 1 B PROCEDURE
2 = RETENTION TIME WINDOW'S
j = TABLE ENTRIES
4 = PEAK GROUPS
5 = C « L I B OPTIONS
SEC II ON TO BE EDITED: I
E = EXTERNAL 'STANDARD
I « INTERNAL STANDARD
II = NORMALIZATION
CALIB PROCEDURE C E-'1 •• N * ] : E
SECTION TO ee EOITEQ;
* RUN * "57
si AST
SEP 23.
1.01-4
1 . 3 1 •
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SEP 28- I'3 31
RT
. 5
-------
T H R 3 H • I
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* RUN* 59 SEP 26- 1991 1 4 : 8 5 ! 3 1
i T M R T
tf __.
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436
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382
059
256
295
732
1 53
BB
BB
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SPB
SPB
BB
PB
Be
PB
PB
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2589
239
3347253
6755779
1 0 4 2 9 Z 2 4
13799136
17335768
120419
994
13367
21668263
U IDTH
. 033
1 53
213
171
222
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177
146
637333
1 23-859
1773933
1452983
1435339
9632
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1 795
1 562767
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3
4
5
7
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, 872
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M E T H R H E
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P P. 0 P M N E
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TOTAL
-------
RUM FHRHHETERS
ZERO = iw
H T T 2 •" = - I
CHT iP « 1 . a
IH P. R E J = 0
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F K ui D = a, is a
-------
RUN »
START
SEP 20, 1991 14:21119
i, e 3 -a
k . 3 2 a
I . '•> j o
3 . J 7 5
3.63-3
7.
k o. a i
11.151
15.a 1 o
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T1METftiLE STOP
RUHK
5-9
SEP 28,
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2134524
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fi T T 2 "•
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* S)UN *
S T M R T
61
SEP 28, 1991 15:20:05
3,53,-
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1.312
1.916
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508
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86
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68
66
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3« 1424
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366085
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tiT T i - = - \
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F K ij D =
-------
r RUN K 6E
START
SEP
STOP
U N
i E P 28. 1551 1 3 : 5 e : 2 T
R T T Y f- E
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I BP
UilDTH
5 « 2 r " . 1 Q 7
1330285 . 71.T
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73-47 1 R 1 . 5 5 i H E T ri H H E
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ri fi. R t J -s y
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* P, lift *
T H R T
63
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SEP28,
15:53:5
0.6-43
RUN*
i E P 2u, 1991 15=53:53
R T T V P E
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1 1 D T H HEIGHT C M L » C 0 HC. HUME
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T H F, S H = \
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-------
RUN II 64
• T H F. T
STOP
SEP 28. 19 -51 15:56:87
-1-F
.654
RUN*
64
EP 28, 1591
ESTD-ftftEH
ftTT'r'PE
,is54 6B
MftEA ytDTH
34377-? .639
HEIGHT CALtlCOHC. HftME
oSoJl 1 R 13.330 METHftHE
T 0 T H L
HUL F
497 ,~ 9
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; E F. o =
HIT i"- =
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* F; U N
S T H ft T
65
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S E P i ft . 1 '3 '31 1 6 : 6 0 : i '
R T T V P E
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.655 66
H R E A U I C T H
731 .333
3 ? 1 €1 ~ '3 .893
HEIGHT C.AL» CONG.
393
66193 1 ft II. 45"
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R I j K F H ?,« M E T E ft S
IE r 0 = 1 Q
HIT i = - i
C H T S F = 1 . -j
H F: ft E J = u
T H F, 'I H = 1
F i. WO = -3 , 08
-------
* SUN 4
:. T H R T
SEP 26. 1991 1 6 •• 8 3 : 1
u . 5 3 3
U - c, 5 0
R U N #
SEP 2 a , 19-51 1 6 : a 3 : 1 y
E5TD-MF. EM
F; T T V P E
. iio5 6B
1 . Q c 1 i B P
7 •+ 2 1 9
l-tflio'J
U1DTH HE1C.HT CALK CONC. H H ft E
.126 'JS e I 1 R i . 29 2 tnE T H M II E
. 0 8 i Z 3 7 5 i 2 1 . ? 5 * E T H S M E
TOiinL MREM= 214333
M U L F H C T 0 R = 1 . 0 a t) 6 E -r Q 0
F U H FrtRrtflETEP.':
ZERO - ID
c ri ~ .; P = 1.5
h F: R E J = 0
T H R S h = i
F K LJ (j = 5.^
-------
Jk-
«... ... ,.„ ,..„.
.,
0 . j 1 3
STOP
Run*
RT TYPE
- 3 1 i 6 B
• o i -i 5 e
MIDTH
,155
HEIGHT
CONC.
> 5 ETHANE
• 3
f-'-IN
-1 r. >j- a v
"IT 2' = .,
HT SP = 1-
F. P.EJ » «
-------
c RUN * 68
5 T H R T
SEP 20, 1991 U: 1
i:Si8
RUN*
i E P
1991 t 6 : I £ : 8 12
, iTD-AREw
ft T T Y P E
.£56 PB
.SQO BB
1 . 0 'i 4 I B P
32873
3 6£
I -t 1 3 7 2
.448
HEIGHT C H L t» C 0 H C . H A PI E
7541 IF; .998 METHHHE
221 £ .912 ETHHHE
I 63 4 " S 1.SJ4
TOTnL MREri= 1 ~ 4 3 1 2
MUL FACTO F:=1.000aE»00
P U N F M F. H M E T E ft i
I E R 0 = i is
H T T 2 - ~ i
CHT 'i r = 1,0
H r; R E j = U
T H R S H .= I
P K u u = 13 , 6 8
-------
A'
* RUHtt 69
STnRT
S E P E 0 . t 9 9 i I 6 s I 4 : 4 7
STOP
9 . o 6 7
a, 91 5
RUN*
o 9
SEP
1 9 S I 1 <•> '• I 4 : 4 ?
ESTD-MP.EM
ft T T T P E
. 6 c 7 P B
.915 1 6 H
HftEfl U1IDTH
7258 .066
HEIGHT CHLfl CONC,
6335 1R
12/71 i
M M M E
.341 M E T H Hh E
: . 432 ETHftNE
TOTML
FACTO R=l.
R U H P A E H M E T E R 'i,
Z E r: 0 * t y
H T T 2 = - i
C K T S f - l . 0
H F, R E J = 6
7 n F. 'i H = 1
F K. LJ D = a . o 3
-------
RUH 4 7u
•i T H R T
STOP'
SEP 26. 1991
t?
0 . J -9'}
e. 3 -4 ?
RUN*
S E K 2 B , 1991
: I 6 = 3
fi 7 T V P E
^ 9 '5 B B
i>i5 BB
3 4 ' 6 &
H F: E ri UIIDTH
j j 6 1 9 7 .253
3L145 .«55
124252 .f> 4 7
HEIGHT CALItCGNL.
3 I j "i S 10.193
?559 1R .'362 METKMHE
3 2 u 1 2 1.731 E T H » 1 1 E
TOTflL SftEA= -4 3 3 S '? 4
H U L F H C T 0 R = 1 . 0 0 u y E •» « 0
r, U r I F H R H M E T E F: :i
ZERO = L fl
M T ? 2 " = - i
C H T S F = 1 . a
k R R E J = o
T M F; 'I H * 1
r (, U D = 0 . 0 i
-------
RUM*
T H R T
7 1
SEP 28, 1 9 9 1 16:22:22
ZE= la,
-^ r
0.
1 u - •} i .a
15.
1 13 .
-------
TIMETABLE STOP
RUM It
7 I
SEP 20,
16:22 :
E3TD
1 V
15
1 6
1 6
17
2^
22
2 ~i
-rfRE*
P,T
. €5£
. 823
. uiu
. o 7 w
.357
. 3 7 2
.291
.155
.131
4
T V p E
6B
PB
BE
&B
PB
VB
VB
PB
id
H R E H
5 4 "1 7
24 & 1866
7 A 3 7 1
. 3 tf 2 3 W
49355
5 3-3'33 9 2
2977
5416730
WIDTH HEIGHT CwL* COHC. NAME
.893 5 3'5 1 R .170 METHnHE
. 2 1 i [ 3 5 4'? & 7 3.443 BENZENE
227755 2.373
737 3 .262 TOLUENE
1 3 £l 7 1.524
1 bo. 679
9 .192 ETH-BEHZENE
654
455
371
5 19
3S-2
6 3 i
242443
! 377
1 3 o
12.323 X V u E N E
TOTrtL MREM=l.j425E»
M LI L F M C T 0 fi: = 1 . Q M 0 0 E *
RUN F H f. A !1 E T E P.
ZERO = 10
H T T 2 " =
C H T i F =
H F, F: £ J =
T H R •< H =
F' f, ul u =
-------
L. I i T : ,; ,* L : B
E i Tu
rEF ". F 7 i
L E V Ei_: 1
Cr. L »
IF
f T
0.6:
1 , •» i 0
•i it. = 4 i
f i 3 . 0 5 r
•J 1 \ . 2 i -i
t. • l i - '•! E
L -HETn-riE
i E Tn~ aE
: - ~ I- *• M "• t
«j a u n 0 H - P E F ', P. T Ul : - 5 . o 0 e
f. CCHLlBKH?IuM?: 1
L v « N r p, n T H r E n
1 I . 4 ^ O 0 E-u I I,i?ji£-q5
i i . -i 2 "3 y E - y i 5 , -i 0 2 6 E - >a i
i i.-iiyijE-Oi is.4i;^E-Od
1 i , 4 j. o C' E * 9 1 j , J o •£ j E - 0 '.
I , 4 j 0 0 E ' j i 4.i35?t-0>i
i ; . r 7- y C' E - 0 i : , i • ' C" E - 0 •=
i r1 . i i d 'j E ' o 0 i , 5 i i A £ - rj ^
i J. . 0 .; o >J t - ti 1 2 . } :, •-. 0 £ - >J «•
- ^ ! - C '• C.
-. ^ ,• c. r < i.
« ™-Z£ .^£-,£
•.. r', r T u e- a i 11 , . MO
»J i' 0 '.< E
I . 0 £ v fcj E • i
j E r i j - 1 r j 1 I "i -' l o : 4 19
-------
7, lit
11. 189
-17.931
2-* , 5 1 £
TIMETABLE 'iTQP
F; J N fl
72.
SEP 2B,
1 6: 5(3 i 46
EiTO
1
J
4
4
7
1 1
^ p
-AREA
RT T
. 645
. 3 15
. 3 o 5
. 3sfc
. 47 1
.765
. a.58
.189
. 2 3 1
VPE
?'B
BB
BB
66
BB
BB
BB
BB
E&
AREA
45256 1
1 ti6B457
i 4 5 a a 6 3
i 175754
56062
136121
2371776
2996 1 44
463
WIDTH
. 373
. 036
.094
.166
1.395
i . iea
. 281
, 221
. S23
HEliiHT
•36344
193353
239336
£185-32
4 3 3
^9 13
212937
£25434
C A Lit
1R
2
3
4
COHC.
I . 3 . 97 3
13.534
13
13.
1,
3
13
13
717
553
731
746
904
922
,984
NAME
METHnNE
ETHANE
PROPrtME
BUTftNE
PENTMHE
HEXANE
-TOLUENE
-------
* L I 3 Ti LIST
PERK CAPflCITYl 1221
ZERO
BTT 2" -
CHT 3P -
fift REJ -
THU2H =
PK mo «
i a, -1 a.aaa
-1
i. a
a
i
0. pa
LIST: THBSH
L I J T; CH LIS
EiTO
REF \ RTUi
LEVELi I
3.930 NQH-REF -. RTU: -5.393
REC«LIBRfiTI
r,L»
i P
s
3
4
5
1
™
9
1
1 «
nL«
1
e.
s
-1
^
o
T
f
'•y
i
P T L V ft PI T
a. »5 i i i . 59eeE*e i
3,3-tr ; i . 4 5 e o E - a i
l.-ljo 1 [.4£OdE->-01
i . ^4 1 1 1 . 4630E<-9 1
p , 5 j 6 1 1 I 4 o 3 8 E - 0 1
; ; . j i T i i . 4 •; t> e E » o i
5 . •j'iS'B J 1 . 9900E*-0 1
L6.?«7 1 ».obQ9E+39
2o.ii?^ i :.oebOE*oi
i J . i ,1 -9 1 i . 1 0 3 S E » a I
H n 11 E
METHANE
ETHHHE
P R Q P H N E
6 U T H N E
P E N T rt H E
H E X ft H E
BENZENE
TOLUENE
E7H-BENZENE
Pi I1) T -' A R E A
3. 93~bE-85
i . 39t3E-93
9. 4a26E-6e>
•., 4 1 12E-96
5 , 4065E -9o
4.5535E-86
j, >35i3E-6b
9. 632eE-<36
i . JS30E-e6
£ . 2739E-96
6-3
-------
-------
A
£ £ p i a _ 1 •? 9 I 9 2 ! 2 £ ! 2 t
i.
-------
>'
985
:»9 i
ORE :"> •'.
i .
I .
2 .
^ .
2 .
3 .
'i .
7 .
10 .
! 3 .
1 1 ,
1 I .
I 2.
I J .
i e ,
i~ .
i 7.
1 3 .
19.
20.
2 1 .
22.
23.
23,
£3.
23.
24.
ft T
Q30
56?
307
i73
696
739
>3u2
I 23
725
2 !5
765
9 32
151
92 1
933
223
369
249
040
1352
c7e
49 I
•33a
652
524
1 65
090
336
453
510
864
r, D £ ft
31-33
3-t S7&9
16-4 1332
395 5992
1415453
669444
1191951
4 y 2 2 7 4
5206699
1522621
2807376
5-45
76506
8645
6709
93043
160
1 466841
2607234
1193524
93938
2168547
25599
910106
249
483
537
10702
3843
27330
931
Type
69
EP
P V
VV
V V
V V
V V
VV
VV
VV
ve
BB
BV
VV
VV
VP
PB
PV
VV
VV
VV
VV
VV
VP
BB
PB
BV
VV
VV
. VB
PV
i! ! D T H
. 021
• .279
. 172
. 526
. 238
. L09
. 204
.071
. 930
. 396
. 663
.011
.312
. 120
. 074
. 769
. 029
. 854
I . 423
.772
, 073
1.394
. 051
.913
.614
. 037
. 030
. 173
. 038
. 362
. 109
A RE ft*
- .01131
3 . 058 1 2
5.92958
14.27993
5 . 11194
2.33521
4 . 30476
I .45292
13.30195
5. 49901
7.23149
.90197
. 27630
.03194
,02423
. 34325
, 00058
5. 36976
9,41609
4 . 32859
• .33926
7.93176
.09243
2, 92572
. 00090
.00174
.00194
. 83994
.01388
. 69870
. 90336
-------
+ R U H K
S T ft R T
•SEP 19. 1991 e
-------
STOP
5:1??
R U H «
1 4
SEP 19. 1991 09:04:11
ft R E H '-:
4 .
4 .
9 .
I 2.
1 2.
1 '3 .
i 5 .
13.
1 '?.
1 -J-
20.
20.
26 .
26.
P. T
1333
K* 4 g
7 ) 4
9Q4
4 15
965
475
633
833
733
9 i l
55B
b 9 7
343
993
rt R E ft TYPE
1£!7 BP
3 7 5 4 9 S V V
8464 352
27681
3722
-55 37Q
665325
76ia6 1 23
152.343S
42222
298225
2 3 7 2 Z
27843
•3 7 8 3
23239
VB
BB
BB
PV
V V
vv
vv
V V
V V
vv
vv
vv
VB
UIOTH
.31?
2.913
. 063
1 . 429
. 3we
. 029
. 272
. 462
3 . (374
1.148
. 332
.641
, 163
. 122
. Q3l
.329
(t R E ft y.
48.67229
I . 02235
23.04546
. a~s i s
.61013
. 85630
1.64863
36. 70332
4 . 14791
. 1 H36
- 3 1 1 96
,06459
.97362
. 32665
. 37633
TOTAL «REfl'3.S721JE*i37
MUL FH
* RUN i
S T M R T
- —ij-. g 3 4 F
SEP 19, 1991 0f!3S:35
-------
STOP
RUN*
A R £ A'/.
15
SEP 19. 1991 09138=35
RT
.630
.570
.660
.751
ftREft TYPE UIDTH
376? 88 , 6 2 3
649 B B .039
2165 8P .059
17439 P B ,226
15, 65019
2,69630
3.39463
72.63991
TOTAL f< P, E 0 =
MUL FACTOR-i.08806*98
f RUN • 16
STSRT
2.639
SEP 19. 1991 8-5= 4 9: 42
P. U M #
SEP 19, 19 91
= 49:43
ft R e A v.
,
2
2 »
*j
RT
936
667
•a 39
240
335
AREA
2149
2067 12
1 3358 1 6
253836
997336
TYPE
BP
PV
vv
vv
VB
WIDTH
.018
. 384
1 . 247
.253
.679
6 .
5o .
ie.
£6 .
AREAX
86426
19193
36536
55635
3333 1
TOTAL HR£ft=-3344299
MUL FflCTOR»l.
RUN *
17
SEP 19, 1991 if:59:
START
"p9T"B;
-------
STOP
"3. 383
3:
RUN*
RT
. 931
3.335
1.684
3 . 869
TOTni.
SEP 19. 1991 09i39'26
SREA TYPE ylOTH
253 BB .083
6505661 6V 1.798
474363 VV , 133
367732-'' W 2.287
aaaie+aa
.80168
43.2822?
3. 1334?
53. 6426 1
* L I 'a T ; C M L I B
HO CH L I 6 T 5 L
* RUN * is
-I;
•3-335
4:211
4. 629
4. see
SEP 19, 1991 !8i28 = 81
r' 8 . a i 3
"' 1 . 4 4 a
-------
10 . 148
STOP
~J 1 1 . 2 7
R U H H
L9
SEP 19, 1931 10 s 28 : 01
M R E IH ;:
.
I .
£ .
2.
2.
2.
i .
"i .
4 .
4 .
4 .
4 .
7.
3.
9.
i a.
i i .
RT
639
866'
446
4 1 4
565
635
396
438
335
1 36
23i
626
960
175
35 1
126
148
274
rtREA T'
531434
1657679
1532790
1 605
451
5 i I
599
217533 7
3422 '?
7 ?49
3 U94
12116
54999
2792862
14764
J0S3272
63704
3266534
r'PE
BV
VB
ee
ee
6P
P6
P6
BV
V V
VV
VV
VV
VB
66
VV
V V
VP
pp
U I DTH
.998
. 098
. 1 04
. 050
.041
. 064
. 033
.161
.343
. 03 1
. 3dd
. 1 '33
.330
. 291
.195
. 3S7
. 343
. 220
fiftEM*
3 . 6 6 1 Q 4
7.28633
Id. 55937
.09692
.00311
. 00335
.06413
14.98621
.23580
.05476
. 2142S
. 0 S 3 4 7
.37889
13.61999
. i e i ~ i
21.24862
. 47330
22.03976
TOTAL nf, EH=l.-»5115E'-ia.r
Mut_ FH
PREP CHLIB
E = EX'TERHnL
I ~ INTEftllrtL STHHOflRD
M = NORMALIZATION
CHL;B PROCEDURE tE*/i
REF ;; RTU
NOH-REF '.'.
C 3.090]:
RTU C 3.060]:
PF BMSEQ ON AREfl OR HEIGHT C A * /• H ] :
CALK PT ANT
I :.6'39aSJ»-.689
; 15.e
2 : -,363 : 1 4 . 5
3 s-1.44 :14.2
4 ! -3 . 43 NO mflTCH
4 :-3.438 :l4.b
5 =-7.175 i I 4 . 6
6 : I 1 . 2741flaail-1 1 . 274
: 14.5
i METHftNE
s ETHHNE
:PROPrtNE
:BUTANE
:PENTflNE
iHEIEXANE
CROUP PEflKS
-------
'_HLiO*HlIun 'jr lian
RF 01' j rvi a I ; o r » - • a
R • P I a c • calibration f i -. [ Y / N • ] :
Disable nail-run R T uociate t Y .•' H * ]
SAMPLE PiMT C9.0000E*99 ]= 1511
MUL
* RUN »
S T ft R r
SEP 19p 1991
ifl. 5
O . 766
2 . 'i 3 £
3.15-4
3.397
3. 62y
—7.791
~6 .Q 5 7
8.975
9 . -4 e 3
9 . 6 2 S
11.Hi
11.155
1 1 .
15.771
1 f> . 4 3 4
u. ase
17.823
16 .
19. 637
21.419
-------
STOP
—25.33:
RUN*
SEP 19, 1991 I 0!5?s 06
R T TYPE
3 . f> 2. 6 V B
II . I 3 5 V V
AREA WIDTH
653984 .549
23 2 1 5 .223
HEIGHT CftLtt COHC. NAmE
1-3899 4fi 1.-4S3 BUTflNE
2112 oR .156 HEX. SHE
TOTflL rtR
MUL Frt
f LlbT: TIME S
Cl . a 0 8 INTQ » = 8
30.006 STOP
RUN »
T ft P T
a i
SEP 19, 1591 11:26:18
3.
4 . 4 7
-------
13.
16.66?
II;III
iTOP
14.9^4
fc U H #
SEP 19. 1991 1 L : 23: 16
tSTD-HREM
R T T V P E
.396 V V
WIDTH HEIGHT C ft L « COHC, HHFIE
.£24 139993 2f> 25.342 ETHflME
TOTHL
n 'j L F
=l . 2496E*69
-------
1 - Cfl!_ I 9 PROCEDURE
£ = RETENTION TIDE UINDOUS
3 = TABLE ENTRIES
« = PEAK CROUPS
5 = CflL IS OPT I ONS
SECTIQN TO BE EDITED: 3 .
CHL »: ?
P, T : 9 . 9 2 b
ft M T s 19.9
B M T *• A R E H :
SECTION TO BE EDITED'• 1
E = EXTERNAL S T M ND fl R D
1 = INTERNAL STANDARD
H * H 0 R M ft U 1 2 H T 1 0 N
CHLIB PROCEDURE CE*/I/NJ=
SECTION TO BE EDITED: 2
R E F ''. RTU C 5 . Q a 0 ] :
HON-REF !-: RTU [ 5.356]!
SECTION TO BE ED1TEO: 5
CALIBRATION OPTIONS
P, F of 'j n c a 1 i b r a t. e d P e- a k i [ 2 . ? 3 0 9 E - 3 5 ]
R e D I » c + ii a 1 i b r a t i o n t i \. L Y ,-M * ] :
D i 5 i b 1 » P o •» i. - r 'j n R T u P d a i * C V / H * ] :
SAMPLE H n T C0.30Q8£ + diO 3 :
n 0 L r A C T 0 F: C l . -3 -5 13 y E * 0 9 1 :
SECTION TO BE EDITED: 3
C K L » : 7
ftf: -9.926
M H T : 19.9
fiMT /AREH : 3 . 36E-96
BEHENElfllZENE
C (H L * > 3
ftT : -14.924
A n T : 20.8
(HMT.-HREft! 2.95E-06
N A ri E : TOLUENE
RT : -17.717
29 . 9
N ft M E i ETH-BENZEHE
CAL«: 1 0
RT: 22Hfl~22 . 3^811
H II T : 2 i . 1
AI-1T /ftREH : 1 , 1 8E-06
X'fLENE
-------
SECTION TO BE E 0 I T E D ;
RUN » 22 SEP
STfiRT
1991 12:89:33
L . 825
-3.a 1 5
mill
1 b . 5 2 3
16. &:3?
-------
STOP
RUN! 22 S E P 1 9 - 1991 1 2 > 6 9 : 5 3
ESTD-HREfl
RTTYPE flREfl WIDTH HEIGHT CfiLHCONC. NAME
.696 VV 3136,06 .939 83110 1R 3.852 METHANE
16.337 VV 3637S2 .927 19417 9R 2.8H ETH-BENZENE
21. Oil VP 30419 .231 2191 1 a P. .03o XYLENE
TOTAL fiREA = 1 , I 5 15E + 87
MuL FMCTi;iR=i
« RUN* 23 SEP 19. 1991 13!00:24
START
-0.691
1.326
6.364
•si .992
STOP
q. 1441
-------
Q - 1 J
3
6
9
1 1
~ r» W C rt
RT 1
.631
. S 17
. do-)
.892
.065
1 VPE
PB
PV
VV
BV
VV
x)RE.4
2784i
475
443 =
23334
49778
'J ! 0 r H
.353
. a 7 2
. 073
. 252
.364
HEIGHT C a i. * '-
3435
i 19
1660
1576
22 a a
1R
4 P.
5R
7R
6R
0 N C .
. ass
.924
.aas
NrtrtE
NtTHHNE
BUTrtHE
PENTANE
BENZENE
H E X M H E
T 0 T H L H R E fl • 5 "9 5 7 0 2
MUL
L I i T : C (4 L I B
E3TD
REF '/.
L E V E L
CHL4
1 R
2ft
3R
4R
5R
BR
7P;
eft
?P.
l VJ R
C M L tt
1
i
3
4
5
*2
™
3
*•>
l f>
P. T U : 5 . 0 8 6
: I
P, T L V
u . 6 3 '5 I
y . 8 o 6 I
I . 4 4 0 I
3.493 I
7.175 I
11.374 1
9.926 1
14 . 9 2 4 1
17.717 1
22.391 1
H A H E
fl E 7 H H N E
i T H H H E
PROPANE
BUTflHE
P E N T M H E
H E X A H E
BENZENE
TOLUENE
ETH-BEN2EHE
X V L E H E
H 0 N - R E F *: R T hi : 5.89
RECflLlBRAT IONS: 1
ft M T H 11 T '• A P. E A
1 , 3 6 8 y E - 6 1 2.322oE-65
I ,450eiE*vjl 1 . 3783E-IS5
l.^SySE*1?! 3,;'i42E-0e!
i , 4690E*ia 1 6.711 -tE-96
1 , 4 6 a 0 E » 6 1 5.49I7E-66
l.43dflE+81 4,322aE-a6
L.9900E+01 3.S600E-06
2',96aeE*8[ 2.85aaE-as
2.0'5eeE-t-Sl 2 . 6 -5 ft & E - 0 4
2.118ISE*yl i . I 9 8 e E - 9 6
IQN OPTIONS
RF or uricalibrtttd P «a k 4
Cilibrakion fit
Disabl* coil-run RT
i M M P L £ A in T
MUL F M C T 0R
2.
P
NO
a,
* RUN
5 T H R T
SEP 19, 1991
1 . 345
-------
6. 945
8 . 1 28
11.815
t 1 .798
12,125
STOP
RUN*
SEP 13. 1991 1 3 : 2 2 « 2 5
ESTO-HREfl
R T TYPE
o.?45 BB
11.615 V B
AREft yiDTH
55*6552 .201
3873397 .223
HEIGHT CAL» CONC. HfiWE
215249 5R 14,026 PEHTflME
22977? 6R 13.89B HESflNE
TOTflL MR
MUL
BREAK
t RUN » 23
START
SiP 19, 1991 13: 4 1 :06
6.525
Q. 742
1.333
1 . 255
1.358
3.625
3.587
-------
18.
11,668
Ml
1 & . b 1 6
RUN* £5 SEP 19, 1951 13:41:86
RT TYPE fifiEfl LltDTH HEIGHT CflL* tONC-
j.58/ VV 3369433 .453 123330 4ft ;2.5,14
16.672 BB 13904 .296 3W0 6P. .a^i HEXHrlE
i 2.5 6 ^ V 8 2356? ,261 1436 Iflft .0^7 XYLEHE
T.OTHL fiRErt-4. 1 939E
MUL
EDIT CfiLlB
-------
« • PEAK GROUPS
3 • CflL IB OPT IONS
SECTION TO 9E EDITED: 5
CALIBRATION OPTIONS
RF of uncslibrntd peaks C2 ,
Replace calibration fit C Y / N * 3 :
Disable po*i-run RT update C Y .• N * )
SAMPLE A PIT ce.eeaaE+aa ]:
MUL FflcroR ci.aeaaE+ae ]:
SECTION TO BE EDITED! 1
E = EXTERNAL STANDARD
I = INTERNAL STANDARD
N = NGRmAL IZwTION
CftLIB PROCEDURE C E * / I -• N ] i N
SECTION TO BE EOITED!
SEP 19. 1991 14: 1 1 ! 36
P,UN» 2b SEP 19. l?9l 14:11136
NO C A L I 6 PEAKS FOUND
H R E H ;-.
RT
. 2i"
.49?
1.093
AREA
422-322
435796
495652
T Y P E
BV
V V
VV
WIDTH
.164'
.161
. 294
AREA/;
3 1 . 22 1 96
32. 17227
3 6 . 6 0 S B 7
MUL FACTOR=l.000flE'-00
P.UM » 27 SEP 19, 1991
START
0.515
Q.?23
i . a i -3
3.222
3.444
-------
9.753
—1 2. £ I 5
13,5-39
15:6gg
16 . 154
17 . 340
1 & . 8 U 'i
IS, 675
19,2-31
-J . 7 ,- 1
4.u 33
STOP
R i J N ft
HOftPl-AREft
SEP 19, 1991 14:23=40
RT TYPE
.723 P V
3.444 V B
9,758
1 -5 . ri u 5
17, 349
24. e 35
BB
V V
V V
VP
22S4909
2759470
2 ri 5 Q 3
2024582
5 3 3 9 15 3
193128
y i DTH
. 153
,672
. ies
1.048 -
,511
.335
HE JCHT
232710
4206
32198
1 365&
3957
CrtLH COHC.
»ft 78. 706
4R 21.041
7R
3R
9R
1 WR
, 1 16
6. 555
1.315
. 266
M E T H M H E
B U T H M E
BEMZEKE
TOLUENE
ETH-BEHZENE
XYLEHE
TOTAL MftEft«2.'?723E*a7
MUL FACTOR=i,aae^Et00
-------
STOP
PLOT
STOP
SEP 19, 1991 13i 85: £.2
3 . 196
3 .133
2, 9 r a
-5.757
6.057
o. 777
1.773
1 Q . :3 7 5
10.341
11.742
It.14*
17.032
19. 18 1
IN
19. g{
21.981
-------
24 . j I <
STOP
RUN*
SEP 19, 1391 15:05:22
HOKH-AKEA
3,
••i ,
1 1 .
1 7 .
a i .
RT
7 i a
435
770
742
6 i 2
991
TYPE
V V
ye
BP
'•-' V
vv
vv
AREA
1412130
5 2 S 4 9 5
99501
223851
o 156963
15401976
y IDTH
. iee
,408
^37
.491
1 . 043
2. 1 38
HE
2 3
2
•3
12
IG
5 1
15
•37
7 -•
7S>
05
HT
2 I
95
32
6 ~i
39
30
CSL*
LR
4 P.
7R
isR
9P
IflR
CONC.
52.
4 ,
1 .
1 6.
23.
537
B/5
586
364
•?bl
956
HflME
M E T H fl H E
BUTAKE
BENZENE
H E X ft N E
ETH-8EN2EME
XYtENE
TOTAL AREfl=9.l366E+e7
MUL FrtCTOP-i
* RUN *
i T M & T
SEP
1991
15 s
: 0 1
c^'i
0. W 3 I
0.515
U. 728
1 . 2 i U
t. a i a
2 . J 7 3
-------
15.785
16.959
£1.338
24.293
T IMETflBLE STOP
RUN*
SEP 19- 1'?'?! I3i 36: 61
N U P, PI - H R E H
ftT TYPE
3.437
} . 7 4 7
li. '555
21.330
VB
66
VV
vv
HP,E« yiDTH HEIGHT
3966397 .383 91761
n i a a .834 438i
5118632 2.529 33732
,'52772 1.381 1015?
C 0 N C .
4 R o * . 3 4 5
7 R .062
9R 27.949
1QR
2.444
HUME
BUTANE '
BENZENE
ETH-8ENZENE
X. V L E H E
TOTAL
. 6686E+87
r «
-------
.333
4.594
STOP
I'.L_ I 0.348
RUN!
3 1
SEP 19, 1991 16:37:37
H F: E A '•',
.
\
/':
; i •
4.
U.
RT
u 30
627
7 9 1
3 1 3
2 29
"394
543
H P, E H
7fse8
5 3 7 -J 6~9)
i8b±LL2j
2152! 23
2 I 48(3
-isLJLiii2|
T V P E
BB
i '•/ B
| BB
] BB
BB
[ BB
U 1 OTH
. 0 9 4
. 684
. 692
. 357
. 69525
6 . 63975
1 3 . 302 18
19. 35435
26 . 762 10
33,52358
T i j T M L H K E H = 3 6 4 l 6 9 3
M U L F ti C T 0 F: = 1 . 0 U W 0 E * V 0
* R lj N
T M F: T
1391 16:47:14
-f-F-
0.
B.
.
4. >i a ri
4.554
a.
-------
'a l 'J P
BUNt
«1 ft E M V,
.
4 .
4 .
9 .
Q __
10.
i a .
i : .
1 4 .
15.
15.
1 7 .
19.
32.
3
RT
W56
537
63S
b'58
639
954
750
333
764
342
4 1 1
3 39
553
639
593
319
765 i
ARE*
23746
676261
63692
154703
14751843
5892682
31 8 i 6S5
(^4586 64>
1441
670
3161
' S "7 "s & fll •"3™"
_j^t:6d_l_£^
435849
636543
/^7T634TT;
794
<^7& 373972""
SEP
TYPE
BV
VP
PV
vv
vv
VB
BP
> PB
BB
BV
VP
> PV
V V
VB
> VB
66
> BV
19, 1991
L110TH
.872
. 253
. 848
. 832
3. 44e
1.465
.364
.213
.312
. 661
. 154
. 246
.411
. 633
.359
. 101
.694
16847:14
M K E K '/.
, 63939
1 , 12196
. 1 1296
.25664
24 . 472 1 a
9 . 77348
5. 14544
7.47947
. 38239
.001 1 I
. 88524
9 . 5883 1
.72304
1.15551
12.21540
.08132
27 . 99235
14 . aib
13:3*8
17.593
=19. S 1-5
22.705
TOTAL ftREfl-6.e288E+07
FfiCTOR=1 . 8098E* 80
-------
APPENDIX F
ANALYTICAL DATA
F.I PM/Metals
F.2 PM1D/CPM
F.3 Aldehydes
F.4 PAH
F.5 Sample Log
-------
APPENDIX F.I
PM/ METALS
-------
Run 9
/Ho
Client
Want .
Sample type
Technician
Sheet L_ of
Run 9
Sample
!D#
Sample
Vol.
Blank
Con.
(ml)
Tam
Weight
Hnal
Weight
Sample
Weight
Commenta
1SO.L,
n
LL\1
*&*
0,60^3-
400 V/
/a 3
5-03
if
-1L7
fefr
fcu*. ^
Method 5 Analysis Data Sheet
-------
JflN 30 '92 li:03 RflCIflN CORP PPK NC
P.S
ftttl
Cii*m
Warn .
Samel* ttp€
Run w
Simpto
ID*
Vol.
tmtt
Cflir.
(rrt)
(oi
Wajqltt
(01
10)
OCDflVflflfffB
ol
/
•HO
o'?
3 If 3
R
•w
i
Method E Anatymi Data Sheet
-------
M* 2.
JUT - Mffwlt;
cull* in »!*(
CM
Uter
1-10-010- 16*
1-10-010- IF*
1- IB-Q10- 18*
1-10-010 19.
'1-10-010-12*
'I- 10-010- IS*
'1-10-010- 14*
'1-10-010- IS*
>1-IO-Q10-20*-H
i- IO-OIO-2U-M
>1- 10-010-22*-!
1 10-010-
(«• ihan S Hi
ilGUUtriOIS:
Met 1/2
4-
f*-pU
Dncrlptlon
•6 • 1
» - 2*
M • 42
« - S9
N2& - 14
K26 - 10
H2* - S?
H2A - 66
••Hud fptka
Mthod tf»tk«-<**>
Hfthad 11*1*
ICS
m I)M dgttction li»it
*« 1 »•
ICAP | ICW
1
• 0.700 | 1.01
« 0,62? | 0,815
< 0.63J | 10.5
• 0.611 | 1.42
• 0,671 |< 0.112
« 0.634 | |,J2
< 0.451 | 1,66
< 0.631 | I. 11
1
41.01) U.21
30.41) n.M
1
1
< 0.616 |» 0.106
1
107I| 91.61
1
Be
ICAP
< 0.111
« a. 104
< 0.10S
f 0.105
< 0.112
< 0.106
< 0.105
< 0.103
83.41
91,4*
< 0.106
»?.4I
Df
ICAP
< 0.222
* 0,282
10. 1
* O.TW
< 0.224
* 0.2S4
* O.T16
« 0.210
W.H
as 51
i 0.212
1041
tf
1DU>
* O.B11
« l.W
11.0
1.M
< 0.671
* 1.26
' 1.07
* 1.H
«?.W
§6.5*
« 0.616
1001
Cu
ICAP
< 0.444
6.23
199
i,*2
< 0.447
* 1,07
2,8V
< 0.421
W.rt
7*,J1
* 0.424
9ft.4I
Nl
ICAP
1.2S
2.81
40. S
1.34
* 0.447
1,04
24,8
2.01
«.o*
B4.«
2.17
S7.1*
II
IMP
• 0.95S
2.1?
10.6
i.n
" B.1W
2.»
4,69
2.04
M.H
W.SI
• 0.572
1B21
C | M,
1CAP | US GF
• 77. S |- 0.375
* 59.0 (• 0.886
iei | 2*.s
• 73.1 | 1.66
• SO. 2 |< 0.115
• 64.9 |' 0.155
• n.l I 1,50
• 67.5 |- 0.*4»
1
78,2S| 8B.6X
Bft.SX) Ml. SI
1
1
i 11,8 |" 0.744
1
9».OS[ W.OX
1
Sb
ICAP
* .6?
« .57
« ,58
i .58
< .68
< .59
< .54
< 1-M
86,81
96.81
« 1.59
1091
S«
ICAP
< 1.78
* 1.67
« l.W
< 1.60
« 1.79
« 1,*9
< 1,68
i 1,68
8S.B
95.81
« 1.70
1061
TI
ICW
« 11.1
* 10.4
< 10,5
< 10.5
< 11.2
« 10.6
< 10.5
< 10.5
94.71
*?.5I
« 10.6
98.51
In
ICM>
* Z.24
16.1
245
11.4
i 1.68
14,4
24,1
* S.84
90.71
101X
< 1,59
1051
1
Al
MS CF
< 0.444
• 0.418
« 1.10
< o.4ai
€ 0.44V
< 0.42J
< 0.421
< 0.421
66.01
97.BI
< 0.424
1071
final
Vottoe
0.100
0.100
0,100
0.100
o.ioo
0.100
0.100
0.100
0.100
0.100
0,100
Initial
Voliae
0.5030
1.1615
0.9605
1.0191
0.4755
0.9246
LOOM
1.0161
0.100
0.100
0.8814
Digested
VOtw
0-4J1G
1.1115
0.9105
0.9691
0.42S5
a. a fu,
O.W69
0.966]
0.100
0.100
0.81*4
Inull (ug/l) I Final Ualiac (l> K Initial Voliae / Dljttted VoluM • lotil ug
-------
• 2,
T - AMtfllll; Front V2
lit In lotil 14,
UN
utxr
10-OIO-flli
10-010-021
10-OIO-QJa
10 010 «•
10 010-051
10 010 04.
10-010-07*
10 010-08*
13 010 09.-R
10-010- IOa-M
IO-010-lli-l
IO-OOJ-
S«^)le
D*icripiion
N26 - IS, 16, 1?
tat - ".12,11
H26 - S4.M.J6
N26 - 67,48.69
W • Z.I.*
M - Z5,Z6,?7
M - 41,14,4%
W - 40.61,42
Mlhad Spike
Method lfiUi-
MIlMd UK*
LCS
»»
ICAP
1.50
S.ll
7 4S
5.05
4.05
7.00
5.35
< 1.50
n.n
21. n
• 0.600
ion
Bl
ICAP
45 0
M.3
to. a
rv.a
i.ea
9.15
r.ta
V.SO
«1 41
VI, 01
• 0.100
Ol.tt
e<
ICM>
0.400
0.550
0,125
o,zn
0.210
o.»o
0.250
0.230
M.OX
95.21
« o.ioo
97. tl
Cd
ICAP
• i.ia
• Z.I5
1.10
i.TD
• 1.58
2.»1
* O.U
« 1.*I
IOOT
W.9I
« 0.200
IKK
Cr
IUP
• 24. S
* 101
105
27.8
• J,7B
* 7.75
• 1.20
• J-M
99. 61
W.4I
t 0.600
1001
Cu
ICAP
2.60
21,0
19.1
ir.o
< 1.00
« 1.00
< 1.00
« 1,00
01.51
V1.V1
i 0.400
W. 41
Mi
ICU>
55. J
&2.0
H.D
105
4,H
58.0
19, 0
*1.5
M.II
M.It
• 0.1M
97. II
Hi
ICAP
IS.]
1U
W.i
11,1
• J.M
*5.0
* 2,«]
« J.iC
» «
ion
' 0.100
ton
p
ICAP
11!
311
1QA
»0
75.0
75.0
75.0
n.o
m.n
PJ.IX
< 30.0
«-«
Pb
AAS CF
S.I]
Jl.O
28.3
16. S
• 1.7*
1.SZ
< 0.751
6,]5
ti, a
ion
< 0 100
1011
Sb
ICAP
v.u
15.1
11.0
9-58
13.6
U.I
12.1
12.1
ion
1001
< 1 50
lOVt
Sc
ICAP
(.00
.00
.00
.00
.00
.00
.00
,00
m.oi
w.ii
< 1.60
10AI
II
ICAP
25.0
25.0
ZS.B
25-0
25.0
«.o
25.0
25-0
1031
1001
< 10.0
m.5i
In
ICAP
69.5
24V
26B
Hi
21. A
23- B
15.4
15.0
1051
1041
2.41
1051
At
AAS Cf
16.1
21.5
20,2
27.0
< 1.00
< 1.00
< 1.00
• 1.00
87,41
95,41
< 0-*fl
91. 4*
Final
VDlUK
O.Z5Q
0.250
(LZSO
0.250
0.250
D.Z50
0.250
0.250
0.100
O.IOQ
0.1OO
54,0
•I thjn i llan the dtiicilon liaii.
ULATIOK;
I«pl< inull (to/L) I Miul Voli^n ID • 1oi*l ug
-------
APPENDIX F2
PM10/CPM
-------
Client
Plant .
Run * .
Data
Sample type
Technician _
Sham L
of
Run
Sample
ID0
Sample
Vol.
(mil
Blank
Con-.
(mlt
Tare
Weight
(g)
Rnal
Weight
Sample
Weight
Comments
/J
LU\3
33
0 ^.
re 3H
K
a
fof.t.gt?
ix
5
LLoS"
3
5
-------
Client ETPA
Plant
Run #£Lk
Date
?/
SampletvB.
±
Run #
Sample
ID*
Sample
vol.
(ml)
/Blank
Corr.
Tans
Weight
(g)
Fnal
Weight
Sample
Weight
(g)
Commerita
01
ID
ad
f m fO
oT
(Wo
0%
o
OS
1C
a
Method 5 Analysis Data Sheet
-------
Run it A?
Client
Rant
Data
/
Technician
Sample type
CYC
Sheet
of
Run
Sample
ID*
Sample
Vol.
(ml*
Blank
COIT.
Tare
Weight
Rnai
Weight
Sample
Weight
(g)
Comments
ere
etc
Alll
etc
02,24 /J
- 6 Id
*
.3
CrC
. ft
s
r*.
05
Method 5 Analysis Data Sheet
-------
APPENDIX F,3
ALDEHYDES
-------
Radian Work Order P1-09-010
Analytical Report
12/16/91
ENB
EMB
Radian Corporation
RTP,
Larry
NC
Ronasburg
Customer Work Identification Asphalt Test Site 6
Purchase Order Hunter 275-026-*fl-27
Contents:
1 Analytical Data Sanitary
2 Sanple History
3 Contents Sunroary
4 Motes and Definitions
Radian Analytical S«rvic«s
900 Perimeter Park
Hornsvi lie, NC 27560
919-481-0212
Client Services Coordinator: LRCMESBURG
Certified by:
-------
Analytical Data Sunmary
Page:
EHB
Radian Work Order;
P1-09-010
Method:Aldehydes, Hod T011, HPLC (1)
List:Cdrpendiun Method TO-11
SanpLe 10:
Factor;
Results in;
Matrix:
H6-091S-ALD-F"
B (12, 13)
5.4
Total ug
09*
Stack
M6-0919-ALD-1
(28, 29)
10
Total ug
1QA -
Stock
H6-0920-ALD-2
(44, 47)
10
Total ug
11A
Stack
M4-0920-ALD-J
163. 64)
10
Total ug
12A
Stack
Acetaldehyde
Acetone
Aceiophenone/o-Tolualdehyde
Aerolein
Beniaidehyde
Butyraldehyde/lsobutyraldehyde
Crotonaidehyde
2.5-Qimlhylbenzaldehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehyde
MISK/p-ToluaLdehyde
Methyl Ethyl Keton«
Propionaldehyde
Quinone
m-Tolualdehyde
Valeraldehyde
Result Det. Limit
NO 5.8
6640 T 7,3
NO 12
ND r.i
NO 11
ND 9.4
NO 0.4
ND 15
10.7 - i.fl
NO f1
ND 9.4
ND 9.1
ND 12
ND 9.4
ND ?,J
ND 9.4
ND rz
NO 9,1
Result Det. Limit
822
23700 T IMlII
HO an
NO 111!!!
199
47.0 • laiili
37.1 • lillii
ND pi
2950 9*3il;
40.7 • iHlll
ND lllll
wo
":.:^:;«::5S
N0
ND
ND 14*%!:;
48. B • 1»;»i?;
ND a|tU
ND tiiw
Result Det. Limit
-•-v.-y.-y.-y.-W
1040 128«>
11200 150313
MO 2|||I
MO llfll
198 2t;!S
ND 18^;:f:
29,5 • ial»:
ND 2ft|:,-:;
4470 9*!SK:
62.5 • 20*:s:l:
NO lalii
m lilil!
ND Z|||i
ND iaHlS
ND Ttll-i-?
27.0 • WPi'
ND Zllfe;
ND 18«-:- '
Result Det. Limit
1170 120
2570 ISO
NO 23
26.7 - 13
211 21
75.4 - 1» '
65.0 « IS'
ND 2*
2770 ~ 96 "
ND 20
ND 18
ND 18
ND 23
93.5 1* "
94.6 U
1040 IS
ND 23
56.9 • 1ft
ND Not detected at specified detection limit * Est. result less than 5 times detection limit
(1) For a detailed description of flags and technical terra In this report refer to Appendix A in this report.
-------
Analytical Data Sumary
Page:
EHB
Radian Work Order: P1-09-010
l
Method:Aldehydes. Mod T011, HPL
List :Compend!um Method TO- 11
Sanple ID:
Factor:
Results in:
v
Matrix:
Aoetaldehyde
Acetone
Acetophenone/o-Tolua Idehyde
Acrolein
Benzaldehyde
Butyra Idehyde/ I sobutyra Idehyde
Crotonaldehyde
2,5-Dimethylbenzaldehyde
Formaldehyde
Hexanal
[sophorone
Isovaleraldehyde
H 1 BK/p-Tolua Idehyde
Methyl Ethyl Ketone
Prop! ona Ldehyde
Ou i none
m- To I ua Idehyde
Val era Idehyde
C (1)
NETHQ
.54
Total
17A
DNPH
Result
0.66 *
1.74 »
ND
ND
NO
ND
ND
ND
1.06 •
ND
ND
3.68 •
ND
ND
ND
NO
ND
ND
0 BLANK
UB
Det. Limit
0.18
0.73
K2
6.71
T.1
0.9*
0.9*
t.3
&.48
f,l
ff.9*
0.94
&.9t -
ft.fS
0.94
1.2
0,98
METHOD SPIKE
1
X
ISA -
DNPH
Result Det. Limit
90 1II1I1
83 ilil
70 Q Illll
23 <5 Illl
119 Illl
NA Illl;
•,•:•:•:•:•:•::•••:•••
25 0 fyffjxJM:
as iiiii
87 iillli
117
91
NS
106 iSili
NA
107 Illl
W Q iilil
93 ^y:?:-;^:'"^
82 :li|l
Calibration
Check OC
\
%
19A
ACM
Result Det. Limit
1140 Illll
NS 1! 11
NS :li 11
NS m •;;!
UC "..'"".-:< -•*'.'-:-:-:'
H3 . .-I,:.- ";'.'-.;'•'.
106 ::|| II
NS .||;: 1;|
HS HI li
t f J v.;>:;': .•:::£'•:
W-j'S-iSS;;?:'
:-:-:v:Xs:--;;;:;:;
NS |-:|f !§|
NS 9 &Z
NS 1| 11 ' •
"S HI If
165 ° II 11
NS :ll!li
NS 3l|:
NS :li:^'i
Result Det. Limit
^
- «^
• Est. result less than 5 tinea detection Unit
Q Outs id* control limits
NS Not spiked
NO Hot detected at specified detection limit
NA Not analyzed
(1) For a detailed description of flags and technical terra in this report refer to Appendix A in this report.
-------
History
Page:20
EHB
Radian Uorlc Order: Pl-09-010
Sample identifications and Dates
Sample ID H6-0920-ALD-2 M6-0920-ALD-3 METHOD BLANC MET HOC SPIKE METHOD BLANK METHOD SPIKE
(46, 47) (63, «)
Date Sampled 09/20/91 09/20/97
Date Received 09/23/91 09/23/91 09/23/91 09/23/91 09/23/91 09/23/91
Ham* Stack Stack XAD-2/ffr XAD-2/FI ONPH ONPH
11 12 15 16 17 18
Swa270- Semi -Volati Les
Prepared
Analyzed
Analyst
File ID
Blank ID
Instrunent
Report as
Aldehydes, Mod T011, HPLC
Prepared
Analyzed
Analyst
File ID
Blank ID
Instrument
Report as
09/30/91
10/18/91
LKK
09/30/91
10/18/91
LKK
OWEN 127/1 74 CVEN126/173
LLHA75
V5000
received
LLUA7S
V5000
received
09/30/91
11/04/91
RK
45B6532.TI
45B6532.TI
GC/HS B
received
10/11/91
11/05/91
RK
45B6534.TI
45B6533.T!
GC/HS B
received
09/30/91
10/04/91
LKK
LLWA75
LtyATS
V5000
received
09/30/91
10/M/91 '"
LKK
LLWA76
LLWA75
V5000
rec« i v«d
-------
ENB
Radian Work Order: PI-09-010
Sanple History
Page:21
Identifications and Date*
Sample 10
Date
Date Received
Matrix
Calibration
Check QC
ov/u/91
ACN
19
Aldehydes, Hod T011, HPLC
Prepared
Analyzed
Analyst
File ID
Blank ID
Instrument
Report as
10/18/91
LUC
OWEN 124
V5000
received
-------
Appendix A
Garments, Motes and Definitions
-------
EHB
Radian Work Order: PI-09-010
Report Canneries and Narrative
Page: A-i
General Cornnents
Aldehyde Data: Y - Outside, of calibration curve.
0 - Spike recovery OC limits range 'ram 80 to 120 percent.
Calibration check OC limits range from 85 to 115 percent,
HA - The butyraldetiydes and HEK eoeluted.
-------
Motes and Qefinicions Page: A-
EHB
Radian work Ord«r: Pl-0°-010
B This flag indicates that the analyse was detected in the reagent blank
but the sanple results are not corrected for the amount in the blank.
J Indicates an estimated value for GC/HS data. This flag is used either
when estimating a concentration for tentatively identified corrpotnds
where a response factor of 1 is assured, or when the mass spectral
data indicate the presence of a compound that meets the identification
criteria but the result is less than the sample quantitat ion limit.
NA This analyte was not analyzed.
ND This flag (or « ) is used to denote anaIytea which are not detected
at or above the specified detection limit. The value to the right of
the < symbol is the method specified detection limit for the sanple.
NS This analyte or surrogate was not added ( spiked) to the sanple for
this analysis.
0 This quality control standard is outside method or laboratory spec-
ified control limits. This flag is applied to matrix spike, analy-
tical OC spike, and surrogate recoveries; and to RPD(relative percent
difference) values for duplicate analyses and matrix spikeVmatrU
spike duplicate result.
The asterisk(") is used to flag results which are less than five times
the method specified detection limit. Studies have shown that the
uncertainty of the analysis will increase exponentially as the method
detection limit is approached. These results should be considered
approximate.
-------
Notes .and Definitions
EHB
Radian work Order: PI-09-010
Page'
TERMS USED IN THIS REPORT:
Analyce - A chemical for which a sanple is to be analyzed.
EPA method and QC specifications.
The analysis will meet
Compound • See Analyte.
Detecrion Limit - The method specified detection limit, which is the lower limit of
quantitat ion specified by EPA for a nwthod. Radian staff regularly eaeeis their
laboratories-1 method detection limits to verify that they meet or are lower than those
specified by EPA. Detection limits uhich are higher than method limits ire baaed
on experimental values at the 991 confidence level. The detection limits for EPA CLP
(Contract Laboratory Program) methods are CRQLs (contract required quantitation
Limits) for organics and CRDLs (contract required detection limits) for inorganics.
Note, the detection limit nay vary from that specified by EPA based on sample
size, dilution or cleanup. (Refer to Factor, below)
EPA Method - The EPA specified method used to perform an analysis. EPA has specified
standard methods for analysis of environmental samples. Radian will perform its
analyses and accompanying DC tests in conformance with EPA methods unless otherwise specified.
Factor • Default method detection limits are based on analysis of clean water samples.
A factor is required to calculate sample specific detection Units based on alternate
matrices (soil or water), reporting units, use of cleanup procedures, or dilution of extracts/
digestaces. For example, extraction or digestion of 10 grams of soil in contrast
to 1 liter of water will result in a factor of 100.
Matrix - The sanple material. Generally, it will be soil, water, air, oil, or solid
waste.
Radian Uork Order • The unique Radian identification code assigned to the samples reported in
the analytical summary.
Units - ufl/L micrograns per liter (parts per billion),-liquids/water
ug/kg microgreoa per kilogram (parta par billion); soils/solids
ug/M3 microuraras per cubic meter; air sample*
mg/L milli or ems per liter (parts per fliiUion);llquid*/water
nig/kg milligrams per kilogram (parts per mi I Uoo);soi ts/sol Ids
X percent; usually used for percent recovery of QC standards
uS/cm conductance unit; nfcroSleoans/cemimeter
nt/hr mi IIillters per hour; rate of settlement of matter in water
NTU turbidity unit; nephelometric turbidity unit
Cu color unit; equal to 1 mg/L of chloroplatinate salt
-------
APPENDIX F,4
PAH
-------
Radian Uort Order P1-09-01Q
Analytical Report
12/16/91
EHB
EHB
Radian Corporation
RIP. NC
Larry Ranesburg
Customer Uort Identification Aephalt T«t Slto 6
Purchase Order Hunbar 275-026-48-27
Contents:
1 Analytical Data Sunnary
2 Sample History
3 Conmenta Sumary
4 Notes and Definitions
Radian Analytical Services
900 Parimater Park
Horrisvillo, NC 27560
919-481-
Client Services Coordinator: URCWESBURG
Certified by;
-------
EHB
Radian Uorlc Order:
Pl-09-010
Analytical Data Summary
Page:
Hethod:SU8270-Semi-Valatiles (D
List:PAHs by SWB44 827D
Sample 10:
Factor:
Results in;
Matrix:
H6-0918-PAH-F-
B (6-113
5
Total ug
02A
XAD-2/Ff
M6-0919-PAH-1
17,18,20-23
5
Total ug
04A -
Stack
Mr0919-PAH-2
(35, 37-41)
5
Total ug
06*
Stack
N6-0920-PAH-J
(48, 50-54)
5
Total ug
08A
Stack
. Acenaphthene •.
.Acenaphthylene .
, Anthracene
Benzo(a}anthracene ,
Benzo(a)pyrene
Benzo(b)f luoranthene
, Benio(g,h, i Jperylene '
Benzo(k)f luoranthene
Chrysene
• Dibenz(a,n)anthrecene
Dibenzofuran
7, 1 2-0 i me thylbenz( a) anthracene
• F luoranthene
Fluorene -
Indenocl ,2,3-cd)pyrene ,.
2 -He thy (naphthalene
Naphthalene •
Phenanthrene
Pyrene
(See ne»t page for te
Result Det. Limit
NO 50
ND 90
NO 50
ND 5.0
ND SO
ND 50
ND 50
NO SO
ND 5D
ND SO
ND 50
ND 100
NO SO
ND 90
ND 50
2.36 J SO
751 B 50
0.275 J' 50
ND 50
ntatively identified ca
Result Det. Limit
14.9 J_ . SOf :!
41.8 J Sfll&il
10.2 J 5fll»
ND Wlffl
ND SOjill
ND soiil
NO
ND
ND 50W1 .
ND sili!
ND
ND 1001!:!::!:
ND 51111
ND Sttllil
ND SttiBIP
408 Sl«iifi
416 B 50«::.
9.04 J SOtV'-:
1.26 J 50: -"r:.;
npounds.)
Result Det. Limit
ND SOlil
37. 7 J Sllil
8.99 J 56'S*
NO SOP; .
NO SOff. -
NO SO i;!*?-;.
NO SPP'7
MD 5Qf;;:.
ND W^-:
ND . S'Olivi
ND Jicrte-:-'
,::.M::L::, ..,.>-
NO lot);
NO soli? _^
ND SO;;;. :.
ND SO ,:.::.•-"
348 safe;- '
776 B SO:!::
7.94 J SO*
0.625 JB« 50 V
Result Det. Limit
NO H!::;M;
48.1 J MA:;;,?*
9.62 J SOm.J'
ND SOS- ="•'
ND SOt/,
ND 50li-
NO 50K>'-
ND 50;%;
NO • • ^oi;?*';;
ND J0p||
ND SO1:-'" J
ND 100;
ND S4T-.V'.;
ND 5fr?xv ;
ND 50
417 Sfl? '
1470 B 50
8.49 J 50
0.805 J« 50
ND Not detected at specified detection limit
B Detected in blank,result not corrected
J Detected at less than detection limit
• Est. result less than 5 times detection limit
(1) For a detailed description of flags and technical terro in this report refer to Appendix A in this report.
(2) 4-Hethylphenol co-elutes with 3-methylphenol. The
value reported is the combined total of the 2
-------
Analytical Data Summary
Pas*:
EMB
Radian Work Order: P1-09-010
Method;Su8270-Semi-Volotiles (1)
List:PAHs by SU844 8270
Sample 10; N6-09t8-PAH-F- H6-09I9-PAH-1 N6-0919-PAH-2 H6-0920-PAH-3
B (6-11) 17,18,20-23 (35, 37-41) (48, 50-54)
Factor: 5
5 5 S
Results in: Total ug Total ug Total us Total ug
Q2A
04A ~ 06* DBA
Matrix: XAD-2/Fi Stack Stack Stack
Result
Surrogate Recovery(X)
2-Fluorobip*ienyl 141 Q
Control Limits: 30 to 115
Nitrobenzene-d5 96.4
Control Limits: 23 to 120
Terpnenyl-d14 112
Control Limits; 18 to 137
(See ne«i page for tentatively
Oet. Limit Result Det. Limit
146 Q
113
111
' identified conpcxxids.)
Result Oet. Limit
124 Q
93.9
112
Result Det. Limit
153 Q
113
121
0 Outside control limits
CD For a detailed description of flags and technical terms In this report refer to Appendix A in this report.
(2) 4 -Methyl phenol co-elutea with 3-methylphenol. The
value reported is the combined total of the 2
-------
EBB
Radian work Order;
P1-09-010
Analytical Data Sunnary
Page:
Method;SW8270-Seflii-VolBtiles (1
ListrPAHs by SU8A6 8270
Sanple ID:
Factor:
Results in:
-•
Matrix:
Acenaphthene
Acenaphthylene
Anthracene
Benzo(a)anthracene
Benio':;'':'"y-:
NS ':»;:B»:-.H
135
•.ivii'W^'Sw
1||
'illK
''%••$?'•{•'{•:
:"x''"x"i"x*"'!>y*
Illll
.::;:||g|::;
lliS
.'Islli!"
1!llvi;
""':r'i!:^..':i'::''
•j:".5x.:^;.
'
*
- •*.
ND Not detected at specified detection limit
• Est, result less than 5 times detection Unit
J Detected at less than detection limit
NS Not spiked
(1) For a detailed description of flags and technical terms in this report refer to Appendix A in this report.
(2) 4-Methylphenol co-elutes yith 3-melhylphenol. The
value reported is the corrbined total of the Z
compounds.
-------
ENB
Radian Uork Order: P1-09-010
Analytical Data Summary
Page:
Mechod:3HaZ70-Semi-Volatflea (1)
List;PAHs by SU646 8270
ID:
METHOD BLANK
METHOD SPIKE
Factor:
Results in:
Matrix:
5
Total ug
ISA
KAD-2/FI
5
X
16A
XAD-Z/M
Surrogate Recovery**)
2 - F I uorob i pheny I
Control Limits: 30 to 115
Nitrobeniene-d5
Control Limits: 23 to 120
Terphenyl-dU
Control Limits: 18 to 137
Result Det. Limit
130 Q
87.4
111
Result Det. Limit
143 Q
105
127
Q Outside control, limits
(1) For a detailed description of flags and Technical terms in this report refer to Appendix A in this report.
(23 4-Nelhylphenol co-elutes with 3-methylphencS. The
value reported is the combined total of the 2
-------
EMB
Radian Uork Order: P1-09-010
Analytical Data Sums
Page:
Tentatively Identified Confounds
Method; SuaZTC-Semi-Volati les (1)
List; PAHs by SU846 8270
Sanpie 10 »nalyt«
M6-0918-PAH-FS (6-11)
M6-0919-PAH-1 17,18,20-23
1«Methyl naphthalene
OiethylphtKalate
Result Units Scan
1.94 B*J Total ug
7.27 S«4 Total ug
Di--'-butylpr alace
Oiphenylatnine
Bis-(2-ethylhexyl)-pnthalate
Phenol
Acetophenooe
3-Methylpherwl
indent
1-Meihylnaphthalene
Buiylbenrylpnlhalate
Bis-(2-ettiythexyl)-phthalate
Di-n-octylphthalate
2,6-Oimethylheptadecane
2.6-Dimethylnonarw
TetramethyI benzene
1-Ethyl-2,3-dimethylbeniene
9.44 e*J Total ug
0.72 'J Total u?
11.4 B'J Total ug
34.6 *J Total ug
93.5 Total us
5,70 -J Totai >jg
421 Total ug
249 S Total us
0.67 "J Total ug
47.4 8-J Total ug
0.66 >J Total ug
NO Total ug
NO Total ug
HQ Total ug
NO Total ug
-------
Analytical Data sunmary
Page:
EHB
Radian Work Order: P1-09-Q10
Tentatively Identified Conpounds
Method: SW8Z70-Semi - Voletiles (1)
List: PAHS by SW&46 8270
Sample ID
M6-0919-PAH-2 (35, 37-41)
Analyte
5 ,4-Dimethylmtecane
2,3-Dihydro-4-meihyl-lH-lndene
(1,1-0imethylpropyI)-benzene
6-Mettiyldodecane
2,4-Dimethyl-l-
(1-methylprepyl)-benzene
r-Methyliridecene
i, ,7-DinethylLniecarM
3-Hethyltridecane
1,l'-Biphenyl
2*H«thylirtecan«
2-Ethyl naphthalene
Dimethyl naphthalenes
Acetophenone
J-Methyl phenol
Indene
Oiethylphthalate
Sis-CZ-ethylhexyD-phthalate
1 -Hethylnaphthalene
Resu L t
NO
HQ
NO
HQ
NO
NO
NO
NO
NO
NO
NO
NO
Units Scan
Total ug
Total ug
Total ug
Total ug
Total ug
Total, ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
83.4 Total ug
3.46 *J Total ug
387 Total ug
12.2 B'J Total ug
390 B Total ug
m B Total ug
-------
EHB
Radian Work Order: PI-09-010
Analytical Data Surinary
Page:
tentatively Identified Compounds
Method: SU827Q-Semi-Volaci les (1)
List: PAHs by SUB46 8270
Sanple 10
Analyte Result Units Scan
Decane NO Total ug
1,3,5-Trimethylbenien* NO Total ug
l'Heptyl-2-methyleyclopropane NQ Total ug
Ethylmethylbenzenes NO Total ug
Uknown oxygenated hydrocarbons NQ Total ug
Unkoun branch hydrocarbons NO Total ug
2,3-Oimethyloctarw NO Total ug
(l-Methylethyl)-benzene MO Total ug
Oimethylbenzenea NO Total ug
1-Heptyl~2-mthyUyclopropane MQ Total ug
2,3,4-TrimeihylNexane MO Total ug
Unknown alcoxy alcohol NQ Total ug
1-Octene HO Total ug
4-Methyl-3-penten-2-one NO Total ug
Octan* NO Total ug
2-Propenylcyclotieftene MQ Total ug
(l-Methylpropyl)-cyclooctane NO Total ug
Toluene NO Total ug
M6-0920-PAH-3 (48, 50-54)
Phenol
24.0 *J Total ug
-------
Analytical Data Surmary
Page:
EMB
Radian Work Order: P1-W-010
Tencaiively Identified Campou-ids
Method: syfl27u-Semi-Volaii Us (1)
List; PAHs by SW&46 8270
Sample ID
Ana lyre Result
Acetopheoone 114
3-neihylphenol 2.74
Indent 426
Cyclohenane 996
!•Methyl naphthalene 262
Diethylphthalate 17,9
iis"C2-ethylhe«yl)-phthaUte 36.9
Di-n-octylphthalate 1.17
Cyelohexene NO
Unknown branched hydrocarbons NO
Toluene HO
4-Hettiyl-3-penten-2-one NQ
Xytene isomers HQ
1-Ethyl-2-methylbeniene NO
Decane HQ
1,3-Diethylbenzerw MO
1,4-Oiethylbenzene NQ
1-Methyl-2-(2-propenyl}-benten NQ
Undecan« NO
(E)-(1-Neihyl-l-prop*nyU-beni NQ
Units Scan
Total us
•J Total ue -
Total ug
Total ug
Total yg
*j Total ug
*J Total ufl
*J Total ug
Total ug
Total ufl
Total ug
Total u0
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
-------
EHB
Radian Work Order: P1-09-010
Analytical Data Summary
Page;
Tentatively Identified Compounds
Method: SUBZ70-Seroi-Volatiles (1)
List: PAHs by SU846 3270
Sanple ID
METHOD BLANK
METHOD SPIKE
Anaiyte Result
2,3-Dihydro-4-melhyl-1H-indene WQ
4,7-Dimethylundecane
2-Fluoro-1,T-biphenyl
NO
HO
1 • He thy I naphthalene 0.365
Diechylphthalate 22.3
Di-n-butylphchalace 11.7
Bis-(2*ethylhexyl)-phthaLate 19,5
Cyelohexerte NO
4-Methyl-3-penten-2-one NO
2 ,2' -Oiybis-ethanol di acetate NO
Oi ethyl ben ten* isomers NO
Benzoic acid, methyl ester NO
Unsaturated branched benzyl NQ
MQ
Oxygenated hydrocarbons
Phenol
2-Chlorophenol
1,4-Diehtorobenien*
Units Scan
Total ug
Total ug
Total ug
•J Total ug
•J Total ug
•J Total ug
'J Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
84.8 X
94.2 X
95.6 X
-------
EHB
Radian Uork Order: P1-09-010
Analytical Data Suimary Page;
Tentatively Identified Compounds
Method: SU8270-Seini-VolotUes (1)
List: PAHs by SU8A6 8270
Sample 10 Arwlyte Result Units Sean
N-Nitroso-di-n-propylamin* 104 X
1,2,4-Trfehlorobenien* 109 X
4-Chloro-3-methylphenoL 99.9 X
4-Mitrophenol S3 X
2,4-Dfnitrotoluene 94.6 X
PencacMorophenol 26.6 X
Di-n-butylptithalate 2.15 X
-------
Analytical Data Surma TV
Page;
EMB
Radian Work Order: P1-09-010
Method: Tuenty TICS Co be reported (1)
List:
Sanfile ID:
Factor:
Results in;
-,'
Matrix:
N6-091B-PAH-F- H6-0919-PAH-1 M6-0919
B (6-11) 17,18rZO-23 IK, 37
5 5 5
•P«H-2 H6-0920-PAH-3
•41J (48. 50-54)
5
Total ug Total ug Total ug Total ug
02A MA - 04A
XAD-2/Fi stock Stack
oa*
stack
Result Oct. Limit Result Det. Limit Result De
t. Limit Result Det. Limit
<1) For a detailed description of flags and technical terms in this report refer to Appendix A in this report.
-------
Analytical Data Sunmary
Page: 1
EMB
Radian Llork Order: P1 -09-010
Tentatively Identified Coniaounds
Method: Twenty TICS to be reported (1)
List:
Sampie ID
H6-0918-PAH-FB (6-11)
Analyte
Result Units Scan
Toluene
4-Nethyl-3-p*nten-2-on*
Cyclohexene
1,l'-Bicyclopropyl
2,3-Dimethylheptane
Z-NethyI octane
1.4-Diethylbeniene
1,3-Diethylbenzene
1-Hethyl-2-(2'propenyl5-benzen MQ
1•EthenyI•4•ethyI benzene
-<1-methyl-1-propenyt)-
benzene
(1,1-Oimelhylpropyt)-benzene
Oecahydro-2,3-dimBthyl-
naphthalene
1,3,5-Triethyl benzene
Unknown oxygenated branched
hydrocarbons
Unkown unsaturated branched
MQ
NO
NQ
HO
NQ
MQ
HO
NQ
MQ
HQ
NO
NQ
HQ
NQ
NQ
NQ
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total u0
Total ug
Total ug
Total UQ
Total ug
fatal ug
Total ug
-------
EHB
Radian Uorlc Order; PI-09-010
Analytical Data S urna TV
Page
Tentatively Identified Confounds
Method: Twenty TICS to be reported (1)
List: '
Sample ID
H6-0919-PAH-1 17,18,20-23
Analyte
hydrocarbon
Cyelohexene
Toluene
2-Methyl-l-Heptene
t-Oetene
4-Nethyl-3-penten-2-one
Octane
2-Nethyloetane
Trimethyl naphthalenes
Si me thy I benzenes
1-Heptyl-Z-nwthylcyclopropane
Heptadecane
Hexadecane
Propyl eye 1 ohexanc
3-Methylnonone
2,3 -Dimethyl octane
E thy In* thy I benzenes
2,6-Dimethylheptadecane
1-Hepty I -2-methyL cyclopropane
Result
-
NO
HQ
NO
NO
NQ
NQ
NO
NO
NO
NQ
NO
NO
NO
NQ
NO
NQ
NO
NO
Units Scan
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
-------
Analytical Data Surma TV
Page: 1
EKB
Radian Uork Order: P1-09-010
Tentatively Identified Compounds
Method: Twenty TICS to be reported (1J
List:
Sample ID
M6-Q919-PftH-2 (35, 37-41)
Analyte
Trfmthylbenierw
Decane
2 , fl-0 i methy Inonane
Trimethylbenzene iscmer
1-Ethenyl-2-mettiylbenz«ne
1 , 3 • D i ethy I beruene
2-Ethyi- 1 ,4-Oimethylberaene
1-Hethyl-2-(2-propenyO-b€fizen MQ
4, 7-Oimethylund*cane
1 ,3-OietHyl -S-methylbenzene
1-f thyl'2,3-diiwihylbenzene
{C)-(l-N«tliyl-1-prepenyl)-benz NO
5,6-OimethylLndecane
naphthalene Sktetituted with a NO
branch alkyl chain
1,1 -Dimethylpropylbenzene
t ,6-Dimethylnaphthalene
Result
NO
NO
no
NO
NQ
NQ
NO
NQ
NQ
MO
NO
NQ
NO
NQ
MQ
NO
NQ
NQ
Units Scan
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
-------
EMB
Radim Work Order: P1-09-Q10
Analytical Data Surrary
Page: 1
Tentatively Identified Confounds
Method: Twenty TICS to be reported (1)
List;
Sairple ID
M6-0920-PAH-3 (48, 50-54)
Analyte
2,6-Dimethylhe0tad*cane
He*ad*cajne
4,7-DimethyI undecane
1,6-Oimethylnaphrhalene
1 ,B-Oimethylnaplithalene
1,5-Oimethytnaplithalene
2,6- 0 itwthy I hepcadecane
Hexadecsne
Heptadecane
Result Units Scan
MQ Total yg
MO Total yg * '
NO
MQ
NO
NO
NQ
NO
NO
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
Total ug
-------
Appendix A
, Note* and D*finftlera
-------
EHB
Radian Work Order: P1-09-010
Sample History
Pcje:19
Sample Identifications and Dates
Sanple ID H6-091B-PAH-F- H6-W19-PAH-1 M6-0919-PAH-2 M6-0920-PAH-3 H6-Q91B-ALD-F- H6-Q919-ALD-1
B (6-11) 17,18,20-23 (35, 37-41) (48, 50-54} B (12, 13) (28, 29)
Date Sailed 09/18/91 09/19/91 09/19/91 09/20/91 09/18/91 09/19/91
Date Received 09/23/91 09/23/91 09/23/91 09/23/91 09/23/91 09/23/91
Matrix XAO-2/H Stack Stack ~ Stack Stack Stack
02 04 06 08 09 10
SU8270-S«ni -Volatites
Prepared
Analyzed
Analyst
File ID
Blank ID
Insirunent
Report as
Aldehydes, Hod T011, HPLC
Prepared
Analyzed
Analyst
File 1C
Blank ID
Instrunent
Report as
Tuenty TICS to be reported
Prepared
Analyzed
Analyst
File ID
Blank ID
Instrunent
Report as
09/30/91
11/05/9T
BE
4586538. T I
45B6532.T!
GC/NS B
received
09/30/91
11/05/91
RK
4586538. T I
45B6532.T1
GC/MS B
received
09/30/91
11/05/91
HK
4586535. Tl
45B6532.TI
GC/HS B
received
09/30/91
11/05/91
RK
<.5B6535.T]
45B6532.T1
CC/MS B
received
09/30/91
11/05/91
RK
45B6536.T1
45B6532.TI
GC/MS B
rece i ved
09/30/91
11/05/91
RK
45B6536.U
45B6532.TI
GC/HS B
received
09/30/91
11/05/91
RK
4584537. Tl
45B6532.TI
GC/MS B
received
09/30/91
11/05/91
RK
4584537. Tl
4504532, TI
GC/HS B
received
09/30/91
10/18/91
LKK
OWEN125
LLWA75
V5000
received
09/30/91
10/18/91 ".
LKK
OWEN1Z6/175
LLWA75
V5000
received
-------
EHB
Radian Work Order: PI-09-010
Report Carments and Narrative
Page:
General Comwnta
Aldehyde Data: T • Outside of calibration curve.
Q - Spike recovery QC limits range from 80 to 120 percent.
Calibration check QC limits range from 65 to 115 percent.
NA - The butyraldehydes and MEK coeluted.
-------
Notes and Definitions Page: »•
EHB
Radian Uork Order: PI-09-010
a This flag indicates chat the analyte wai detected in the reagent blank
but the sample results are not corrected tar (he amount in the blank.
J Indicates an estimated value for GC/HS data. This flag is used either
when estimating a concentration for tentatively identified confounds
where a response factor of 1 is assumed, or when the mass spectral
data indicate che presence of a compound that meets the identification
criteria but the. result is less than the sample quantitat ion limit.
NA This analyte was not analyzed.
ND This flag (or < ) is used to denote analytes which are not detected
at or above the specified detection limit. The value to che right of
the < symbol is che method specified detection limit for the sample.
NS This analyte or surrogate was not added ( spiked) to the sample for
this analysis.
0. This quality control standard is outside method or laboratory spec-
ified control limits. This flag is applied to matrix spike, analy-
tical 3C spike, and surrogate recoveries; and to HPO(relative percent
difference) values for duplicate analyses and matrix spike/matrix
spik« duplicate result,
• The ascerisk(') is used to flag results which are less than five times
the method specified detection limit. Studies have shown that the
uncertainty of the analysis will increase exponentially as the method
detection limit is approached. These results should be considered
approximate.
-------
Notes and Definitions
Page:
1MB
Radian Work Order: P1-09-010
TERNS USED IN THIS SEPOflT:
Analyie - A chemical for which « sample is to be analyzed.
EPA method and QC specifiesc ions.
The analysis will
Compound • See Analyte.
Detection Limit - The method specified detection limit, which is th* lower Unit a1
quantitation specified by EPA for a method. Radian staff regularly asae-ss their
laboratories' method detection Limits to verify that they meet or sre lower than those
specified by EPA. Detection limits which ere higher than method limits are baaed
on experimental values at the 99% confidence level. The detection IT mi to for EPA CLP
(Contract Laboratory Program) methods are CRQLs tcant root required quantitatfon
limits) for arsenics and CRDLs (contract required detection limits) for inorganics.
Note, the detection limit may vary from that specified by EPA based on sample
site, dilution or cleanup. (Refer to Factor, below)
EPA Method • The EPA specified method used to perform an analysis. EPA has specified
standard methods for analysis of environmental samples. Radian will perform its
analyses and accompanying QC tests in conformance uith EPA methods unless otherwise specified.
Factor - Default method detection limits are baaed on analysis of clean water samples.
A factor is required to calculate sample specific detection Haiti baaed on alternate
matrices (soil or water), reporting units, use of clean*! procedures, or dilution of extracts/
digtstates. For example, extraction or difntion of 10 grams of soil in contrast
to 1 liter of water will result in a factor of 100.
Matrix - The sample material. Generally, it will be soil, water, air, oil, or solid
waste.
Radian work Order - The unique Radian identification code assigned to the samples reported in
the analytical summary.
Units • ug/L raicroflrans per liter (parti par bill fan);liquids/water
us/kg microgratM par ktlogrssi (parti per billion); so Us/solids
ug/H3 mlcrograms par cubic meter; air saoples
mg/l milligrams par If tar (parti par milllon);llqulds/nater
mo/kg milligrama per kltograa (parti par milllon);soiU/sollds
X percent; usually us*d far percent recovery of QC standards
uS/cm conductance unit; nicreSienans/centtmeter
mL/hr mill Utters per hour; rate of tattlenent of matter in water
MTU turbidity unit; nepfcaioBBtric turbidity unit
CU color unit; equal to 1 09/1 of chloroplatlnaie salt
-------
APPENDIX F,5
SAMPLE ID LOG
-------
I I
IE.
Project No
\
3m Page No—
witnessed & Understood by me,
-------
Project No
--
Bftfi WK Book No._252B 4TFTLE
om Page No.
pie
~ .MS
HPLC14
Witnessed & Understood by me,
-------
APPENDIX G
CALIBRATION DATA SHEETS
-------
Post Test- Mathey
Meter Box Calibration
Date
10/3/91
Cal Meter
6830264
Pbar
29.9
Box*
N-30
Cal Meter Yd
0.9967
Vaccum
10 "Hg
Orifice
Setting
1.1
1.1
1.1
Cal. Meter
Pressure
-0.07
-0.07
-0.07
Gas Volume
Cal. Meter
Final
IniL
Total
Final
IniL
Total
Final
IniL
Total
43.149
39.743
3.406
49.823
43.515
6.308
57.947
49.823
8J24
Gas Volume
Meter Box
52,743
49.400
3.343
59,250
53.100
6.150
67,182
59.250
7.932
Cal. Temp
In Out
68
68
67
67
Av^ 67,5
66
66
67
67
Av|. 66.5
67
68
67
68
Avg. 67.5
Meter Temp
In Out
70
71
68
69
Avg. 69.5
71
70
68
69
Avg. 69.5
70
73
69
70
Avg. 70.5
Time
6
11
14.25
Average
Yd
1.0164
1.0252
1.0237
1.0218
Delta
H@
1.92
1.87
1.90
1.90
-------
Post Test - Mathey
Meter Box Calibration
Date
10/4/91
Cal Meter #
6830284
Pbar
29.88
Box*
N-32
Cal Meter Yd
0.9967
Vaccum
12 "Hg
Orifice
Setting
1.0
1.0
1.0
Cal. Meter
Pressure
-0.06
-0.06
-0.06
Gas Volume
Cal. Meter
Final
Ink.
Total
Final
Ink.
Total
Final
Ink.
Total
31507
2Z882
9.625
37,323
32.507
4.816
44.398
37.323
7.075
Gas Volume
Meter Box
47.087
37.450
9.637
51.885
47.087
4.798
58.962
51.885
7.077
Cal. Temp
In Out
65
66
65
66
Avg. 65.5
66
67
66
67
Avg. 66.5
67
67
67
67
Avg. 67.0
Meter Temp
In Out
71
73
69
70
Avg. 70.8
73
74
70
71
Avg. 72.0
73
75
71
71
Avg. 72.5
Time
18
9
13.25
Average
Yd
1.0028
1.0083
1.0042
1.0051
Delta
H@
1.95
1,95
1.%
1.95
-------
Post Test- Ma they
Meter Box Calibration
Date
10/15/91
Cal Meter #
6830284
Pbar
29.88
Box*
N-33
Cal Meter Yd
0.9967
Vaccum
11 "Hg
Orifice
Setting
1.1
1.1
1.1
Cal. Meter
Pressure
-0.07
-0.07
-0.007
Gas Volume
Cal. Meter
Final
Init.
Total
Final
[nil.
Total
Final
Init.
Total
67,375
61.057
6,318
73,116
67.375
5,741
79,410
73,116
6.294
Gas Volume
Meter Box
76.428
70.000
6.428
81298
76,428
5.870
88.777
81298
6,479
Cal. Temp
In Out
70
72
70
72
Avg. 71.0
73
72
73
72
Avg. 72.5
73
72
73
72
Avg. 715
Meter Temp
In Out
73
78
70
72
Avg. 73.3
80
77
75
73
Avg. 76.3
82
79
78
75
Avg. 7&5
Time
11
10
11
Average
Yd
0.9810
0.9788
0.9765
0.9788
Delta
H@
1.89
1.89
1.90
1.89
-------
APPENDIX H
SAMPLE EQUATIONS
-------
SAMPLE CALCULATIONS
COMPANY : 90RGESS MEDICAL CENTER
PLANT SITE : KALAMAZOO, MI INPUT PARAMETERS
SAMPLING LOCATION : BAGHOUSE OUTLET
DATE : 09/07/91
EXAMPLE «l: PH/Metals , RUN 02
STANDARD CONDITIONS: 68 F, 29,92 In Hg
1) Volume of dry gas sampled at standard conditions;
As
Cp
On
Kp
P(std) •
Pb
Pmg(avg)-
551.55 sq.ln.
O.B4
0.313 In.
84.59
29,92 in. Hg
29.52 In. Hg
0.45 In. H20
Pa
XC02
XN2
102
T(std3 -
Tm(avg) •
Vm
29,48
4.69
80,26
15.05
68.00
110.09
91.40
in. Hg PM COLLECT. -
AVG SQRT OEL.P •
MOISTURE •
COLLECTED
F SAMPL TIME •
F T9(avg) -
ft*3 Y
0-0102 gran
0.2546 IN Y
211.60 gran
Z40 min.
294,42 F
1.0108
Pm - Ping/13,6 * Pb
Pm • 29.5530
Vm(std)
Y • Vm ' (T(std) + 460) " Pm
P(std) • (Tm(avg) • 460)
Vra(std) • (1.011 * 91.40 * (68 + 460) * 29.55) / (29.92 • ( 110.09 + 460))
Vm(std) • 84.52 dscf
2) Volune of nater vapor at standard conditions:
V-(gas) - 0.04707 ft3/g * (moisture collected)
Vw(gas) • ( 0.04707 * 211.60 )
Vw(gas) = 9.95 scf
3) Percent moisture In stack:
100 * V*(gas)
XV •
Mstd) + Vw(gas)
XV - (100 *9.95) / (64.52 * 9-95)
XV = 10.53
4) Mole fraction of dry stack gas:
100 - XV
MFd
100
MFd - (100 - 10.53) / 100
MFd- 0,895
-------
DEFINITION OF TERMS
SYMBOL DEFINITIONS
As AREA OF STACK
Cp PITOT COEFFICIENT
Ca CONCENTRATION OF PASTICULATE
Dn DIAMETER OF SAMPLING NOZZLE
ER EMISSION RATE OF PARTICULATE
Kp PITOT TU8E COEFFICIENT
MFd HOLE FRACTION OF DRY STACK GAS
MWd MOLECULAR WEIGHT OF DRY STACK GAS
MWw MOLECULAR WEIGHT OF WET STACK GAS
MOISTURE COLLECTED IN IMPINGERS
P(std) STANDARD PRESSURE (29.9? In. Hg)
Pb BAROMETRIC PRESSURE
Ping(avg) AVERAGE GAUGE HETER PRESSURE
Ps ABSOLUTE STACK PRESSURE
PARTICULATE CATCH
Qsd AVERAGE STACK DRY VOLUMETRIC FLOW RATE
XC02 PERCENT CDZ IN STACK GAS
XNZ PERCENT NZ IN STACK GAS
xoz PERCENT oz IN STACK GAS
XV PERCENT MOISTURE IN STACK
XXS PERCENT EXCESS AIR
TOTAL SAMPLING TIME
T(std) STANDARD TEMPERATURE (63 F)
Tm(avg) AVERAGE TEMPERATURE OF THE METER
Ts(avg) AVERAGE TEMPERATURE OF THE STACK
Vm TOTAL HETEREO VOLUME
Vm(std) STANDARD METERED VOLUME
Yw(gas) VOLUME OF WATER IN STACK GAS
Vs VELOCITY OF STACK GAS
Y TEST METER CALIBRATION COEFFICIENT
UNITS
In. '2
grains/ft'3
In,
Ib/hr
lb/lb-mole
lb/lb-mole
grama
In. Hg
In, Hg
in. Hg
in. Hg
grama
dry fO/mln.
mln.
F
F
F
ff 3
dry standard ft'3
standard ft"3
ft/mln
-------
10) Excess air (X):
100 * XOZ
WC H ~ I
&AJ B • ••»«.»*> <••<••
(0.264 • VIZ) - K)2
MS - (100 • 15.05) / ((0.264 * 80.26) - 15,05)
XXS • 244.53
11) Concentration of participate:
Ca ' {paniculate catch) / Vm(std) / 453.59 ' 7000
Ca » 0.0102 / 84,52 / 453.59 • 7000
Ca <• 0.00186 grains/dscf
12) Paniculate Emissions Rate;
ER • (concentration) * (Qsd) • 60 / 7000
ER - 0,0019 • 2444.95 * 60 / 7000
ER - 0.039 Ib/hr
-------
5) Average motecuTar weight of dry stack gas:
FWd - (0.44 ' XC02) + (0.32 • X02) • (0.28 * XH2)
KWd - (0.44 * 4.69) + (0.32 * 15.05) + (0,28 • 80.26)
MWd • 29.35 Ib/lb-rmle
6) Average molecular weight of «t stack gas:
HUM • MM * MFd + 18.0 • (1,0 - MFd)
MVw - 29.35 " 0-895 + 18.0 • (1.0 - 0.895)
MVw - 28.16 Ib/lb-mole
7) Stack velocity (feet/min) at stack conditions:
Vs » Kp*Cplr[SQRT(dP)]avg-(SQRT[(T5)avg])*[SORT(l/P3*MW*)]*60
Vs - 84.59 • 0.84 • 0.25 * SQRT[(294.42 +460) / (29-48 * 28.16)]
Vs » 17.24665 fps
1034.799 fpm
8) Average stack dry volumetric Flo* rate:
Vs • As • MFd • (T(std)+460) • Ps
Qsd » --
144 sq.fn./cu.ft. * (Ts(avg) + 460) * P(std)
Qsd - 17.25 * 551.55 • 0.895 • (68.0 * 460) * 29.48 / (144 • (29«.42 + 460) * 29-92)
Qsd = 2444.95 dscfm
69.24236 dscim
9) Isoklnetic sailing rate (X):
1039.5746 * Vm(std) * (Ts(avg) + 460)
XI m --........_. ...... ......
Vs • samp, time • Ps ' MFd • (On)'2
XI - (1039.5746 • 84.52 * (294.42 + 460)) / (1034.80 * 2«0 * 29.48 * 0.895 ' (0.313)"2)
XI - 103.24
-------
APPENDIX I
PROJECT PARTICIPANTS
-------
PROJECT PARTICIPANTS
RADIAN CORPORATION
Rod Brown
Joan Bursey
Jamie Clark
Geoff Johnson
Jack Johnson
Vince Laura
Julie Lopez
Tom McDonald
Terry Medley
Charlie Parrish
Katherine Potter
Jon Proulx
Larry Romesberg
Tim Skelding
Judy Smith
James Southerland
Joette Steger
ENVIRONMENTAL PROTECTION AGENCY
Dennis Holzschuh
NATIONAL ASPHALT PAVEMENT ASSOCIATION
Thomas Brumagjn
-------
APPENDIX J
SAMPLING AND ANALYTICAL PROTOCOLS
J.I PM/Metals
J.2 PM10/CPM
J3 Aldehydes
J.4 PAH
J.5 CEM and GC
-------
APPENDIX J.I
PM/METALS
-------
EMB DRAFT METHOD LO/3L:
METHODOLOGY FOR THE DETERMINATION OF METALS EMISSIONS
IN EXHAUST GASES FROM INCINERATION PROCESSES
1. Applicability and Principle
1.1 Applicability. This method is applicable Tor the determination of
arsenic (As), beryllium (Be), cadmium (Cd), total chromium (Cr), lead (Pb),
mercury (Hg). nickel (Ni), and zinc (In) emissions from municipal waste
incinerators and similar combustion processes. These elements are referred to
hereafter as the primary aetals. This method may also be used for the
determination of antimony (Sb). barium (Ba), copper (Cu). manganese (Mn),
phosphorus (P). selenium (Se), silver (Ag), and thallium (Tl) emissions from
these sources. These elements are referred to hereafter as the secondary
metals.
In addition, the method may be used to determine partieulate emissions by
following the additional procedures described. Modifications to the sample
recovery and analysis procedures described in this protocol for the purpose of
determining partieulate emissions may potentially impact the front half nercury
determination.•
1.2 Principle. The stack sample is withdrawn isoklnetieally from the
source, with particulmte emissions collected in the probe and on a heated
filter and gaseous emissions collected la a series of chilled Impingers
containing a solution of dilute nitric acid la hydrogen peroxide in two
iopingers. and acidic potassium permanganate solution in tvo (or one)
inpingers. Sampling train components are recovered and digested in separate
front and back half fractions. Materials collected in the sampling train are
digested with acid solution* to dissolve inorganics and to remove organic
constituents that may create analytical interferences. Acid digestion ii
performed using conventional Parr1 Bomb or microwave digestion techniques. The
•Field tests to data haw shown that of thm total amount of mercury measured
by thm method, only 0 to <2% was measured la tarn front half. Therefore, it is
tentatively concluded, based on the above data, that partieulate emissions a ay
be measured by this train, without significantly altering the mercury results.
-------
nitric acid and hydrogen peroxide impinger solution. the acidic potassiun
permanganate ifflpinger solution, and the probe rinse and digested filter
solutions are analyzed for eercury by cold vapor atomic absorption spectrescopy
(CVAAS). Except for the permanganate solution, the remainder of the sampling
train fractions are analyzed for As, Be, Cd, Cr, Pb, Ni. and Zn (and Sb, Ba,
Cu, Mn, P. Se. Ag. and Tl. if desired) by Inductively coupled argon plasna
emission spectroscopy (ICAP) or atomic absorption spectroscopy (MS). Graphite
furnace atomic absorption spectroscopy (GFAAS) Is used for analysis of AS, Cd.
and Pb (and Sb. Se. and Tl. when measured) if these elements require greater
analytical sensitivity than can be obtained by ICAP. Additionally, if desired.
the tester may use AAS for analyses of all target metals if the resulting in-
stack aethod detection limits (combined sampling and analytical detection
limits) meet the data quality objectives of the) testing program. For
convenience, aliquots of each digested sample fraction can be combined
proportionally for a single analytical determination. Thm efficiency of-the
analytical procedure is quantified by thm analysis of spiked quality control
samples containing each of the target metals Including actual sample matrix
effects checks.
2. Range. Sensitivity. Precision, and Interferences
2.1 Range. For thm analyses described in this methodology and for siailar
analyses, the ICAP response is linear ovmr severe! orders of magnitude. Sam-
ples containing metal concentrations in the naoognms per milliliter (ng/ml) to
mlcrograms per mlllllitmr (ug/ml) range In the) analytical finish solution can
be analyzed using this technique. Sample* containing greater than
approximately 50 ug/ml of arsenic, chromium, or lead should be diluted to that
level or lower for final analysis. Samples containing greater than
approximately 20 ug/ml of cadmium should be diluted to that level before
analysis.
2.2 Analytical Sensitivity. ICAP analytical detection limits for the
primary [and secondary] metals in thm sample solutions (based on 3W-846. Method
6010) arm approximately aa follow: As (53 ng/ml). Be (0.3 ng/ml). Cd (<*
ng/ml). Cr (7 ng/ml). Pb (0.2 ng/ml). Mi (ij ng/ml), Zn (2 ng/ml) [Sb (32
ng/ml), Ba (2 ng/ml). Cu (6 ng/ml). P (75 ng/ml). Nn (2 ng/ml), Se (75 ng/ml),
Ag (7 ng/ml), Tl (40 ng/ml}]. Thm actual method detection limita are saaple
dependant and may vary aa thm ssmple matrix may affect thm limits. The
-------
analytical detection limiti for the primary [and secondary] eetals in sample
solutions analyzed by direct aspiration AAS (based on SW-846. Method 7000) are
approximately as follows: As (2 ng/ml). Be (5 ng/ml). Cd (5 ng/il), Cr (50
ng/al). Pb (100 ng/ml). Mi (40 rvg/nl). Zn (5 n«/ml) [Sb (200 ng/«l). Ba (100
ng/nl), Cu (20 ng/nl). Mn (10 ng/ml). Se (2 ng/ml), Ag (10 ng/ftl). Tl (100
ng/nl)]. The detection Halt for mercury by CVAAS is approKinately 0.2 ng/ml.
The use of GFAAS can give added sensitivity compared to the use of direct
aspiration AAS for the following primary and secondary Mtals: As (1 ng/nl). Be
(0.2 ng/nl). Cd (0.1 ng/ml), Cr (1 ng/ml). Pb (1 ng/ml). Sb (3 ng/il). Se (2
ng/ml}. and Tl (1 ng/nl).
Using (1) the procedures described In this Mthod. (2) the analytical
detection limits described in the previous paragraph, (3) a volume of 300 ml
for the front half and 150 «1 for the back half samples, and (**} a stack gas
sample volume of 1.2? m3 , the corresponding in-stack method detection Halts
are presented in Table A-l and calculated as shown:
where: A • analytical detection lialt, ug/ml.
B • volume of sample prior to aliquot for analysis, al.
C • stack sample volume, dsca (dam*).
D • in-stack detection limit,
Values in Table A-l are calculated for the front and beck half and/or the total
train.
To ensure optimum sensitivity in obtaining the measurements, the
concentration* of target metal* in the solution* are suggested to be at least
ten times the analytical detection limit*. Under certain condition*, and with
greater care in the analytical procedure, thi* concentration can be as low as
approximately three time* the analytical detection limit. In all case*.
repetitive analyses, method of standard addition* (MBA), serial dilution, or
natrix spike addition should be umed to e*tabll*h the quality of the data.
Actual in-stack Mthod detection limit* will be determined based on actual
source sampling parameter* and analytical reeult* a* described above. If
required, the method in-stack detection limit* can be made mere sensitive than
those shown in Table A-l for a specific teat by u*ing one or sore of the
following option*:
-------
TABLE A-1. IK-STACK NHHOD DETECTION LIMITS *
0.9
4.8 (0.1)*
11.5 (l.U*
0.8
2.1 ' "
0.7 (0.3)*
27
27 (0.8)*
2.6
14.4 (0.3)*
)* Detection llait when analysed by OPAAS.
*• Detection ll«lt when analyzed by CVAAS.
Actual eethod in-stack detection limits will be determined based
on actual source sampling parameters and analytical results as
described earlier In tola section.
A normal 1-hour stapling run collects a stack gam sampling volume of
about 1.25 a9. If ths> ssmpllng time la increased and 5 sP are
collected, the in-stack method detection limits would be one fourth of
tba> values shorn in Table A-l (this means that with this change, the
method 1* Four times more sensitive than normal).
The In-stack detection limits assume that til of the sample is digested
(with exception of the aliquot for mercury) sad the final liquid
volume* for analysis are 300 ml for the front half and 150 ml for Che
back half sample. If the front half volume is reduced from 300 ml to
30 ml. the front half in-stack detection limits would be one tenth of
the values shown above (ten times more sensitive). If the back half
volume is reduced from 150 ml to 25 ml. thm in-stack detection limits
-------
would be one sixth of the above value*. Matrix effects checks are
necessary on analyses of samples and typically are of greater signifi-
cance for samples that have been concentrated to less than the normal
sample volume. A volume less than 25 «1 may not allow resolubiliza-
:ion of the residue and Bay increase interference by other compounds.
o When both of the above two improvements are used on one sample at the
same time, the resultant improvements are multiplicative. For example.
where stack gam volume is increased by a factor of five and the total
liquid sample digested volume of both the front and back halves is
reduced by factor of six, the in-stack method detection limit is
reduced by a factor of thirty (the method is thirty times more
sensitive).
o Conversely, reducing stack ga* sample volume and increasing sample
liquid volume will increase limits. The front half and back halfL
samples (Fractions 1 and 2) can be combined prior to analysis. The
resultant liquid volume {excluding Fraction 3. which must be analyzed
separately) is recorded. Combining the sample am described does not
allow determination (whether front or beck half) of where in the train
the sample was captured. The in-stack method detection limit then
becomes a single value for all target metals except mercury, for which
the contribution of Fraction 3 •u*t be considered.
o The above discussion assumes no blank correction. Blank corrections
are discussed later in this method.
2.3 Precision. The precisians (relative standard deviations) for each of
the primary and secondary metals detected in a method development test at a
sewage sludge incinerator, are as follows: Am (13-5*). Cd (11.51). Cr (11.2%).
Pb (11.6*). Zn (11.81), Sb (12.71). Ba (20.6f), Cu (11.51). P (id.62), Se
(15-32). and Tl (12.31). The precision for nickel was 7-71 for another test
conducted at a source) simulator. Beryllium, mmnganese and silver were not
detected in the) tm*ta; however, baaed on tha analytical sensitivity of the ICAi
for these metals. It is assumed that their precision* should be similar to
those for the, other metals, when detected at slallar levels.
2.4 Interference*. Iron can be a spectral interference during the
analysis of arsenic, chromium, and cmdaiua by ICAP. Aluminum can be a spectraJ
interference during the) analysis of arsenic and lead by ICAP. Generally, these
interferences can be reduced by diluting the) sample, but this increases the
-------
in-stack aethod detection Halt. Refer to EPA Method 6010 (SW-646) for details
on potential interference* for this Mthod. For alt GFAAS analyses, aatri*
modifiers should be used to Halt interferences, and standards should be matrix
matched.
3. Apparatus
3.1 Sampling Train. A schematic of the sampling train is shown in Figure
A-l. It is similar to the Method 5 train. The saapUnc train consists of the
following components.
3.1.1 Probe Noszle (Prcae Tip) and Borosilicate or Quarts Glass Probe
Liner. Same as Method 5, Sections 2.1.1 and 2.1.2. Glass noszles are
requiredunless an alternate probe tip prevents the possibility of contamination
or interference of the tuple with its eaterials of construction. If a probe
tip other than fless is used, no correction of the stack sample test results
can be made because of the effect on the result* by the probe tip. . „
3.1.2 Pitot Tube and Differential Pressure Gauge. Sea* as Method 2,
Sections 2.1 sad 2.2. respectively.
3.1.3 Filter Holder. Glass, a saw a* Method 5. Section 2.1.5. except that
a Teflon filter support Bust be used to replace the flaas frit.
3.1.4 Filter Heating System. Saae as Method 5, Section 2.1.6.
3.1.5 Condenser. The following systea shell be used for the condensation
and collection of gaseous aetals end for determining the moisture content of
the stack gas. The condensing ays tea should consist of four to six iapingers
connected in series with leak-free ground glass fitting* or other leak-free.
non-contaminating fittings. The first iapinger is optional and is recommended
as a water knockout trap for use during test conditions which require such a
trap. The iapingers to be used in the aetals train are now described. When
the first iapinger is used as a water knockout, it shall be appropriately-sized
for a& expected large soisture catch and constructed generally as described for
the first iapinger in Method 5. Paragraph 2.1.7. The second impinger (or the
first HN03/H,0, iapinger) shall also be ss described for the first Iapinger in
Method 5. The third ispinger (or the) iapinger used ss the second HNOj/11,0,
iapinger) shall be the sasa ss the Oreenburg Smith ispinger with the standard
tip described as the second impinger in Method 5. Paragraph 2.1.7. All other
iapingers used in the aetals train are the saae as the second impinger (the
first HMOj/HjOj iapinger) previously described in this paragraph- In suaaary.
-------
GlM* /
taiM y
T»>#=^-
M glu* Mflfrt* ««pos«
-------
che first impinger should be empty, the second and third shall contain known
quantities of a nitric acid/hydrogen peroxide solution (Section 4.2.1). the
fourth (and fifth, if required) shall contain a known quantity of acidic
potassium permanganate solution (Section k,2.2) nd the laat .npinger shall
-ontain a known quantity of silica fel or equivalent desiccant. A thermometer
capable of measuring to within 1°C (2*F) shall be placed at the outlet of the
laat iapinger. When the water knockout impinger it not needed, it is removed
from the train and the other impingers remain the some. If mercury analysis is
not needed, the potassium permanganate iaplngors are removed.
3.1.6 Metering System. Barometer, and Gas Density Determination
Equipment. Same as Method 5. Sections) 2.1 through 2.1.10, respectively.
3.1.7 Teflon Tape. For capping opening* end Maiing connections on the
sampling train.
3.2 Saeple Recovery. Sate as Method 5. Section! 2.2.1 through 2.2.8
(Nonmetallic Probe-Liner and Probe-Nozzle Brushes. Hash Bottles. Sample ~.
Storage Container*. Petri Dishes. Qloss Graduated Cylinder. Plastic Storage
Contalnere. Funnel and Rubber Policemen, and Gloss funnel), respectively, with
the following exception* and additions;
3.2.1 Nonmetallic Probe-Liner and Probe-Nettle Brushes. For quantitative
recovery of aateriala collected in the fr-.^t half of the sampling train.
Description of acceptable ell-Teflon coepcrent brushes to be included in EPA's
Emission Measurement Technical information Center (EJfTIC) files.
3.2.2 Sample Storage Containers. Olass bottles with Teflon-lined caps.
1000- and 500-al. shell be used for KJtoO,-containing samples and blanks.
Polyethylene bottles may be used for other sample types.
3.2.3 Graduated Cylinder. Qlsss or equivalent.
3.2.U Funnel. Gloss or equivalent.
3.2.5 Labels. For identification of samples.
3.2.6 Polypropylene Tweezers and/or Plastic Qloves. For recovery of the
filter from the sampling train filter holder.
3.3 Sample Preparation end Analysis. For the analysis, the following
equipment is needed:
3.3.1 Volumetric Flasks. 100 ml. 250 ml, and 1000 ml. For preparation of
standards and sample dilution.
3-3-2 Graduated Cylinders. For preparation of reagents.
3-3-3 Parr" Bombs or Microwave Pressure Relief Vessels with Capping
-------
Station (CEM Corporation model or equivalent).
3.3.4 Beakers and Watchglasses. 250-nl beakers for sample digestion with
watchglasaes to cover the tops.
3,3.5 Ring Stands and Clamps. For securing equipment such aa filtration
apparacus.
3.3.6 Filter Funnels. For holding filter paper.
3.3.7 Whatman 541 Filter Paper {or equivalent). For filtration of
digested samples.
3.3.8 Disposable Pasteur Pipets and Bulbs.
3.3.9 Voluaetric Pipets.
3.3.10 Analytical Balance. Accurate to within 0.1 iff.
3.3.11 Microwave or Conventional Oven. For heating samples at fixed
power levels or temperatures.
3.3.12 Hot Plates.
3.3.13 Atomic Absorption Spectrometer (AAS). Equipped with a background
corrector.
3.3.13.1 Graphite Furnace Attachment. With As, Cd. and Pb (and Sb, Se.
and Tl. if measured) hollow cathode lamps (HCLa) or electrodeless discharge
lamps (EDLs). Same aa EPA Methods 7060 (As). 7131 (Cd), 7421 (Pb). 704i (Sb),
7740 (Se), and 7841 (Tl).
3-3.13-2 Cold Vapor Mercury Attachment. With a mercury HCL or EDI. The
equipment needed for the cold vapor mercury attachment includes an air
recirculation pump, a quart* cell, an aerator apparatus, and a heat lamp or
desiccator tube. The hmat lams should be capable of raising the ambient
temperature at the) quart* cell by 10*C such that no condensation forma on the
wall of the quarta call. Same aa EPA Method 7470.
3-3-14 Inductively Coupled Argon plaaaa Spectrometer, with either a
direct or sequential reader and an alumina torch. Sam* aa EPA Method 6010.
4. Reagents
Unless otherwise indicated, it is intended that all reagents conform to
the specificationa established by thm Committaa en Analytical Rmagents of the
American Chemical Society, where such specifications arm available: otherwise.
use thm beat available) grade.
4.1 Sampling. Ifem reagents used la sampling arm aa follow:
4.1.1 Filters. Thm filters shall contain leas than 1.3 ug/ln.a of each of
-------
che metals to be measured. Analytical result* provided by filter manufacturers
are acceptable. However, if no such result* are available, filter blanks oust
be analyzed Tor each target metal prior to emission testing. Quartz fiber or
glass fiber filters without organic binders shall be used. The filter* should
exhibit at Least 99-95 percent efficiency (<0.05 pereei": penetration) on 0.3
micron dioctyl phthaiate smoke particles. The filter efficiency test shall be
conducted in accordance with ASTM Standard Method D2986-71 (incorporated by
reference). For particulate determination in sources containing S0a or SO,.
the filter material must be of a type) that is unrmaetlve to SO, or SO,. as
described in Q'A Method 5- Quartz fiber filters meeting these requirements are
recommended.
4.r.2 Water. To conform to ASTM Specification 01193-77. Type II
(incorporated by reference). Analyze the water for all target metals prior to
field use. All target aetals should be less than 1 ng/al.
4.1.3 Nitric Acid. Concentrated. Baker Instra-analysed or equivalent.
4.1.4 Hydrochloric Acid. Concentrated. Baker Instre-analyzed or
equivalent.
4.1.5 Hydrogen Peroxide, 30 Percent (V/V).
4.1.6 Potassium Permanganate.
4.1.7 Sulfurlc Acid. Concentrated.
4.1.8 Silica Qel and Crushed Ice. Seam as Method 5. Sections 3.1.2 and
3-1.4. respectively.
4.2 Pretest Preparation for Sampling Reagents.
4.2.1 Nitric Add (HNOj)/Hydrogen Peroxide (H,0,) Absorbing Solution.
5 Percent HNOj/10 Percent H,0,. Add 50 ml of concentrated HNO, and 333 al of
30 percent H^O, to a 1000-ml volumetric flask or graduated cylinder containing
approximately 300 ml of water. Dilute to voliass with water. The reagent shall
contain leas than 2 ng/ml of each target metal.
4.2.2 Acidic Potassium Permanganate (KMnO,) Absorbing Solution, 4 Percent
KMnO, (W/V). Prepare fresh dally. Dissolve 40 g of KMnO, in sufficient 10
percent H,S04 to makm 1 liter. Prepere and score la glass bottles to prevent
degradation. Ths) reagent shall mnrsin Imma than 2 nf/sd of H§.
Precaution; To prevent autocatalytic decomposition of tb* permangsnate
solution, filter the solution through Whatman 5*1 filter paper. Also, due to
reaction of the potassium permanganate with the meld, there may be pressure
buildup in the sample storage bottle; these bottles should not be fully filled
-------
and should be vented both to relieve excess pressure and prevent explosion due
to pressure buildup. Venting la highly recommended, but should not allow
contamination of the sample; a No. 70-72 hole drilled in the container cap and
Teflon liner has been used.
4.2.3 Nitric Acid. 0.1 N. Add 6.3 al if concentrated HNO, (70 percent) to
a graduated cylinder containing approximately 900 al of water. Dilute eo 1000
al with water. Mix well. The reagent shall contain less than 2 ng/ml of each
target metal.
4.2.4 Hydrochloric Acid (HC1). 8 N. Add 690 al of concentrated HCl to a
graduated cylinder containing 250 nl of water. Dilute to 1000 «1 with water.
Mix well. The reagent shall contain lees than 2 ng/al of Hg.
4.3 Glassware Cleaning Reagents.
(t.3.1 Nitric Acid, Concentrated. Fisher ACS grade or equivalent.
4.3.2 Water. To confer* to AST* Specification* 01193-77, Type II.
4.3.3 Nitric Acid. 10 Percent (V/V). Add 500 al of concentrated KH03 to a
graduated cylinder containing approximately 4000 ml of water. Dilute to 5000
nl with water.
4.4 Sample Digestion and Analysis Reagents.
4.4.1 Hydrochloric Acid. Concentrated.
4.4.2 Hydrofluoric Acid. Concentrated.
4.4.3 Nitric Acid. Concentrated. Baker Instre-analyzed or equivalent.
4.4.4 Nitric Acid. 10 Percent (V/V). Add 100 ml of concentrated KNO, to
300 ml of water. Dilute to 1000 ml with water. Nil well. Reagent shall
contain less than 2 ng/al of each target metal.
4.4.5 Nitric Acid. 5 Percent (V/V). Add 50 ml of concentrated KNO, to
800 ml of wmter. Dilute) to 1000 ml with wmter. Reagent shall contain less
than 2 ng/ml of each target metal.
4.4.6 Water. To conform to ASTM Specifications DU93-T7. Typa II •
4.4.7 aydrojcylamine Bydrochlorld* and Sodium Chloride Solution. See EPA
Method 7470 for preparation.
4.4.8 Stannoua Chloride.
4.4.9 Potassium Permanganate, 5 Percent (V/V).
4.4.10 Sulfurlc Add. Concentrated.
4.4.11 Nitric Acid. 50 Percent (V/V).
4.4.12 Potaaaium Pereulfat*. 5 Percent (U/V).
4.4.13 Nickel Nitrate. Nl(NO,), 6H,0.
-------
4.4.14 Lanthanum Oxide,
4.4. 15 AAS Grade As Standard. 1000 ug/ml.
4.4,16 AAS Grade Be Standard, 1000 ug/nl.
4.4.17 AAS Grade Cd Standard. 1000 ug/nl-
4.4.13 AAS Grade Cr Standard. 1000 ug/ml.
4,4.19 AAS Grade Pb Standard. 1000 ug/ml.
4.4.20 AAS Grade HI Standard. 1000 ug/ml.
4.4.21 AAS Grade Ni Standard, 1000 ug/ml.
4.4.22 AAS Grade Zn Standard, 1000 ug/ml.
4.4.23 AAS Grade AI Standard. 1000 ug/ml.
4.4.24 AAS Grade Fe Standard. 1000 ug/ml.
4.4.25 AAS Grade Sb Standard. 1000 ug/ml. Optimal.
4.4.26 AAS Grade Ba Standard, 1000 ug/ml. Optional.
4.4.27 AAS Grade Cu Standard. 1000 ug/ol. Optional.
4.4.28 AAS Grade Nn Standard. 1000 uf/el. Optional.
4.4.29 AAS Grade P Standard. 1000 ug/el. Optimal.
4.4.30 AAS Grade Se Standard, 1000 ug/ml. Optimal.
4.4.31 AAS Grade Ag Standard. 1000 ug/el. Optional.
4.4.32 AAS Grade Tl Standard. 1000 ug/el. Optional.
4.4.33 The eetala standards may also be eade fro* aolld chemicals as
deacrlbed In EPA Method 200.7. EPA Method 7470 or Standard Methods for the
Analysis of Water and wastewater. 15tb Edition. Method 303? should be referred
to for additional Information on Mercury standards.
4.4.34 Mereyry Standards and Quality Control S«aple«. Prepare freih
weekly a 10 uf/al Intanedlate •ercury etandard by adding 5 •! of 1000 ug/al
mercury stock solution to * 500-el volusetric flask; dilute to 500 el by first
adding 20 •! of 15 percent HM)3 and then addiof water. Prepare a working
mercury standard solution fresh daily: edd 5 el of the 10 ug/el intermediate
standard to a 250 el volumetric flask end dilute to 250 ml with 5 ml of
4 percent KMnOt, 5 el of 15 percent HMO,. and then water. At least six
separate allquots of the working eercury standard solution should be used to
prepare the standard curve. These allquots should contain 0.0. 1.0. 2.0. 3.0,
4.0, and 5-0 ml of the working standard solution. Quality control samples
should be prepared by making a separate 10 ug/ml standard and diluting until in
the range of the calibration.
4.4.35 ICAP Standards and Quality Control Samples. Calibration standards
-------
for ICAP analysis can be combined into four different alxed standard solutions
as shown below.
MIXED STANDARD SOLUTIONS FOR ICAP ANALYSIS
Solution Eleaencs (secondary petal a in parar theses)
I As, Be, Cd, Pb, Zn (Kn, SB)
II Fa (Ba. Cu)
III Al, Cr, Nt
IV (Sb, P, Ag. Tl)
Prepare these standards by combining and diluting the appropriate volumes of
the 1000 ug/al solutions with 5 percent nitric acid. A minimum of one stan-
dard and a blank can be used to fora each calibration curve. However, a
separate quality control sample spiked with known amounts of the target metals
in quantities in the eidrange of the calibration curve should be prepared.
Suggested standard levels are 50 ug/al for Al, 25 ug/el for Cr and Pb, 15 ug/al
for Fe, and 10 ug/al for the remaining elements. Standards containing less
than I ug/«l of metal should be prepared dally. Standards containing greater
than I ug/al of aetal should be stable for a alnlaus) of 1 to 2 weeks.
4.4.36 Graphite Furnace AAS Standards for Arsenic, Cada\iua, and Lead (and
Antimony. Selenium, and Thalliusi). Prepare a 10 uf/al standard by adding l ml
of 1000 ug/al standard to a 100-al volumetric flask. Dilute to 100 el with 10
percent nitric acid. For graphite furnace AAS. the standards oust be aatrix
matched; e.g., if the samples contain 6 percent nitric acid and 4 percent
hydrofluoric acid, the standards should also be aade up with 6 percent nitric
acid and 4 percent hydrofluoric acid. Prepare a 100 ng/ml standard by adding
1 al of the 10 ug/al standard to a 100-al volumetric flask and dilute to 100 ol
with the appropriate matrix solution. Other standards should be prepared by
dilution of the 100 ng/ml standards. At least five standards should be used to
sake up the standard curve. Suggested levels are 0, 10, 50, 75. and 100 ng/ml.
Quality control saaples should be prepared by asking a separate 10 ug/al
standard and diluting until it is in the range of tha ses&lee. Standards
containing lass than i ug/al of aetal should be prepared daily. Standards
containing greater than 1 ug/al of aetal should be stable for a ainiaua of 1 to
2 weeks.
4.4.37 Matrix Modifiers.
4.4.37.1 Nickel Nitrate. 1 Percent (V/V). Dissolve 4.956 g of
Ni(N03},6^0 in approximately 50 al of water in a 100-al volumetric flask.
-------
Dilute to 100 •! with water.
l*.4.37.2 Nickel Nitrate. One-tenth Percent (V/V). Dilute 10 »1 of 1 per-
cenc nickel nitrate solution to 100 ml vith water. Inject an equal amount of
sample and this nodifler into the graphite furnace during AAS analysis for As.
4,4.37.3 Lanthanum. Dissolve 0.5864 g of La,0.j in 10 ml of concentrated
HNO-, and dilute to 100 ml with water. Inject an equal amount of sample and
this modifier into the graphite furnace during AAS analysis for Pb.
5. Procedure
5.1 Sampling. The complexity of this method Is such that, to obtain reli-
able results, teeters should be trained and experienced with the test procedure:
5.1.1 Pretest Preparation. Follow the same general procedure given in
Method 5. Section 4.1.1. except that, unless particulate emission* are to be
determined, the filter need not be desiccated or weighed. All sampling train
glassware should first be rinsed with hot tap water and then washed 'in hot
soapy water. Next, glassware should be rinsed three times with tap water.
followed by three additional rinse* with water. All glassware should then be
soaked in a 10 percent (V/V) nitric acid solution for a minimum of 4 hours,
rinsed three times with water, rinsed • final time with acetone, and allowed
to air dry. All glassware openings where contamination can occur should be
covered until the sampling train is assembled, prior to sampling.
5-1.2 Preliminary Determinations. Same as Method 5. Section 4.1.2.
5.1.3 Preparation of Sampling Train. Follow tbm seme general procedures
given in Method 5. Section 4.1.3, axcmpt pise* 100 ml of the nitric
acid/hydrogen peroxide solution (Section 4.2.1) in the two WOj/H^O, iapingers
(normally the second sad third impingmrs). place 100 ml of thm,acidic potassium
permanganate solution (Section 4.2.2) in the fourth and fifth Impinger, end
transfer approximately 200 to 300 g of preweighed silica gel from its container
to thm last iapinger. Alternatively, the silica gel may be weighed directly in
the impinger Just prior to train assembly.
Several options arm available to the tester based on the sampling
conditions. Tbm use of an empty first impi&tmr can be eliminated if the
moisture to be collected in thm imp infers is calculated or determined to be
less than 150 ml. The taster shall tnelude two impinger* containing the
acidic potassium permanganate solution for thm first test run, unless past
tee tine experience at thm same or similar sources has shown that only one is
-------
necessary. The last permanganate lapinger may be discarded if both
permanganate impingers have retained their original deep purple permanganate
color. A oaxiauM of 200 ml in each permanganate impinger (and a oaxiaua of
three peroanganate iapingers) nay b« used, if necessary, to ealntaln the
desired color in the l*»at pemanganate inplnger.
Retain Tor reagent blanks, 100 al of the nitric acid/hydrogen peroxide
solution and 100 ol of the acidic potassium permanganate solution. These
solutions should be labeled and treated as described in Section 7- Set up the
sampling train as shown in Figure A-l. If necessary to ensure leak-free
sampling train connections, Teflon tap* should be used instead of sillcone
grease to prevent contaalnation.
Precaution; Extreme care should b* taken to prevent contaalnation within
the train. Prevent the mercury collection reagent (acidic potassium
permanganate) from contacting any glassware of the train which is washed and
analyzed for Nn. Prevent hydrogen peroxide fro* mixing with the acidic
potassium permanganate.
5.1.4 Leak-Check Procedure*. Follow the leak-check procedures given-.in
Method 5. Section 4.1.4.1 (Pretest Leak-Cheek). Section 4.1.4.2 (Leak-Checks
During the Sample Run), and Section 4.1.4.3 (Post-Test Leak-Checks).
5.1.5 Sampling Train Operation. Follow the procedures given in Method 5,
Section 4.1.5- For each run. record the data required on a data sheet such as
the one shown in Figure 9*2 of Method 9-
5.1.6 Calculation of Percent Isokinetie. Same M Method 9. Section 4.1.6.
5.2 Sample Recovery. Begin cleanup procedures a* soon as the probe is
removed from the stack at the end of a sampling period.
The probe should be) allowed to cool prior to sample recovery. When it can
be safely handled, wipe off all external particulate utter near the tip of
the probe nocile and place a rinsed, non-eoDtsminatlnf cap over the probe
nozzle to prevent losing or gaining particulate matter. Do not cap the probe
tip tightly while the sampling train is cooling. This normally causes s vacuum
to form in the) filter holder, thus causing the undssired result of drawing
liquid from the implngers into the) filter.
Before moving the) sampling train to the cleanup site, remove the probe from
the sampling train and cap the open outlet. B» careful not to lose any
condensate that eight be present. Cap the filter inlet where the probe was
faatened. Remove the umbilical cord fro* the) last impinger and cap the
-------
impinger. Cap off the filter holder outlet and Impinger inlet. Die non-
contaainating caps, whether ground-glee* stoppers, pleetic cepe. serum caps.
or Teflon tape to close these openings.
Alternatively, the train can be disassembled before the probe and niter
holder/oven are completely cooled, if this procedure is followed: Initially
disconnect the filter holder outlet/iapinger inlet and loosely cap the open
ends. Then disconnect the probe fro* the filter holder or cyclone inlet and
loosely cep the open end*. Cap the probe tip end reeove the umbilical cord as
previously described.
Transfer the probe and filter-impinger assembly to a cleanup area that is
clean and protected from the wind and other potential causes of contamination
or loss of sample. Inspect the train before and during disassembly and note
any abnormal conditions. The sample is recovered and treated as follows (see
schematic in Figure A-2). Assure that all itema necessary for recovery of the
sample do not contaminate it. - - - •
5.2.1 Container No. 1 (Filter). Carefully remove the filter from the
filter holder and place it In its identified petri dish container. Acid-
washed polypropylene or Teflon coated tweezers or clean, disposable surgical
gloves rinsed with water should be used to handle the filters. If it is
necessary to fold the filter, make certain the participate cake is inside the
fold. Carefully transfer the filter and any partlculate matter or filter
fibers that adhere to the filter holder gasket to the petrl dish by using a dry
(acid-cleaned) nylon brittle brush. Do not use any metal-containing materials
when recovering this train. Semi the labeled petri dish.
5-2.2 Container No. 2 (Acetone Ulnae). Talcing care to see that dust on
the outside of the probe or other exterior surfaces does not gee Into the
sample, quantitatively recover particulate matter and any condensate from the
probe noiile. probe fitting, probe liner, and front half of the filter holder
by washing these componentjs with 100 ml of acetone and placing the wash in a
glass container. Motet The use of exactly 100 el la necessary for the
subsequent blank correction procedures. Dlatllled water may be used instead of
acetone when approved by the Administrator and ahall be used when specified by
the Administrator; in theae cases, save • water blank and follow the
Administrator's directions on analysis. Perfora the acetone rinses as follows:
Carefully remove the probe nozzle and clean the inside surface by rinsing with
acetone from a waah bottle and brushing with a ncnmetallic brush. Brush until
-------
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-------
the acetone rinse shows no visible particles, after which make a final rinse of
the inside surface with acetone.
Brush and rinse the inside pares of the Swagelok fitting with acetone In a
sinilar way until no visible particles remain.
Rinse the pnjbe liner with acetone by tilting and rotating the probe while
squirting acetone into its upper end so that all inside surfaces will be wetted
with acetone. Allow the acetone to drain from the lower end into the sample
container. A funnel say be used to aid in transferring liquid washings to che
container. Follow the acetone rinse with a nonjsetallic probe brush. Hold the
probe in an inclined position, squirt acetone Into the upper end as the probe
brush is being pushed with a twisting action through the probe: hold a
saaplecontalner underneath the lower end of the probe, and catch any acetone
and partlculate Batter which is brushed through the probe three tiees or acre
until no visible partlculate matter is carried out with the acetone or until
none remains in the probe liner on visual inspection. Rinse the brush with
acetone, and quantitatively collect these washings in the sample container.
After the brushing, take a final acetone rinse of the probe aa described above.
It is recommended that two people clean the probe to ainimite sample
losses. Between sampling runs, keep brushes clean and protected fro»
contamination.
Clean the inside of the front half of the filter holder by rubbing •
surfaces with a nonmetallie nylon bristle brush and rinsing with acetor
Rinse each surface three times or sere if needed to remove visible partlculate.
Make a final rinse of the brush and filter holder. After all acetone washings
and particulate matter have been collected In the sample container, tighten the
lid on the sample container so that acetone will not leak out when it is
shipped to tha> laboratory. Hark the height of the fluid level to determine
whether or not leakage occurred during transport. Label the container clearly
to identify its contents.
5.2.3 Container No. 3 (Probe Rinse). Rinse the) probe liner, probe nozzle,
and front half of the filter holder thoroughly with 100 ml of 0.1 N nitric acid
and place the wash into a sample storage container. Hote: The use of exactly
IX ml is necessary for the subsequent blank correction procedures. Perform
the rinses as described la Method 12. Section $.2.2. Rscord the volume of the
combined rinse. Nark the height of the fluid level on the outside of the
storage container and use this mark to determine if leakage occurs during
-------
transport. Seal the container and clearly label the contents. Finally, rinse
the nozzle, probe liner, and front half of the filter holder with water
followed by acetone and discard these rinses.
5-2.14 Container No. 4 (Impingers 1 through 3. Contents and Rinses). Due
cc the large quantity of liquid involved, the tester «ay place the inpinger
solutions in sore than one container. Measure the liquid in the first three
impingers volutietrically to within 0.5 •! using a graduated cylinder. Record
the voluae of liquid present. This information is required to calculate the
moisture content of the stapled flue gas. Clean each of the first three
lapingera. the filter support, the beck half of the filter housing, and
connecting glassware by thoroughly rinsing with 100 ml of 0.1 N nitric acid as
described in Method 12. Section 5-2.4. Note; The use of exactly 100 ml of 0.1
N nitric acid rinse is necessary for the subsequent blank correction
procedures. Combine the rinses and iapinger solutions, measure and record the
volume. Calculate the 0.1 N nitric acid rinse volume by difference. Mark the
height of the fluid level on the outside of the container to determine if
leakage occurs during transport. Seel the container and clearly label the
contents.
5-2.5 Container No. 5 (Acidified Potassium Permanganate Solution and
Rinses, lapingers No. 415)- Pour all the liquid from the permanganate
iapingere (fourth and fifth, if two permanganate impingers are used) into a
graduated cylinder and measure the volume to within 0.5 sd. This information
is required to calculate the moisture content of the sampled flue gas. Using
100 ml total of the acidified potassium permanganate solution, rinse the
permanganate impingmr(s) and connecting glass pieces a minimum of three tiaea.
Combine toe rinses with the permanganate implnger solution. Finally, rinse the
permanganate iapingmr(s) and connecting glassware with 50 ml of 8 N HC1 to
remove any residue. Mote: The use of exactly 100 ml and 50 ml for the two
rinses is necessary for the subsequent blank correction procedures. Place the
combined rinses and isplnger contents in a labeled glass storage bottle. Mark
the height of the) fluid level on the outside of the bottle to determine if
leakage occurs during transport. See the following note and the Precaution in
Paragraph U.2.2 and properly seel the bottle and clearly label the contents.
Note; Due to the potential reaction of the potaasluB permanganate with the
acid, there may be pressure buildup in the sample storage bottles. These
bottle* should not be filled full and should be vented to relieve excess
-------
pressure. Venting is highly recommended. A No. 70-72 hole drilled in the
container cap and Teflon liner has be«n found to allow adequate venting without
loss of sample.
5.2.6 Container No. 6 (Silica del). Note the color of the indicating
silica gel co determine whether it has been completely spent and nake s
notation of its condition. Transfer the silica gel froe its impinger to its
original container and seal. The tester may use a funnel to pour the silica
gel and a rubber policeman to remove the silica gel from the impinger. The
small amount of particles that may adhere to the Iapinger wall need not be
removed. Do not use water or other liquids to transfer the silica gel since
weigf rained in the silica gel iapinger is used for aoisture calculations.
Alter- .itively, if a balance is available in the field, record the weight of
the spent silica gel (or silica gel plus Iapinger) to the nearest 0.5 g.
5.2.7 Container No. 7 (Acetone Blank). Once during each field test, place
100 al of the acetone used in the saaple recovery process into a labeled
container for use in the front half field reagent blank. Seal the container.
5.2.8 Container No. 3 (0.1 N Nitric Acid Blank). Once during each field
teat, place 200 al of the 0.1 N nitric acid solution used in the saaple
recovery process into a labeled container for use in the front half and back
half field reagent blanks. Seal the container.
5.2.9 Container No. 9 (51 Nitric Acid/IOS Hydrogen Peroxide Blank). Once
during each field test, place 200 ml of the 5* nitric acid/10* hydrogen
peroxide solution used as the nitric acid impinger reagent into a labeled
container for use la the back half field reagent blank. Seal the container.
5-2.10 Container Mo. 10 (Acidified Potassium Peraangmnate Blank). Once
during each field test, place 300 al of the acidified potassium permanganate
solution used as the iapinger solution and in the sample recovery process into
a labeled container for use in the back half field reagent blank for mercury
analysis. Seel the container.
Note? This container should be vented, as described in Section 5-2.4. to
relieve excess pressure.
5.2.11 Container No. 11 (8 N HC1 Blank). Once during each field test,
place 50 al of the 8 N hydrochloric acid used to rinse the acidified potassiua
permanganate tapingers Into a labeled container for use In the back half
reagent blank for mercury.
5.2.12 Container No. 12 (Filter Blank). Once during each field test,
-------
place an unused filter from the same lot as the sampling filters in a labeled
petri dish. Seal the petri diah. This will be used in the front half field
reagent blank.
5-3 Sample Preparation. Note the level of the liquid in each of the
containers and determine if any sample was loit during shipment. If a
noticeable amount of leakage has occurred, either void the sample or use
oethods. subject to the approval of the Administrator, to correct the final
results. A diagram illustrating sample preparation and analysis procedures for
each of the sample train components is shown la Figure A-3.
5.3.1 Container No. l (Filter). If particulate emissions are being
determined, then desiccate the filter and filter catch without heat and weigh cc
a constant weight as described in Section 4.3 of Method 5. For analysis of
metals, divide the filter with its filter catch Into portions containing
approximately 0.5 g each and place Into the analyst's choice of either
individual microwave pressure relief vessels or Parr" Bombs. Add 6 ml of
concentrated nitric acid and 4 ml of concentrated hydrofluoric acid to each
vessel. For microwave heating, microwave thm sample vessels for approximately
12-15 minutes in Intervals of 1 to 2 minute* at 600 Watts. For conventional
heating, heat thm Parr Bombs at 140°C (2B5»F) for 6 hours. Then cool che
samples to room temperature and combine with thm acid digested probe rinse as
required in Section 5-3-3. below.
Notes: 1. Suggested microwave heating times arm approximate and are dependent
upon the number of samples being digested. Twelve to 15 minute
heating tlmms have bmmn found to be acceptable for simultaneous
digestion of up to 12 individual samples. Sufficient heating is
evidenced by sorbmnt reflux within tnm vmmsml.
2. If thm sampling trmln usms an optional cyclonm, thm eyeIons catch
should bm prepared and digested using thm saam procedures described
for thm filters and combined with the digested filter samples.
5.3.2 Container No. 2 (Acetone Riase). Not* thm level of liquid in the
container and confirm on thm analysis shmmt vhmthmr or net leakage occurred
during transport. If • noticeable amount of leakagm hms occurred, either void
thm sample or use methods, subject to thm approval of thm Administrator, to
cornet thm final results. Mmasurm thm liquid in this container either
volummtricslly to *l ml or grmvimmtrically to ±0.5 ff> Transfer thm contents to
an acid-cleaned tared 250-ml beaker and mvapormtm to drynass at ambient Figure
-------
Container }
•eld Prat* HIM
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oa II
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Figure A~3- Saaple preparation and analysis
by MS, If dolrtd
-------
temperature and pressure. (If particulate emissions are being determined.
desiccate for 2k hour* without heat, weigh to a constant wight according to
the procedures described in Section 4.3 of Method 5, and report the results to
the nearest 0.1 mg.) Reaolubilize the reiidue with concentrated nitric acid and
combine the resultant sample including all liquid and any partlculate Batter
with Container No. 3 prior to beginning the following Section 5.3-3.
5.3.3 Container No. 3 (Probe) Rinse). The pH of this Maple shall be 2 or
lower. If the pH la higher, the sample ahould be acidified with concentrated
nitric acid to pH 2. The sample should be rinsed into a beaker with water and
the beaker ahould be covered with a ribbed wetchglaae. The sample voluae shculc
be reduced to approximately 50 ml by heating oa a hot plate at a temperature
Juat below boiling. Injpect the sample for visible perticulate aatter. and
depending on the reaulta of the inapectlon. perform one of the following. If nc
partlculate Matter la observed, coebine the sample directly with the acid
digested portlona of the filter prepared previously in Section 5.3.1. If
particulate Batter la observed, digest the aaaple in microwave vessels or Parr"
Bombs following the procedures described in Section 5-3-1; then coabtne the
resultant sample directly with the acid digested portions of the filter prepared
previously in Section 5-3-1. The resultant combined aample is referred to as
Fraction 1. Filter the combined solution of the acid digested filter and probe
rinse samples using Whatman 541 filter peper. Dilute to 300 al (or the
appropriate volume for the expected metals concentration) with water. Measure
and record the combined volume of the Fraction 1 solution to within 0.1 ml.
Quantitatively remove • 50-ml aliquot and label as Fraction IB. Label the
remaining 250-al portion aa Practice 1A. Fraction 1A is used for ICAP or AAS
analysis. Fraction IB la used for the determination of front half mercury.
5-3-** Container No. 4 (Xmpingers 1-3). Measure and record the total vol-
ume of this sample (Fraction 2) to within 0.5 ml. Remote a 50-al aliquot for
mercury analyei* and label aa Fraction 2B. Label the remaining portion of
Container No. 4 aa Fraction 2A. The Fraction 29 aliquot ahould be prepared and
analyzed aa described la Section 5-^.3. Fraction 2A shall be pB 2 or lover.
If necessary, use concentrated nitric acid to loner Fraction 2A to pB 2. The
sample should be rinaed into e beaker with water end the beaker ahould be
covered with a ribbed watcnglasa. The sample volume ahould be reduced to
approximately 20 ml by heatlna; on a hot plate at a temperature Juat below
boiling. Then follow either of the digestion procedures described in Sections
-------
5,3-«-l and 5.3-<*.2, below.
5.3,4.1 Conventional Digestion Procedure. Add 30 ml of 50 percent nitric
acid and heat for 30 minutes on a hot place to Just below boiling. Add 10 ol of
3 percent hydrogen peroxide and heat for 10 acre alnutaa. Add 50 al of hot
water and heat the sample for an additional 20 aiiutaa. Cool, filter the
sample, and dilute to 150 al (or the appropriate volume for the expected aetals
concentrations) with water.
5.3.U.2 Microwave Digmstion Procedure. Add 10 al of 50 percent nitric
acid and heat for 6 alnutea in interval! of 1 to 2 ainutea at 600 Watts. Allow
the sample to cool. Add 10 al of 3 percent hydrogen peroxide and heat for 2
more ainutea. Add 50 al of hot water and heat for an additional 5 ainutas.
Cool, filter the sample, and dilute to 190 ml (or the appropriate volume for the
expected metals concentrations) »ith water.
Note: All microwave heating times given are approximate and are dependant
upon the number of samples being digeated at • time. Heating time* as given
above have been found acceptable for simultaneous digestion of up to 12
individual samples. Sufficient heating la evidenced by solvent reflux within
the veaael.
5-3.5 Container Mo. 5 (Implngera 4 4 5). Haaaure and record the total
volume of this sample to within 0.5 ml. This aample la referred to aa Fraction
3, Follow the analyala procedure* described in Section 5.4.3.
5-3-6 Container No. 6 (Silica 0ml). Weigh the spent ailica gel (or silica
gel plus impinger) to the nearest 0.5 g umioff a balance. (This step
may be conducted la the field.)
5-4 Sample Analyala. For each sampling train, five individual samples are
generated for analysis. A schematic identifying each aample and the prescribed
sample preparation and analyeia scheme la shown in Figure A-3. The first two
samples, labeled Fraction* 1A and IB. canalst of the digs*tad samplea from the
front half of tbm train. Fraction 1A la for ICAP or AA3 aaalyaia am described
in Section* 5.4.1 and/or 5.9.2. Fraction IB 1*) for determination of front half
mercury am described la Saction 5-4.3-
The bade hmlf of tbm train warn used to prepare tbm third through fifth
samples. Tbm third and fourth samples, labeled Fractions 2A sad 2B. contain
the digested samples from tbm HjO and HNO]/B>Oa Implngars 1 through 3- Frsctioi
2A is for ICAP or AAS analysis. Fraction 2B will be analysed for mercury.
The fifth sample, labeled Fraction 3. consists of the impinger contents and
-------
rinses froa the permanganate Ispinger* 4 and 5. This sample is analyzed for
aercury as described in Section 5.4.3. The total back half mercury catch is
determined from the SUB of Fraction 2fi and Fraction 3.
5.^.1 ICAP Analysis. Fraction 1A and Fraction 2A are analyzed by ICAP
using EPA Method 200.7 C*0 CFR 136. Appendix C). Calibrate the ICA?. and set up
an analysis program as described in Method 200.7- The quality control proce-
dures described in Section 7-3-1 of this Mthod shall be followed. Recoamended
wavelengths for use in the analysis of the primary, secondary, and ineerferring
metals are listed belov.
Element Wavelength (am)
Arsenic
Beryllium
Cadmium
Chromium
Lead
Nickel
Zinc
Antimony
Barius)
Capper
Manganese:
Selealua
Silver
Thallium
Aluminum,
Iran
193.696
313- CW2
226.302
267-716
220.333
231.604
213.856
206.833
455- <»03
321.794
257.610
196.026
328.063
190.864
306.215
259-940
The wavelengths llatad are reeoaswjndsd because) of their sensitivity and overall
acceptance. Otter wavelengths say bs substituted if they can provide the
needed sensitivity and are traatsd with tha iaua corrective techniques for
spectral interference.
Initially, analyie all saaples for the target aetals plus iron and
alualnua. If iiea and aluainua are present in the saaple, the sample aay hav«
to be diluted so that each of ebasa elsswnts is at a concentration of less than
50 ppej to reduce their spectral interferences on arsenic and Isad.
Note: When analysing samples in a hydrofluoric acid matrix, an alumina
torch should be used; sine* all front half samples will contain hydrofluoric
acid, use an alumina corch.
-------
5.4.2 AAS by Direct; Aspiration and/or Graphite Furnace. If analysis of
metals in Fraction 1A and Fraction 2A using graphite furnace or direct
aspiration AAS is desired, Table A-2 should be used to determine which
techniques and methods should be applied for each target metal. Table A-2
should also be consulted to determine possible interferences and techniques to
be followed for their minimization. Calibrate the instrument according to
Section 6.3 and follow the quality control procedures specified in Section
7.3-2.
5.^.3 Cold Vapor AAS Mercury Analysis. Fraction IB, Fraction 2B. and
Fraction 3 should be analyzed for aercury using cold vapor atomic absorption
spectroscopy following the method outlined in EPA Method 7^70 or in Standard
Methods for Mater and wastewater Analysis. 15th Edition, Method 3Q3F. Set up
the calibration curve as described in Section 7.3 of Method 303?. Add
approximately 5 ml of each sample to BOD bottle*. Record the amount of sample
added. The amount used is dependent upon the expected levels of aercury."
Dilute to approximately 120 ml with mercury-free water. Add approximately 15
ml of 5 percent potassium permanganate solution to the Fraction 2B and Fraction
3 samples. Add 5 percent potassium permanganate solution to the Fraction IB
sample as needed to produce a purple solution lasting at least IS minutes. A
ainimum of 25 al is suggested. Add 5 al of 50 percent nitric acid. 5 «1 of
concentrated sulfuric acid, and 9 ml of 5 percent potassium persulfate to each
sample and each standard. Digest the solution in the capped BOD bottle at 95°C
(205°F) in a convection oven or water bath for 2 hour*. Cool. Add 5 al of
hydroxylamine hydrochloride solution and mix the sample. Then add 7 al of
stannous chloride to each sample and analyze immediately.
6. Calibration
Maintain a laboratory log of all calibrations).
6.1 Sampling Train Calibration. Calibrate the sampling train components
according to Che indicated sections of Method 5« Probe Motile (Section 5.1);
Pitot Tube (Section 5-2); Metering System (Section 5-3): Probe Heater (Section
5-4); Temperature Gauge* (Section 5-5); Leak-Check of the Metering System
(Section 5.6); and Barometer (Section 5-7).
6.2 Inductively Coupled Argon Plasma Spectrometer Calibration. Prepare
standards am outlined in Section 4.4. Profile and calibrate the instrument
according to the instrument manufacturer's recommended procedures using the
-------
TABLE A-2. APPLICABLE TECHNIQUES. METHODS. AND MINIMIZATION OF 1NTEFERENCE KOH AAS ANALYSIS
Metal
Sb
Sb
Aa
Ba
Be
Be
Cd
Cd
Cr
Cr
Technique
Aspiration
Pumace
Purnaca
Aspiration
Aapiration
Pumaca
Aspiration
Purnace
Aaplration
Pumaca
Method
No.
70*10
70*1
7060
7060
7090
7W1
7130
71JI
7190
7191
Wavelength
(i»)
217.6
217.6
193-7
553.6
23*-9
23* .9
22fl.0
228.8
357-9
357-9
Inlerfei
Cause
1000 Bg/al Pb
Ni, Cu, or acid
High Pb
Arsenic wolati -
zation
Aluainiu*
Calciua
Bariua ionization
500 pp. Al
High Mg t Si
Be in optical path
Absorption & light
scattering
Aa above
Excess chloride
Plpat tips
Alkali aetai
Absorption & scatt
200 eg/L cafciua
& phosphate
rence.
NtniBization
Use secondary wavelengin or ifjl.l raa.
Match saaple i standards acid concentration
or use nitrous oxide/acetylene flaae
Secondary wavelength or Zeeaan correction
Spiked saaples ft add nickel nitrate solution
to digestates prior to analyses
Use Zeeman background correction
High hollow cathode current t narrow band set
2 aL of IC1 per 100 aL of saaple
Add O.lf fldUride
Use Method 'of standard additions
Optiaixe paravetera to aiainlze effects
Background correction is required
Aa above
Aaaooiua phosphate used as a aatrix aodifler
Use cad»iuB-rree tips
KC1 ionization suppressant in saaple ft stand
Consult manufacturer's literature
All calciua nitrate For a know constant effect
and to eliminate effect of phosphate
(continued)
-------
TABLE A-2 (CONTINUED)
Metal
Cu
Fe
Pb
Pb
Nn
Ni
Se
AC
Tl
Tl
Zit
Technique
Aspiration
Aspiration
Aspiration
Furnace
Aspiration
Aspiration
Furnace
Aspiration
Aspiration
Furnace
Aspiration
Method
No.
7210
7380
742O
7421
7460
7520
77*10
7760
7840
7841
7950
Wavelength
<•»)
124.7
248.3
283-3
283-3
279-5
232.0
196.0
328.1
276.8
276.8
213 9
Inlerfci
Cause
Absorpt & scatter
Contamination
217.0 am alternat
Poor recoveries
403.1 nm altemal
352.4 nm allernal
Fe. Co. I Cr
Nonlinear respons
Volitality
Adsorpt I scatter
Absorpt I scatter
AgCl insoluble
Viscosity
Hydrochloric acid
or chloride
.c
High Si. Cu 1 P
Con taai nut ion
•ence
Niniaizaiion
Consult atanufac Mirer's uaiui.il
Great care taken to aviutl i:inii.;iainiiii.iuii
Background correction required
Matrix a>odifier. add 10 ul. ol' phosphorus acid
to 1-aL of prepared saaple in suapler cup
Background correction required
Rackground correction required
Matrix Batching or a nitrous-oxide/acety Tlaae
Sanple dilution or uae 3^2.4 na line
Spike saaplea 4 reference aaleriala & add nicke
nitrate to alnlalze volatllizallon
Background . urrection is required i Zeeaan
background correction can be useful
Background correction ia required
Avoid hydrochloric acid unless silver la in
solution aa a chloride coaplex
Saople & standards aonl tared Tor apiration rate
Background correction is required
Hydrochloric acid should not be used
Background correction is required
Verify that losses are not occuring for
volitizatlon by spiked aaaplea or standad addt
Palladium is a suitable aairix aodifier
Stroiitiua removea Cu and phuspliaLe
Care should be taken to avid ctmtaainai Ion
-------
above standards, 'ihe Instrument calibration should be checked once per hour.
If the instrument does not reproduce the concentrations of the standard within
10 percent, the complete calibration procedures should be performed.
6.3 Atoaic Absorption Spectrometer - Direct Aspiration. Graphite Furnace
and Cold Vapor Mercury Analysea. Prepare the standards as outlined in Section
k.k. Calibrate the spectrometer using these prepared standards. Calibration
procedures are also outlined in the Q»A methods referred to in Table A-2 and in
Standard Methods for Water and wastewater. 15th Edition, Method 303F (for
mercury). Each standard curve should be run in duplicate and the Man values
used to calculate the calibration line. The instrument should be recalibrated
approximately once every 10 to 12 samples.
7. Quality Control
7.1 Sampling. Field Reagent Blanks. Thm blank samples in Container
Numbers 7 through 12 produced previously In Sections 5.2.7 through 5.2.11.
respectively, shall be processed, digested, and analyzed as follows- Digest
and process Container No. 12 content* per Section 5-3.1. Container No. 7 per
Section 5-3.2. and half of Container No. 8 per Section 5-3.3- This produces
Fraction Blank 1A and Fraction Blank IB from Freetion Blank 1. Combine the
remaining half of Container No. 8 with the contents of Container No. 9 and
digest and process the resultant volume per Section. 5.3.4. This produces
Fraction Blank 2A end Fraction Blank 28 from Fraction Blsnk 2. Container No. 1(
and Container No. 11 contents are Fraction Blank 3> Analyse Fraction Blank 1A
and Fraction Blank 2A oar Section 5-4.1 and/or 5.4-2. Analyse Fraction Blank
IB. Fraction Blsnk 2B. and Fraction Blank 3 par Section 5.4.3* The analysis of
Fraction Blank 1A produce* the front half reagent blank correction values for
the metals except mercuryt the analysis of Fraction Blank IB produces the front
half reagent blank correct value for mercury. The analysis of Fraction Blank 2>
produces the) back half reagent blank correction values for the metals except
mercury, while separata analysla of Fraction Blanks 28 and 3 produce the back
half reagent blank correction value for mercury.
7.2 An attempt may be made to deteraUae if the laboratory reagents used in
Section 5.3 cauaed contamination. Tbay should be analysed by the procedures in
Section 5.4. Thm Administrator will determine whether or not the laboratory
blank reagent values can be used la the calculation of that stationary source
teat results.
-------
7.3 Quality Control Samples. The following quality control samples should
be analyzed.
7,3.1 ICAP Analysis. Follow the quality control shown in Section 8 of
Method 6010, For the purposes of e three run test series, thsse requirements
have been modified to include the following: two inatniMnt check standard
runs, two calibration blank run*, one Interference cheek sample at the
beginning -f the analytic (must be within 25X or analyze by standard addition).
one quality control sample to check the accuracy of the calibration standards
(must be within 259 of calibration). and one duplicate analysii (must be wichm
5X of average or repeat all analysis).
7.3.2 Direct Aspiration and/or Graphite furnace AAS Analysis for Arsenic,
Beryllium, Cadmium. Chromium. Lead. Mercury. Nickel, and Zinc (and Antimony,
Bariua, Copper. Manganese, Phosphorus. Seleniusj, Silver, and Thallium:, if
neasured). All samples should be analyzed in duplicate. Perform a aatrix spike
on one front half sample and one back half sample or one combined sampler If
recoveries of less than 75 percent or greater than 125 percent are obtained for
the aatrix spike, analyze each sample by the method of additions. A quality
control sample should be analysed to check the accuracy of the calibration
standards. The results muse be within 10X or the calibration repeated.
7.3.3 Cold Vapor AAS Analysis for Mercury. All samples should be analyzed
in duplicate. A quality control sample should be analyzed to check the accuracy
of the calibration standards (within 10* or repeat calibration). Perfora a
aatrix spike on one sample froe the nitric iapinger portion (must be within 151
or samples must be analysed by the method of standard additions). Additional
information on quality control can be obtained from BPA Method 7470 or in
Standard Methods for water and waatewater. 15th Edition. Method 303F.
3. Calculations
8.1 Dry Oaa Volume. Using the data from this teat, calculate va(BIC,. the
dry gas sample volume at standard conditions aa outlined la Section 6.3 of
Method 5.
8.2 Volume of Hater Vapor and Moisture Content. Using the data obtained
from this teat, calculate the volume of water vapor V-(-l-, and the eolsture
content BVi of the stack gas. Use Equations 5-2 and 5-3 of Method 5-
8.3 Stack Gas Velocity. Using the data from this teat and Equation 2-9 of
Method 2, calculate the average stack gas velocity.
-------
8.4 Netala (Except Mercury) In Source Staple.
8.4.1 Fraction 1A, Front Half, Metals (except Hf). Calculate the amount
of each metal collected in Fraction 1 of the •aaplinf train uainf the following
equation:
"r* ' C. F, V..I(lil Sq. 1«
where .*
Nrn • total MM of each Mtal (except Hf) collected in the
front half of the aaaplinf train (Fraction 1), uf.
Ct * concentration of aetal in eaaple Fraction 1A aa read froa the
standard curve (uf/al).
F4 • dilution factor (F4 a the inverae of the fractional portion of the
concentrated saaple in the solution actually uaed in the inatruaent t<
produce the reading C,. For exaaple. when the dilution of Fraction L
la fro* 2 to 10 el, Pd -5).
vioin.i " total voluae of difeited aaaple aolution (Fraction 1), al.
8.4.2 Fraction 2A, Bade Half, Natal a (except Hf). Calculate the Mount of
each natal collected in Fraction 2 of the eaaplinf train uainf the following
equation.
*>„ - C. F. V. Eq. £•
where:
^h • total aaaa of each eetal (except Hf) collected in the back half
of til* aaaplinf train (Fraction 2). uf.
Ca • concentration of aetal in aaaple Fraction 2A. aa read froa the
atandard curve (uf/al).
F4 • aliquot factor, voluae of Fraction 2 divided by voluae of aliquot
Fraction 2A.
V. • voluae of difeated taaple analysed (concentrated Fraction 2A), al.
8.4.3 Total Train, letala (except Hf). Calculate the total aaount of each
of the quantified aetala collected in the aaaplinf train aa follc
•If Fractiona LA and 2A are coablned. proportional aliquot* mat be uaed.
Appropriate chanfea auat be aade in iquatlona 1-3 to reflect thla approach.
-------
where:
Mt « total oaas of each metal (separately stated for each »etal) collected
in the sampling train, ug.
MfnB * blank correction value for Baas of Beta! detected in front half
field reagent blank, ug .
Mbnb • olank correction value for ease of Mtal detected in back half
field reagent blank, ug.
Note: If the aeaaured blank value for the front half (af||1) is in the range O.C
to A ug [where A ug equals the value determined by multiplying 1.4 ug per squar<
inch (1.4 ug/in.3) time* the actual area in square inches (in.3) of the filter
used in the emission sample]. •ff)b aay be used to correct the emission sample
value («,»); if «fh» eaceeds A ug. the greater of the two following values
(either I. or II.) may be used:
I. A ug, or
II. the leaser of (a) ernb. or l Bq. *
Vfii
where:
Hgfll • total Bass of mercury collected in the front half of the sampling
train (Fraction i), ug.
Q,h • quantity of mercury in analyzed sample, ug.
v,om i * total volume of digested • ample solution (Fraction 1). ml.
VM| * volume) of Fraction IB analyzed. ml. See the following Note.
Note; VP1| is the actual amount of Fraction IS analyzed. For example, if 1 ml
of Fraction IB were diluted to 100 ml to bring it into the proper analytical
range, and 1 ml of the 100-ml dilution was analyzed, Vfli would be 0.01.
8.5.2 Fraction ZB and Fraction 3, Back Half, if. Calculate the amount of
•ercury collected in Fractions 2 and 3 using Equations 5 sad 6. respectively.
-------
Calculate the total Mount of aercury collected in the back half of the sampling
train using Equation 7-
« V.OIB.I Eq- 5
11
where:
Hfbh, • total MM of Mrcury collected in Fraction 2. u».
Qbh, • quantity of Mreury in analyzed aaaple, uf.
Vfai • voluM of Fraction 2B analyzed, al (Me Note in
Section 8.5.1).
, • total volume of Fraction 2, ml.
, 4
vr,.
where:
HfbhJ • total aaaa of aercury collected in Fraction 3. uff.
QbhJ • quantity of aercury in aaal/ied taaple, u«.
VM • voluae of Fraction 3 analyzed, al (tee Mete in
Section 8.5.1).
vioin.j ' cotal voluM of Fraction 3. al.
J Bq. 7
where:
h • total MM of aercury collected la the back half of the saaplinj
train, uff.
8.5-3 Total Train Mercury Catch. Calculate the total Mount of aercury
collected la the essplinc train uolng Bquatloa 8.
•here:
Nt • total MM of eercury collected la the taaplinf train, uf.
Hffhb • blank correction value for MM of aercury detected ia front half
field reagent blank, of.
-------
• blank correction value for mass of mercury detected in back
half field reagent blank, ug.
Note: If the total of the neasured blank values (HgThft • Hgbni() is in the rang.
of 0 to 3 ug, then the total may be used to correct the emission sample value
(Hgrh • Hgeh); if it exceeds 3 ug. the greater of the following two values say
be used: 3 ug or 5 percent of the emission sample value (Hgfh • Hgbh).
8.6 Metal Concentration of Stack Gas. Calculate the concentrations of
arsenic, beryllium, cadmium, total chromium, lead, mercury, nickel, and zinc
(and antimony, barium, copper, manganese, phosphorus, selenium, silver, and
thallium, if measured) in the stack gam (dry basis, adjusted to standard
conditions) as follows:
C. ' K* Eq.9
where:
C( • concentration of each metal In the stack gas, mg/dscm.' ~
K, • 10-5 mg/ug.
Mt • total mass of each aetal collected in the sampling train, ug.
v.dta> • volume of gam sample mm measured by the dry gmm meter, corrected
to dry standard conditions, dsem.
8.7 Isokinetic Variation and Acceptable Results. Same as Method 5,
Sections 6.11 and 6.12. respectively.
9- Bibliography
9.1 Method 303P In Standard Methods for the Examination of Mater
Wastewater. 15th Edition, I960. Available from the American Public Health
Association, 1019 18th Street N.H., Washington, D.C. 20036.
9-2 EPA Methods 6010. 7000, 7041, 7060, 713L 7*21. 7470, 7740, end ?84l.
Test Methods for Evaluating Solid Waste: Phyilcml/CI*—<"** «-»h~i. SW-846.
Third Edition. September 1988. Off 1cm of Solid Hamtsj «nd Emergency Response.
U. S. Pin li nimminsl Protection Agency, Washington, D.C. 20460.
9.3 EPA Nmtbod 200.7, Code of Federal Regulations. Title 40. Part 136.
Appendix C. July 1. 1967.
9.4 EPA Methods 1 through 5, Cod* of Federal Regulations. Title 40, Part
60. Append!* A. July 1. 196?.
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APPENDIX J.2
PM10/CPM
-------
Federal Register / Vol. 55. No. 74 / Tuesday. April 17. 1990 / Rules and Regulations 14249
them lo be erroneously measured as
PM».
Drying and shrinking is not thought to
be a problem. Should it be considered a
problem, the tester could choose Method
201A in which there it no recycle gas.
Another commenler said that the use
of recycle gas increases velocity in the
cyclone which could cause friable
particles to break up, becoming PMio.
Prior to size classification by a PM,«
cyclone, (here is no known or suspected
mechanism by which friable particles,
should they exist, may break up. When
particles greater than 10 jim
aerodynamic size reach the cyclone wall
due lo their inertia, they are collected.
One commenter said that no
consideration is made in either method
of the gas density, gas viscosity, or of
the density of the particutate matter
being measured.
Gas density and viscosity are
compensated for in the calculations for
both PMjo methods. Because the
aerodynamic diameter of PMio
emissions is used in both PMio methods,
determination of particle densities,
volumes, or shapes is not necessary and
would be redundant.
Another commenler said if the PMio
measurement ia made downstream of an
electrostatic precipitater (ESP), then the
particles will carry an electric charge
and the measurement of PMio by these
methods will be a flee ted.
The effect of an ESP on partide sizing
when using Method 201 or 201A ia
considered to be negligible.
There was concern by the commenters
that the paniculate matter may settle
out inaide the sample train.
The trains have been calibrated with
lest aerosols and the relative accuracies
to each other have been established.
These tests results and the operation
principles of both methods have shown
that "settling" ia.no! a problem. The
particles travel only 1.5 to 3 in. [nozzle
length) prior to size classification by the
trains.
IV. Administrative
The docket is an organized and
complete file of aU the information
considered by EPA in the development
of this rulemaking. The docket is a
dynamic file since material is added
throughout the rulemaking development.
The docketing system Is intended to
allow members of the public and
industries involved lo identify readily
and locate documents so that they can
effectively participate in the rulemaking
process. Along with the statement of
basis and purpose of the proposed end
promulgated teat method revisions and
EPA responses to significant comments,
the contents of the docket, except for
interagency review materials, will serve
aa the record in case of judicial review
(seciion 3O7\A}[7)[A]).
Under Executive Order 12291, EPA is
required to judge whether a regulation is
a "major rule" and, therefore, subject lo
the requirements of a regulatory impact
analysis. The Agency has determined
that this regulation would result in none
of the advene economic effects set forth
in section i of the Order aa grounds for
finding a regulation to be a "major rule."
The Agency has. therefore, concluded
thai this regulation ia not a "major rule"
under Executive Order 12291.
The Regulatory Flexibility Act (RFA)
of 1980 requires the identification of
potentially adverse impacts of Federal
regulations upon small business entities.
The Act specifically requires the
completion of a RFA analysis in those
instances where small business impacts
are possible. Because this rulemaking
imposes no adverse economic impacts,
an analysis has not been conducted.
List of Subjects ia 40 CFR Part SI
Administrative practice and
procedure. Air pollution control, Carbon
monoxide. Intergovernmental relations.
Lead, Nitrogen dioxide. Ozone,
Paniculate matter. Reporting and
recordkeeping requirements. Sulfur
oxides. Volatile organic compounds.
Dated: March 22.1990.
William K. ReilJy.
Adminislreior.
The EPA amends title 40, chapter I,
part 51 of the Code of Federal
Regulations as follows:
PART 51—[AMENDED]
1. The authority citation for part 51 is
revised to read as follows;
Authority: 42 U.S.C. 7401 (b](l]. 7410, 7470-
7479, 7501-7508. and ran (a), unless
otherwise noted.
2. Subpart K. 1 51-212 is amended by
adding paragraph (cj to read as follows:
{51.212 Tmtlng, Inspection, enforcement,
•nd complaint*.
« • • • •
(c) Enforceable test methods for each
emission limit specified in the plan. As
an enforceable method. Slates may use:
(1) Any of the appropriate methods in
appendix M to this part. Recommended
Test Methods for State Implementation
Plans; or
(2) An alternative method following
review and approval of that method by
the Administrator, or
[3] Any appropriate method in
appendix A. to.40 CFR part 60.
3. Appendix M is added to part 51 to
read as follows:
Appendix M—Recommended Teal
Methods for Stale Implementation Plans
Method 201—Delerminalion of PMio
Emimons (Eithaual Cai Recycle Procedure).
Method 20lA—Determination of PMio
Emission! (Constant Sampling Rate
Procedure).
Presented herein are recommended teal
method* (or measuring air pollutants
emanating [ram an emission source. They are
provided for Staiei to uie in their plans lo
meet the requirements of Subpart K—Source
Surveillance.
The State may alto choose lo adopt other
methods 10 meet the requirement! of Subpart
K of this part, aubject to the normal plan
review process.
The Stele may also meet the requirements
of Subpart K of thia pan by adopting, again
aubject to the normal plan review process.
any of the relevant methods in appendix A to
40 CFR part BO.
Method 301—Determination of PM,»
Emissions
(Enhautl Caa Recycle Procedure)
1. Applicability and Principle
1,1 Applicability. This method applies lo
the in-stuck measurement of participate
matter (PM) emissions equal to or less than
an aerodynamic diameter of nominally 10 jim
(PMi.) from stationary source*. The EPA
recognizes that condensible emissions not
collected by an in-slack method are also
PMi,. and thai emissions that contribute to~
ambient PM,g levels are the sum of
condensible emissions and emissions
measured by an in-atack PMio method, such
as this method or Method 201A. Therefore.
for establishing aource contribution* to
ambient level* of PM,,,, such as Tor emission
inventory purposes. EPA suggests that source
PMi, measurement include both in-slack PMio
and condensible emissions- Condensible
minions may be measured by an impinger
analysis in combination with thia method.
1.2 Principle, A gas sample is
uokinclically extracted from the source. An
in-slack cyclone ia used lo separate PM
greater than PMi«. and an in-slack glaca fiber
filter is used to collect the PM,» To maintain
ieokmeiic flow raie conditions at the lip of
the probe and a constant flow rate through
the cyclone, a clean, dried portion or the
sample ga* al alack temperature ia recycled
into the noule. The particular mass is
determined gravimetrically after removal of
uncombined water.
2, Apparatus
Note: Method S at cited in thi* method
refers to the method in 40 CFR part BO.
appendix A-
2.1 Sampling Train- A schematic of the
exhaust of the exhaust gas recycle (ECR)
train is shown in Figure 1 of this method.
2.1.1 Nozzle with Recycle Attachment.
Stainless stoel (318 or equivalent) with •
sharp ia pared leading edge, and recycle
attachment welded directly on the side of the
nozzle (see schematic in Figure 2 of this
method). The angle of the taper shall be or,
the outside- Uw only straight sampling
nozzles, "Gooseneck" or other nozzle
-------
14250 Federal Raptter/VoK 55, No. 74 / Tuesday. April 17. 1990 / Rules ami Regulations
extension! designed 10 mm th* u
How BO', u in Method S an not •c
Locaie a thermocouple '" •"« recycle
sliachm*ni to mW™ *h* lemperaiweof the
recvck gas •• •her""! in Figure Sol Irw
method. The recycle lUnehmenl shall be
made of §r»iB'e" "e«l and thalt be
connected io 'he probe and nozzle with
ftainlasi •'•*' finings. Two nottle lizes, e.g.,
O.lZS and C.16Q in., sbnuU be available to
allow isekinetictampUng to be conducted
over a r»np* of Raw role*. Calibrate each
nozzle as dRiCTibed in Method 9. Sections.!.
2-1.2 PMn Sizer. Cyclone, meeting (he
Bpedficabonj in Section 5-7 of this method.
2.1-3 Filler Holder, flaram. aiauitess steel
An Andersen filler, pert number SE274, has
been found lo be acceptable for (he m-euek
Tiller.
Now: Mention of trade names or irnccific
product* don noi constitute endorsement by
Ihc Environments) Prelection Agency.
2.1.4 Pilot Tube, Same aa i;i Method 5.
Section Z.I,3. Attach Ihfr pilol lo the pilot
lines with slair.let* Bteel finings and to the
cyclone in a configuration similar to Diet
shown in Figure 3 ol this m'.-lbod. The pitol
lines shall be mnde of heat resistant material
and attached lo the probe with stainless steel
fittings.
2.1.S ECR Probe. Stainless steel
15.9-mm |S-in ) ID tubing with a probe
liner, stainless sie-el 9.53-mm [Vin.l ID
stainless steel recycle tubing, two 6-35-mm
['/4-in.J ID stainless slcel ttrbtng fcr the pilol
tube extensions, three thermocouple leads,
and one power lead, all con:ained by
stainless steel tubing with a diameter ol
approximately 51 mm (2.0 In.]. Design
consideration* should include rririmurn
weight construction materials sufficient for
probe B(ruc*.ural strength. Wrap the sample
and recycle robes with a heating tope lo heat
llie sample and recycle gases lo clack
temperature.
2.1.8 Condenser Same at in Method S,
Section Z-l-7.
2.1.7 Umbilical Connector. Flexible tubing
with thermocouple and power leads of
sufficient length 1o connee: probe to meter
and How control Console,
2.1.a Vacuum Pump. Leak-tight. aiMns,
nonconfammarmg. with en absolute filler,
"HEPA~ type, at the pump exit. A Gaar Model
05ZZ-V1Q3 C18DX pump ha I been found 10 be
satisfactory.
:.V9 Meter and Flow Control Console.
Syiism consisting ol a dry gas meter and
calibraied orifice for memoring sample flow
rate and capable at measuring volume lo s2
percent, calibrated laminar How elements
(LFE's) or equivalent lor measuring tola) and
sample flow rates probe healer control -and
manometers and magnehelic gauges (as
shown in Figure* 1 aod & of this method), or
equivalent. Temperatures needed for
calculations include slack, recycle, probe, dry
gas meter, filter, and total flow. Flow
measurement* include velocity head (ip(,
orifice differential pressure (iHJ. total flow.
recycle flow, and jojal back .pressure tbrough
the system.
2.1.10 Barometer. Same «s in Uelhod S.
Section 3.1.8.
2.1-11 Rubber Tubing. &3S-«nai
ID flexible rubber tubing.
ZJ Sample Recovery.
2-2.1 Noale. Cyclone, and Fitter Haider
Brushes. Nylon biistle -brushes proo«ny sized
aod shaped for cleaning the noule. cyclone,
filter holder, and probe, or probe liner, with
atainles« stee! vmt shafts end handles.
2.2.1 Wash BoPlea. Claw Sample Storage
Containers, Peiri Dish«i, Graduate^ Cylinder
and Balance. Plaslir Storage Container*, and
Funnels. Same as Method 1. Socnaos SJJ.
IhroDgh 2ZJS and 12JL mpextiv«ly.
2,3 Analysis. Same aa in Melrwd 5,
S«clion 13.
3. Reagents
The ren jerrta med hi vampKo^. sample
recovery, and analysis are the tajoem* that
specified in Method i. Sections 3.1* JZ. and
3.3. respectively.
*, Procedure
4.1 Sampling-The complexity of (hit
method is such that. In order to obtain
reliable results, testers ahould be trained and
experienced with the test procedure*.
l.l.l Pretest Preparation.Some an in
Method S, Section 4.1.1.
4.1.2 Preliminary Determination*. Same as
Method 5. Section 4.1^. except use 1he
directions on nozxle size selection in this
section. Use of tho ECR method may require
e minimum eamplinj; port diameter of OJ m (6
in.). Also, the reqaired majcrmom number ol
sample traverse [win-.e %; j^y locaiiun shall
bell.
1.1-2-1 The cyclone and filter holder must
be in-slack or at stack temperature during
sampling. The blockage effect* of the ECR
sampling assembly will be mmimal if th«
cross-sectional area of the sampling'
assembly Is 3 percent or less of the crost-
sectional area of the duct end a pitol
coefficient of Q.M may be assigned lo the
pitol. If '.he cross-sectional ana of the
assembly is greater than 3 percent of the
crass-sectional area of the duct then either
determine the pilot coefficient at se-mpling
conditions or use a standard pilol with «
known coefficient in a configuration with ihe
ECR sampling assembly flucfa thai flow
disturbance! arc miniraiiod.
4.1.2-2 Construct a setup of pressure drops
for various Ap's and temperature*. A
computer is useful for thew calculations. An
exampla of the output of the ECR setup
program it shown in Figure 6 at this method
and directions on ita uie are in section 4,1-5.2
of this method. Computer programs, written
in IQM BASIC computer language. IO do these
types of letup and reduction calculations for
(he ECR procedure, are available through the
National Technical Information Service*
(NT1S). Accession number PBao-SOOOCQ, uas
Port Royal Road. Springfield. Virginia 22161.
4,1.2.3 The ECR setup program allow* the
tester to idea tho nozzle uzc bated on
anticipated average stack condition* and
prints a setup sheet for field use. The amount
of recycle through the nozzle should be
between 10 and 80 percent Input* for the
ECR setup program are slack temperature
(minimum, maximum. »nd average^, aiajck
velocity (rnir-jtnum. maximum, and average).
atmospheric pressure, luck •static preMure.
meter box temperature, stack moisture,
percent a. and percent CO, in Ihc alack gas.
pilot coufTicieni 1C,], orifice A KU, flow me
measurement calibration values (slope |m|
and y-inlcrcept |b) of the calibration curve).
and Ibe number of nozzles available and rhevr
diameters.
4.1 A4 A less rigorous calculation for the
setup sh*et can be dooe manually uamg the
rquations on the example worksheet! in
Figures ". S. and 9 of this method, or by a
rlewIelt-Packard HP*I calculalarunuig the
program provided in appendix D of the ECR
operators manual, entitled ApplicuUans
Guide for Source PMn Exhaust Gcf Uecyclc
Sampling System. This calculation usct an
approximation of the total flow rate and
agrees within 1 percent of the ex.ici solution
for prtMurr drops at slock tcrmperatum frorn
3B lo ZfiO 'C (100 lo 500 T) and slack moralure
up to 50 percent. Also, the example
worksheets use » constant stack temperature
in the calculation, ingoring n l^e pump and
alttch pump lines lo ibe meter and flow
control cons ale.
4.1.4 Le.ik-Check Procedure. The leak-
check for the ECR Method coniutt ol two
perls: Ibe sample-side and the recycle-aide.
The sample-side leak-check is required at ibc
beginning of the run with the cyclone
aUachcd, and after the run with the cyclone
removed. The cyclone Is removed before the
peal-leal leak-check to prevent any
disturbance ofiha collected sample prior to
ar.alytU, The recycle-side leak-check testa
the leak tight integrity of the recyde
components and is required prior lo the first
(cst run and after each shipment.
4.1.4.1 Pretest Leak-Check. A pretest leak-
check of the entire sample-side. Including the
cyclone and nozzle, is required. Use the leak-
check procedure in Section-4.;.«.3 of this
method lo conduct a pretest lenk-check.
t.\.t2 Leak-Check* During Sample Run.
Same as in Method S, Section 4.1.4-1.
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1425J Federal Register (_Vol. 5S. No. 74 /Tuesday. April 17. 1990 f Rules and Regulations
ahnll not exond 1 mm 10.03 in.). U the
exceed (be limil specified adjust
or replace tbe pressure gauae- Alter each
field use. check the calibration of the
pressure paupea.
5.3.3 Tou ILFE. Same as the metering
jysiem in Method i, Section SJ.
5-34 Recycle LFE- Same u the merering
gy5lem in Method S. Section 5.3. exczpl
completely dose bolb the coarse and ftnr
recycle valves.
S.4 Probe Healer. Connect Lhe pnoiie io
the meter and flow control console with Lhe
umbilical connector. Insert a thermocouple
into the probe sample line approximately half
Iha length of the probe lampte line. Calibrate
Hie probe healer at 96 *C [150 "FL m 'C
[250 T). and 177 'C [350 'FJ. Turn on the
power, and set lie probe healer to the
specified temperature. Allow the hcator la
equilibrate, and record the thermocouple
temperature and the meter and How control
console temperature io the nearest QJ "C
[1 *F). The two temperatures should agree
within 5.S 'C (10 T). If this agreement is not
met, adjust or replace the probe healer
controller.
5.5 Temperature Gauges. Conned nil
thermocouple*, and let the meter and flow
contol camole equilibrate Io ambient
temperature All thermoconpleii shall agree to
within I.I "C (Z.O T) with a standard
nercury-in-glan thermometer. Replace
defective thermocouples.
9.6 Barometer. Calibrate again*! a
standard mercury-in-glaM barometer.
5-7 Probe Cyclone and Nozzle
Combinations. The probe cyclone and nozzle
combinations need not be calibrated If the
cyclone menu the design inctiQcaliong in
Figure 1Z of this method and the nozzle meela
the design specifications in appendix B of the
Application Guide far the Source P."uf m
ExJtoutt Gar Recycle Sampling System, EPA/
600/3-88_osa. Thia docutnoot may be
obtained from Roy Huntley at (91B}M1-1060.
If the nozzle* do not meet the design
specifications. Uiea tesi the cyclone nod
nozzle combination for conformity with tie
performance specification* (PS's) In Table 1
of this method. The purpose of the PS teats is
(D determine if the cyclone's ahorpr.cs> of cut
mean minimum performance criteria. If the
cyclone does not meet design specifications.
then, in addition Io the cyclone and Dazzle
combineiiaa conforming to the PS'i, calibrate
the cyclone and determine the relationship
between Haw raU:, gk* viscowity. and gat,
denji'.y. Use ths procedures in Sec Iron S.7 j of
this method la conduct PS iwta and the
procedures m Section B.B of this method to
calibrate the cyclone. Conduct the PS lesli in
a wind tunnel described in Section 5.7.1 of
>w-i method and uiMng a particle generation
•em described in Section 5.7,2 of this
nod. Use five particle sizes and three
- .nd velocities as listed In Table Z of this
method. Perform a minimaoi of three replicate
measurements o! collection efficiency for
each of the IS conditions listed, for a
minimum of 45 measurements.
5.7.1 Wind Tunnel. Perform calibration
and PS testa in a wind tunnel (or equivalent
teal apparatus) capable of establishing and
maintaining the required gas stream
vnlocilies wilhin 10 percent.
5.7.2 Particle Generation System. The
particle generation system shall be capable of
producing solid monodMperacd dye particles
with the raaia mrdien aerodynamic
diameters specified in Table 2 of this method.
The particle size distribution verification
should be performed on an integrated sample
obtained during the campling period of each
test. An acceptable alternative it to verify the
size distribution of samples obtained before
and after each test with both samples
required to meet the diameter and
monodispersity requiiements for an
acceptable test run.
5.7.2.1 Establish the size of the solid dye
particles delivered to the test section of the
wind tunnel using the operating parameters
of the panicle genera U on system, and verify
the size during the testa by microscopic
examination of samples of the particle!
collected on a membrcne filler. Tbe particle
aiu, aa established by the operating
parameters of the generation syjlcin, shall be
within the tolerance spedGed in Table Z of
this method. The precision of the parti de size
verification technique shall be at leant ±0.5
um, and the particle aize determined by the
verification technique shall not differ by more
than 10 percent from thai established by the
operating parameters of the particle
generation system.
5.7.2.2 Certify tha manodiapenily of the
particles [or each lest either by microscopic
inspection of collected panicles on niters or
by other suitable monitoring techniques such
as an optical particle counter followed by a
multichannel pulse height analyzer, U the
proportion of multipleu and satellites in a-
uerosal exceeds 10 percent by mass, thr
pxrticte peneratton system is unaccvptubl*
[or purposes of this lest. Maltiptete anr
particles that are BrjtRkjmeniied. and MlrltiU-j
are particlen that are smaller then the
specified size range.
5,7.] Schematic Drawings, Schematic
drawings of the wind tunnel and blower
system and other information ahowir.j
complete procedural detail] of the lest
atmosphere genera linn, verification, and
delivery trchr.ique* shall be furnished with
calibration data in Inn reviewing agency.
5.7,4 How Rate Measurement, Determine
the cyclone flow relea with a dry gas meter
and a stopwatch, or a calibrated orifice
system capable of measuring flow roles to
within 2 percent.
5.7,5 Performance Specification
Procedure. Establish the test particle
generator operation and verify the particle
size microscopically. If mondiaperaily is lobe
veriftei] by measurements at the beginning
and the end of the run rather than by an
integrated sumplc these measurements may
be made at this limo.
5.7,3.1 Tbe cyclone cut lize f DM) is
defined a* the aerodynamic diampler nf a
particle having a 50 percent probability of
penetration. Determine the required cyclone
flow rate at which D» i* 10 um. A suggcaied
procedure is to vary the cyclone flow rale
while keeping a constant particle size of 10
jim. Measure the PM collected in the cyclone
(m,). exit tube (m.). and Tiller (mr). Compute
the cyclone efficiency (E.) aa follows:, . u
m.
(m, + m, + mr)
y. ico
5.7.5.2 Perform three replicates aed
calculate the average cyclone elGdency as
follow
where Ei. Et. and Ei are rcpllcale
measurements of Er-
5.75.3 Calculate tte standard deviation (o-J
for the rcpbcale mcasuremenls of E. es
follows:
if IT exceeds 0.10, repca'. '.he replicate runs.
5.7.5.4 Using the cyclone flow rait that
produce! Du for 10 uni. measure the overall
cfTicicncy of the cyclone and nozzle. E. at the
particle sizes and nominal gas velocities In
Table Z of this method using thia following
procedure.
5.7.5J Set the oir veiacirj* in The wind
tunnel to one of the nomtial gas velocities
from Table 2 of (his method. Establish
laokinetic sampling condiiiona and the
correct Qow rate ihrough the sampler
(cyclone and nozzle) uung racydsr capacity
so thai the Ob* li ifl ftffi. Sample long enoqgfa
to obtain ±3 percxol precranjo an Ibe taul
collected mase ei determined by the
precision and the senBitivity of the ir.easuring
technique. Dcleoune separately ihe nozzle
utch (m,). cyclone catch (mj. cyclone axil
tube catch (raj. and collection filter catch
(m,).
i7-Sj8 Calculate the overs U efficiency 1EJ
as Follows:
-------
Federal Register / Vol. 55. No. 74 / Tuesday. April 17. 1990 / Rules and Regulations 14251
4.1.4.3 Poil-Tei! Leak-Check. A leuk-
check is required al the conclusion of each
sampling run. Remove ihc cyclone before Ihe
Irak-check to prevent ih« vacuum created by
the cooling of the probe from disturbing the
collected sample and use ihe following
procedure to conduct a post-test leak-check
4.1.4,3.1 The sample-side leak-check is
performed as follows: After removing Ihe
cyclone, seal the probe with a leak-tight
Hopper Before starling pump, close the
coarse total valve and both recycle valves,
and open completely the sample back
pressure valve end Ihe fine total valve, Afler
turning ihe pump on. partially open the
coarse total valve slowly to prevent a surge
in the manometer. Adjust the vacuum to at
least 301 mm Hg (15.0 in. Hg) with the fine
total valve. If the desired vacuum is
exceeded, either leak-check al this higher
vacuum or end the leak-check an shown
below and start over.
Caution: Do no) decrease the vacuum with
any of the valves. This may cause a rupture
of the filter-
Note: A lower vacuum may be used, provided
ihai i! ii not exceeded during Ihe test.
4.1.4,3.2 Leek rales in excess of 0.00057
mj/min (O.OZO ft*/min) are unacceptable. It
the leak rate it loo high, void Ihe sampling
run.
4-1,4-3.3 To complete the leak-check.
slowly remove the (topper from the nozzle
uniil ihe vacuum is near zero, then
immediately turn off the pump.This
procedure sequence prevents a pressure
surge in the manometer fluid and rupture of
the filler.
4.1.4.3.1 The rccycle-side leak-check is
performed at follows: Close the coarse and
fine total valves and sample back pressure
valve. Plug the sample Jnlet at the meter box.
Turn on the power and the pump, dose the
recycle valves, and open Ihe total flow
valves. Adjust the total flow fine adjust valve
until a vacuum of 25 inches of mercury is
achieved. If the desired vacuum is exceeded.
either leak-check al this higher vacuum, or
end the leak-check and siart aver. Minimum
acceptable leak rates are the same aa for Ihe
sorr.ple-side. Lf the leak rale is too high, void
ihe sampling run.
4.1.5 ECR Train Operation. Same as in
Method 5, Section 4.1.5. except omit
references to nomographs and
recommendations about changing [he filter
assembly during a run.
4.1,2.1 Record the data required on a data
sheet such as the one shown in Figure 10 of
this me'.hod. Make periodic checks of the
manometer level and zero to ensure correct
AH and Ap values. An acceptable procedure
for checking the zero is to equalize the
pressure al both ends of the manometer by
pulling off the tubing, allowing the fluid lo
equilibrate and. if necessary, to re-zero.
Moinlain the probe temperature lo within
11 ~C (20 T) of stack temperature.
4.1.5.2 The procedure for using the
example ECR setup sheet is at follows:
Obtain a stack velocity reading from the pilot
manometer (Ap). and find this value on the
ordinals exit of the setup sheet. Find the
stack temperature on Ihe abscissa. Where
these two values intersect are the differential
pressures necessary lo achieve isokinelicity
and it) urn Cu! size (interpolation may be
necessary).
4.1.3,3 The top three numbers are
differentia] pressures (in. HjQJ, and the
bottom number IB the percent recycle at these
flow settings. Adjust the total flow rate
valves, course and Tine, lo the sample value
UH) on the letup sheet, and the recycle Row
rait valves, coarse and fine, to the recycle
flow on the setup sheet.
4.1.5.4 For startup of the ECR sample
train, the following procedure it
recommended. Preheat the cyclone in Ihe
Btack for 30 minutes. Close both the sample
and recycle coarse valves. Open the Tine
total, fine recycle, and sample back pressure
valves halfway. Ensure thai the nozzle is
properly aligned with the sample stream.
After noting the Ap and Black temperature.
select the appropriate AH end recycle front
Ihe ECR setup sheet. Start ihe pump and
liming device simultaneously- Immediately
open both the cuarse total and the coarse
recycle valves slowly to obtain the
approximate desired values. Adjust both the
fine told! end the fine recycle valves to
achieve more precisely (he desired values. In
the ECR flow system, adjustment of either
valve will result in a change In both tola! and
recycle flow ratei. and a slight Iteration
between Ihe total and recycle valves may be •
necessary. Because the sample back pressure
valve controls the (olal flow rate through the
system, it may be necessary (o adjust this
valve in order lo obtain Ihe correct flow rate.
Noia: (sokinetic sampling and proper
operation of the cyclone are not achieved
unless the correct AH and recycle flow rales
are maintained.
4.I.S.: During Ihe lest run, monitor the
probe and filter temperatures periodically.
and make adjustments as necessary to
maintain Ihe desired temperatures. If the
sample loading Is high, the filler may begin to
blind or the cyclone may clog. The filter or
Ihc cyclone may be replaced during Ihe
sample run. Before changing the filter or
cyclone, conduct a leak-check (Section 4.1,4.2
of this method). The total paniculate mass
shall be the sum of all cyclone and the filter
catch during Ihe run. Monitor stack
temperature and Ap periodically, and make
the neceuary bdiustmcnts in sampling and
recycle flow rates to maintain iaokinetic
sampling and ihe proper flow rate through the
cyclone. At the end of the run, turn off the
pump, close Ihe coarse total valve, and
record Ihe final dry gas meter reading.
Remove Ihe probe from the slack, and
conduct a post-test leak-check as outlined in
Section 4.1-4 J of this method.
4.1.8 Calculation of Percent Isokinelic
Rate and Aerodynamic Cut 5iz«, Calculate
percent isokmetic rate and Ihe aerodynamic
cut size (Du) (see Calculations, Section 6 of
this method} lo determine whether the test
was valid or another test run should be made.
If there wsi difficult in maintaining isokinetic
rates or a DM of 10 pa because- of source
conditions, ihe Administrator may be
consulted for possible variance.
4.2 Sample Recovery. Allow the probe to
cooL When the probe can be safely handled.
wipe off all external PM adhering to the
outside of the nozzle, cyclone, and nozzle
attachment, and plew a cap over ihe nozzle
to prevent losing or gaining PM. Do not cap
the nozzle tip lightly while the sampling train
is cunling, as this action would create a
vacuum in ihe filler holder. Disconnect the
probe from the umbilical connector, and lake
the probe lo In* cleanup site. Sample
recovery should be conducted in e dry incuior
area nr. if outside, in an area protected from
wind and free of dust. Cap iht ends of the
impmgeri and carry them to the cleanup site.
Inspect I)IP components of the train prior to
and during disassembly lo note any abnormal
conditions. Disconnect the pilot from ihe
cyclone. Remove the cyclone from the probe.
Recover Ihe sample as follows:
4.2.1 Container Number ! (Filler). The
recovery shall be the same as the! for
Container Number 1 in Method 5. Section t.2.
4.2.2 Container Number 2 (Cyclone or
Large PM Catch). The cyclone must be
disassembled and the nozzle removed in
order to recover the large PM caich.
Quantitetively recover the PM from the
interior surfaces of Ihe nozzle and the
cyclone, excluding the "turn around" cup and
the interior surfaces of the exit lube. The
recovery shall be Ihe same ai that for
Container Number Z in Method 5. Section 4.2.
4.2.3 Container Number 3 (TM,,).
Quantitatively recover Ihe PM from all of the
surfaces from cyclone exit to the front half of
the in-slack filler holder, including the "turn
around" cup end the interior of the exit tube.
The recovery shall be the same as that for
Container Number 2 in Method 5. Section 4.2.
4.2.4 Container Number 4 (Silica Gel): x
Same as that for Container Number 3 in
Method 5. Section 4,2.
4.2.5 Impinger Waler Same as in Method
5, Section 4.2. under "Impingcr Waier."
4.3 Analysis. Same as in Method 5.
Section 4.3. except handle ECR Container
Numbers 1 and 2 like Container Number 1 in
Method 5, EGR Container Numbers 3, 4, and 5
like Container Number 3 in Method 5. and
ECR Container Number 6 like Container
Number 3 in Method S, Use Figure 11 of this
method to record the weight! of PM collected.
4.4 Quality Control Procedures. Same as
in Method 5. Section 4,4-
5. Caffliiatian
Maintain an accurate laboratory log of all
calibrations.
5.1 Probe Norzle. Sair.t as in Method 5.
Section S.I.
5,2 Pilot Tube, Same as in Method 5,
Section 5-2.
5.3 Meter and Flow Control Console,
5.3,1 Dry Gas Meier. Same as in Method
S, Section 5.3.
5.3.2 LFE Gauges. Calibrate the recycle.
total, and inlet total LFE gauges with a
manometer. Read and record flow rales at 10.
50, and 90 percent of full scale on the luial
und recycle pressure gauges- Read and record
flow rales al 10. 20. and 30 percent of full
scale on Ihe inlet tola! LFE pressure gauge.
Record Ihe total and recycle readings to the
nearest 0.3 mm (0.01 in,). Record Ihe inlet
tola! LFE readings lo the nearest 3 mm (0.1
in.]. Make three separate measurements al
each letting and calculate the average. The
maximum difference between the average
pressure reading and the average manometer
-------
142SI Federal Kegisier / Vol. 55. No. 74 / Tuesday. April 17^1990 / Rules and Regulations
The How rule, at actual cyclone condition*.
s calculated as follows:
6.6 1 Determine the water Fraction of ihe
miked gas through the cyclone by using the
equsiion <
Q. =
T.
V....*,
—
B,
Q.I.-I o ->- v.
6.6.2 Calculate (he cyclone gas viscosity
as follow;
fwC, + C.T. + C,T.«+C.[n~C.B.
B.G,3 Calculate the molp.cular weight on a
we I basis of the cyclone gas HI, fotlowc:
M. •= M.(l - Br) + 18.0(D.)
G.B.4 11 the cyclone meets lh« design
tpecificauon in Figure 12 of this method,
calculate the actual D* ai ihe cyclone for the
run as (olio «s:
d,
M. P.
"«•'
IP-m 1 B1
T!
where fl, = 0.1562.
6 0.5 K [he cyclone cloei nol meet the
deiign apecilicationi In Figure 12 of ihii
method, then uee the following equation t
calculule DM.
DM = (3)(10)k (7.376 X 10")~ ' Nlc Pt
68 Aerodynamic Cut Size. Use ihe
following procedure to determine Ihe
aerodynamic cut gize (Du>)-
wherc;
m = Slope of the calibration curve
obtained in Section 5.8.2.
b = y-iniereepi of Ihe calibration curve
obtained in Section 5.B.Z.
67 Acceptable Reiuln. Acceplobility of
anuokinelic variation \s the tame as Method
3, Section B.iz.
671 If 9.0um C Dw
-------
Federal Register / Vol. 55, No. 74 / Tuesday, April 17, 1990 / Rules and Reputation* 14253
- 100
(m, •*
5.7,2.7 Do three replied ice lor each
combination or JIBS velocities and panicle
s:zee in Table 2 of this method- Calculate E.
fur each particle site following the
procedure! described in Ihii section for
determining efficiency Calculate the
itandard deviation ( Cyclone flow rate etn'/tec.
p - Gas density, g/cm',
dg. a Diameter of cyclone inlet, cm.
p^. " Viscosity of gas through the cyclone.
poise.
DM — Cyclone cut aizc, cm,
5.0.1.2 Use a linear regression analysis to
determine the slope (m], und the y-intercept
(b). Use the following formula lo determine
Q. the cyclone flow fata required lor a cut
aize of 10 (int.
m/(m-05|
where:
Q = Cyclone flow rate for a cut size of 10
urn, cm'/aee.
T, = Slack gaa temperature, TC
d = Diameter of nozzle, cm,
K, = 4,077 X 10-".
5.0-Z. Directions for Using Q. Refer to
Section S of the EGR operators manual for
directions in using this expression for Q in
ihe teiup calculations.
8. Calculations
0.1 The ECR data reduction calculation!
are performed by the ECR reduction
computer program, which it written in IBM
BASIC computer language and is available
through NT15. Accession number PB90-
500000. SZ85 Pon Royal Road. Springfield.
Virginia 22161. Examples of program inputs
and outputs are shown in Figure 14 of Ihia
method.
6.1.1 Calculation* can also be done
manually, aa specified in Method 5. Sections
8,3 Ihrough 8.7. and S.9 through 112, with ihe
addition of the following:
8.1.2 Nomenclature.
B, = Moisiure fraction of mixed cyclone
gas. by volume, dimensionleii.
Ci = Viscosity constant, si.12 rrJcropoise
for 'K (51,05 micropoiae for 'RJ.
d =* Viscoeity conalanl. OJT2 tr.icropoise/
"K (Q.2D7 micropoiie/*R).
C, = Vise/wiry wmaiant. 1.03 X10"
micropoise/'K' (3.24 X 10~'mlcropoiec/
•R").
C. = ViacwEty constant, 53.147
micropoite/fractlon Oi.
C. •= Viscosity constant. 74.143
micrepoise/fraction HiO.
Dw = Diameter of parttelei having • 50
percent probability of penetration. >im.
(n B Stack gaa fraction Cs, by volume, dry
baaia,
K, - O.iaSfl 'K/mm Hg [17.64 'R/in. HB).
M, E. Wet molecular weight of mixed gaa
through the PM« cyclone, g/g-mole (lb/
Ib-mole).
M, — Dry molecular weight of slack gas. g/
g-mole (Ib/lb-moie).
P«, • Barometer pressure at sompiing site.
mm Hg (in. Hg),
P»i • Gauge pressure at Inlet to total LFL
nun HiO (in. HjO).
Pi — Absolute slack preasure, mm Hg (In.
H8).
Qi «> Total cyclone flow rale at wet
cyclone conditions, m'/mln (fl*/min).
Q^^o - Total cyclone flow rale at
standard eonditoni. dacm/min (d»cl[
min).
T. — Average temperature of dry gaa
meter. 'K fR).
T, — Average slack gal temperature, 'K
CR).
V^iBd — Volume of water vapor in gaa
•ample (itandard conditions), acm (iff]-
XT
Tgln! LFE linear colibrolion eonftlanl.
i K.O1J
,.
Yt - Tola! LFE linear calibration aonJtonh-
dacm/min (dacf/min),
APT o Pressure differential across lol.il
LFE. mm H,O, (in. HiO).
8 a Total sampling lima. min.
Ug, • Vlicoiily of nixed cyclone gas,
mjcropoise.
um e> Viicoaity of gaa laminar How
elefftenta, micropoiae.
ILaa - Viscosity of standard air. J80.1
micropoiae.
6^ PMn Paniculate Weight. Determine
Ihe weight of PM,« by summing the weights
obtained from Container Numbers 1 and 3.
leu the acetone blank.
8.3 Total Paniculate Weight. Determine
the paniculate catch for PM greater Lhan
PNU from ihe weight obtained from
Container Number 2 Icaa the acetone blank,
and add it lo the PM» paniculate weight.
6-4 PMi* Fraction, Determine the PMio
fraction of the tola) paniculate weight by
dividing Ihe PMu particulale weight by Ihe
total paniculate weight,
6.5 Total Cyclone Flow Rate. The average
flow rate at standard condition* is
dc:ermined from the average pressure drop
across the total LFE and is calculated ai
follows;
K,
»•— J.V- 1 p—
-------
MIXED GAS
TO CYCLONE
SAMPLE
GAS
K
Ul
s
fr
5"
tn
01
2
o
RECYCLE
GAS
Figure 2. Schematic ol EGR noizle assembly.
O.
cu
"
e
5"
a
a.
50
CD
10
c
o
to
-------
PITOT TUBE
EGR PROBE ASSEMBLY
RECYCLE
LINE
HEATED
FILTER
HOLDER
NOZZLE FILTER
HOLDER
HECYCLEl
FLOW
LFE
METER AND FLOW
CONTROL CONSOLE
EXHAUST
SEALED PUMP
o
o
-1
m
la
n.
13
i
30
5"
Figure 1, Schematic ol Ih* exhaust gas recycle Iraln.
ya
i
£7.
O
-------
FINE TOTAL
VALVE
TJ
p.
PROBE HEAT CONTROL
TEMPERATURE
INDICATOR
IB
IB
3
Q.
»
n
'
ia
Figure 4. Example EGR control module (Iron! view)
showing principle Componenls.
-------
Federal Register / Vol. 55, No- 74 / Tuesday, April 17, 1990 / Rules and Regulations 142"
PM 10 CYCLONE
FILTER HOLDER
(63-mm)
TYPE-S PITOT
RECYCLE LINE
STACK THERMOCOUPLE
L J
EGR NOZZLE
RECYCLE THERMOCOUPLE
Figure 3. EGR PM10 cyclone sampling device.
-------
14260 Federal Register / Vol. 55. No. 74 / Tuesday, April 17, 1990 / Ruled and Regulation);
EXAMPLE EMISSION GAS RECYCLE SETUP SHEET
VERSION .1.1 MAY is
TEST I.D.: SAMPLE SFTUI'
RUN DATE: ll/M/W
LOCATION: SOURCE SIM
OPF.RATOR[S): RH |H
NOZZLE D1AMETT.R (IN): .2S
STACK cor;nmoNS;
AVERAGE TEMI'IIKATTHK (1 •'): a«JB ..
AVERAGE VELOCirr (FT/SRC): 15.R,
AMBIENT PRESSLTRE [IN HC): 29.92...
STACK PRESSURi: (IX U3>|: ,in
11:0=10.0%.,
_._, 02 = 20.3*.
. CO2 - .0%
M We 27.75
[LD/LB
MOLE)
TARGET PRESSURE DROI'S
TEMPERATURE (F)
DI'fPTO).
0.02C
.031
,03S,...
.039
150
SAMPLE
TOTAL
RECYCLE
%RCL
,5B
1.HB
z,n
snt
.07
188
1-57
54%
•5
1.B7
2.44
101
-4B
1-fO
tJW
61*
.50
1.89
174
57%
.05
l.BB
2. GO
1.38
17;
.4H
l.WO
:.9i
MS.
55
LBn
2.77
58^
M
1.R9
2.63
S5TS
.72
1.8B
230
52%
1.91
2.94
OZS
.55
1.90
2.00
sa%
.63
1.B9
Z.bf.
50%
.71
1JBS
I'M
.47
1.92
Z.S7
l.ffl
2.K
SfK,
.62
1.W
2.09
56K
.70
ua
ZJO
.40
1.92
3.00
63%
.5-4
I.B1
2.85
59%
.61
1.90
172
57%
.69
1.BO
Z.59
217
,45
1.9J
3.02
aas'f,
-S3
1,91
Z-DA
60%
.CO
1.91
274
57%
-H7
1 90
2.G2
.45
1.93
3.05
(UK
.52
1.K
2.90
60S',
je
1.91
52% 53%
Figure 6- Example EGR wtup sheet
,BT>
1,91
ifi.".
55":-
Barometric preuure,
P«. in. HJ.
Slack static
pressure, P,. in.
a-o.
Ai-eraa* alack
temperature. l». "F.
Mtiir temperature,
U. 'P.
CUB analysis:
?iN5 + XCO
Fraction moisture ™
content. B...
Calibration data:
Nozzic diameter.
D. In.
Pilot coeiTicienL
C»
AHff. in. HjO
Molecular weight
of »tbck ga», dry
Ib/lb
Molecular weight of
•tack gas. wet
baiia:
Abanlulc
pressure:
J]j/lb mole
jn. Hp
K-B48.72 D.' AHfl C.1 (j-B^l
M. (l.-r.4«)) P.,
Ue»ired melur oriHce [irt-ssure (AH] (or
velocity tlead of slack gi«i (ip):
AH»Kip= in. H:O
Figure 7. Example wurkshetl I, meter urificc Absolute iluck
presRure head calculation.
Biiromeiric pressure.
Pv in. Hg.
pre»ure, P, in. Hg-
AverngB Itack
lemperatura. Tr 'R.
Meier (emparature. Tv "R,
-------
ORIFICE METER
DRYGASMETEH
THERMOCOUPLE
TOTAL FLOW
THERMOCOUPLE
DRY GAS METER
MANOMETER
SOLENOID
RECYCLE FLOW
QUICKCONNECT
TOTAL FLOW
QUICKCONNECT
8.
n
s
HEPA FILTER
TOTALLFE
RECYCLE LFE
RECYCLE FLOW
SOLENOID
TOTAL FLOW
SOLENOID
r"
~?,
o
H
n
-------
14262 Federal Register / Vol. 55. No. 74 /Tuesday. April 17. 1990 / Rules and Regulations
Figure 9. Example worksheet .1.
recycle LFE pressure head-
BILLING COOt
-------
Federal Register / Vol. 55, No. 74 / Tuesday. April 17, 1390 / Rules and Regulations 142S1
Molef.ulnr wciph*. of
Hack fa*, wet basis.
M. Ib/lb mole,
Prtmure upstream of
Utin. llg.
Cai analysn:
Fruciion moisture
con i em a...
Calibration dath:
Nozile diameter. D..
in.
Piioi coefficient. C,
OB
Total LFE calibration
constant. X,.
Tula! LFE calibration
constant, T,.
Ahsolule pra*sur*
upstream of LFE;
Viiconiiy oi gat in
LFE
>i LIT -152.
_tn. US
Vi»cosi!y of dry itacfc
T. + 3.1355x10-'
T.!-*O.J
ConblontB:
Ka =0.1539,
-B,)
Figure 8. Example worksheet 2. Iota) LFK
pressure head.
A,'
)*LfT
' X, iBOi X,
Total LFE pressure head:
Jn.HiO
Barometric pressure. P1mr in. Hg=.
Absolute stack pressure. P. in,
Hg=
Average stack lerr.pcralure. T,,
•R=
Absolute pressure upstream 01 Lj-c, i
in. Hg=
CaUbraiion data;
Nozzle diameter. Dn. in.=a
Pilot coefficient. C,=
Recycle LFE calibration conalunl,
X,.
Meter temperature, TB. 'R=
Molecular weight of slack gas. dry basis. Recycle LFE calibration constant,
H,. Ib/lb mole=. Yr=s
Viscosity of LFE gas, MLTE- poise=
Viscosity of dry stack gas, ti*.
poi3e=
K, = urszxio**-
K, - 0.1S39
P.
= — - | H
T.
K. -
B,.]
.K,
X.
Pressure head for recycle LFE:
- in-H.0
-------
14264 Federal Register / Vol. 55, No. 74 / Tuesday. April 17, 1990 / Rules and Regulations
I'i.inl
Diilf
Run no- -
Filler no.
Arnuunl liquid lost during
transport
Acelone blank volume. ml_
Acetone wash volume, ml
Container numoer
Wognt °' PBircuiaie
man*- mg
Final
•wight
Tare
weignt
Wwh<
ga,n
Acetone blank cone,, nig/mj; (Equation
5-4, Method 5)
Acelone wash blank, mg [Equation 5-5,
Method 5]
Tpial ,
Less acciane blank.
Wcigm ol PM...
a...
Less ICItone blank ..
Container numoer
of caniculatc
mailer, mg
Final
Tare
Weiahl
gam
loiai paniculate
.
Figure 11- ECR method analysis sheet.
BILLING COOt. «5*C-SO-M
-------
tn
O
Run
Codt
Simpler
10
Fllttr
IP
Sample!
Ofienlallon
Sampling
Locellon
Nouli
Dllmtltl-ID (In.)
Optriloi (i)
Dale
Slarl
Time
End
Time
Sampling
Duration (mln)
DGM
(InillM)
DGM
(llnal)
Simple
Volume t'l r
Dual Manometer Leveled and Zaroid7
M«gn«hellCi Zerotd?
Hun
Tint
Purl No
Triv. PI,
flP
Pllol
ftK
Sample
•
DGM
Volumt
ftP
Tolnl
Slack
Tcfflpcraluie (°F)
SUck. SUlic
Pressure ' '"'• Hj°)
Ambient
Ttmpcrature (°rl
Amt>l»n1
Preiiurr *'' H3i
Gn
Vclaclly
Syi »
-------
14266 Federal Register / Vol. 55. No. 74 / Tuesday, April 17, 1990 / Rules and Regulations
TABLE 1. PERFORMANCE SPECIFICATIONS
TOR SOUBCE PM,0 Cyclones and Noz-
zle Combinations
I Urwii
eHipaney
2. C**Jnt cul
SM (0^1.
urn...
! Sucft thai
I orincuon
I aim wi
n i.7.S
ana
wodynxne
TABLE 2. PARTICLE SIZES AND NOMINAL
GAS VELOCITIES FOR EFFICIENCY
Target gas velocities
sl.0 I 15=1.5
S±0.5..
7=0.5 ! j L.
lOsQ.s.4 J !..
u-io"' -•—--™i—• -|-
20 ±1.0...! 1 ! - "i
la) Mass median Bwodynamc dianwiiir.
COOC UM-W-M
-------
Federal Register / Vol. 55~ No. 74 / Tuesdav. Apr;] ir, lOjifl / Rules and Regulations
Cyclone Interior Dimensions
Din
0.10 in, r
Z'
L
-Dcup
Hcup
_L
cm
inches
Dimensions (+0.02 on, ±0.01 in.)
Din
07
0,50.
D
4.47
1.75
Dr
1.50
0.59
B
t.E3
0.74
H
6.SS
Z74
h
124
0.88
Z
4.7!
1.85
S
1.S7
0.52
Kmp
L25
0.89
Dcup
4.45
1.7S-
o;
1.02
0,40
0,
1J4
0.43
Figure 12. Cyclone design specifications.
52
BILLINO COM tiao-s»«
-------
14268 Federal Register / Vol. 55. No. 74 / Tuesday. April 17, 1990 / Ruins and Regulations
Emictiun Ga» Recycle. Duta RHdu
Vemrm S.« MAY IMC
Ter.1 ID. Cude: Chapel Hill :.
Ten Locution: Brfjriousp Oulli-I.
Teal Site: Chapel Hill,
Test Dale: lO/IO/Bf..
Oj.eralorK(3|: |U RM Mil,
Entered Kun Dan:
. ii K
TILTH _ ..... ----------------------- m.ii f
TjUCMI ...... _________________________ 78.1! K
SynlRin Prrnum
Diiionn --------------- ............. .. i.
DHTOT) ---------- ..... ------------ I.PI itv'A-r;
............. i:,is ivwc
DPHCI.I _____ ..... __ ....................... E.=l IMVO
DPirroi ------- ..... — . ....... _ ..... ii.no ixwc:
McellancB:
PJDARI ---------------- ........... ... 3U«; IN'WC
urt Dolti — Cunlinui-d
............. uio I
Y(IJCM) ____ ......... _____ ..... _.., 13.7M m
TIME _______________________ ..... _. bO,UU MIN
«•' ."O: ____________ ......... ______ ..... - 8.01)
• ..... ______ , _______________ . ........ zaon
bJitifriaie.,.. __ ,-, ..... ___ _ ____ , ____ 0.0".',
ui
Cu.-iik-nMT ._,..,„ --------- ............. . 7JK Ml,
Cubmf: ...................... .................. «,(i C,M
KM" M;u»t:s:
CALK, lit !..._ ............ ___ .......... _. 21.7 MC
r'iliM ------------ ...... --------------- 11.7 MC
lnipiiu>r P,e*jdiii; -------- .......... G.n MC . -
DJtink Valun:
CYC Kirwe.- ............ ----- ....... _ 00 MO
filler IMiVr Kin-M' .._ ............... L.D Mf,
Ki!t,:r HiniiV. ...... ____________ .......... - O.D MC
lnipinn»i Riniw. --------------- .—... 0.0 MC
CrtnTOTl ___________
MJTOT U-T.l
BITOT LKKI
MIKCI. IJT:I
D1 RCI. I.KF.1 ....
IK:M
- •«lftT
,'lcrfucpc/ iJu
vack (;«>. MnjjiuK: |?;j _______
h,,m[iii- Fiuw BHIC (ACCM1
luinl vii.w R«ii- IACFMI...-
RI:L-VI:|F Film RI.IL- (ACFM)
IVrerni kecjr.lt ... ------
lpiica ID
the in-ttack measuremer.t of particulaie
mailer (PM) cmiiiionB equal lu or lean LJmn
an nerod}*camic diamelcr of nonmully 10
(PMle] from Blalionary Bounces. The EPA
recognizes thai condensible cm: as ion <; not
collected by an jn-atack melhod are also
PM,.. and lhai emiBaions ihal conlnhuie to
ambient. PM,, levels are the sum or
conclensible emissions and emissions
measured by an in-stack PM,, method, such
BS (his method or Method 201. Therefore, for
establishing lource contributions to ambient
levels of PM,.. such as [or emission inventor}*
purpose!. EPA luggesU thai source PM,.
neasuremenl include both in-slack PM.. and
cono'ensible emissions. Condensible
emissions may be measured by an impinger
analysis in combination with Ihii method,
1-2 Principle. A gas sample is extracted at
12 constant flow rcte through an in-Black
sizing device, which separciei PM greater
than PM,.. Vanalions from isokine'ic
sampling condilions ore maintained within
well-defined limits. The paniculate masi it
determined gravimeiric^lly after removal of '
uncambincd water.
r. Apparatus
Note: Method! cited in thia mcihod .TL purl
nf 40 CFR part 60. appendix A.
2.1 Sampling Train. A ichctnatic i>f Ihr
Meihod 201A sampling train it shown in
Figure 1 of ihii method. With the exception of
the PM,. sizing device and in-siack filter, thii
iruin ii the tame at an EPA Mulhod 17 train.
2.1.1 Nonle. Stainleai steel (310 or
) with a sharp tapered leading
~ -^. l!ii.(ven nvz'^tifS that nttet thfc design
ipecificatkm in Figure 2 of this metliod are
recommcnijcd A larger number of nozilci
with small noizie incremenls incirase the
likelihood that a Eir.ple nozzle can be used fur
the entire traverse. If the nazzJcs do not meet
the design spcciHcaliang in Figure - ol this
method, then the nozzle* must mcel the
cnienu in Secliun 52 of this method.
:.!.: PM,. Sizer. Stainle^i steel [3ie or
equivulcnt) capable of determining the PM,.
[ruction. The sizing device shall be either a
cyclone that meets the specifications In
Section 5.2 at this method or a cascade
impactor that ha* been calibrated using the
procedure in Section 5.4 of this method.
2.1.3 Filler Holder. 63-mm. stainless steel.
An Andenen filter, part number SE274. has
been (uund to be acceptable for the m-eiack
Tiller. Note: Mention of trade names ur
specific product) does not constitute
endorsement by !he Environmental Protection
Agency,
2.1.4 Pilot Tube. Same as in Method 5.
Secliun 2.1.3. Tlic pilot lines shall ba made of
heal resiilant tubing and attached lu the
probe with stainless steel fittings.
2.1.5 Probe Liner. Optional, same us in
Method 5. Section 2.1.2,
Z.1,6 Differential Pressure Gauge.
Condenser, Metering System. Barometer, and
Cas Density Determination Equipment. Same
as in Method S. Sections 2.1.4. and 2-1,7
through 2-1.10. retpeclively.
2.2 Sample Recovery.
2^.1 Nozzle. Sizing Device. I'rohe. and
Kilter Holder Crushes. Nylon bristle lirushen
with iluinless steel wire shafts and handles.
properly sized and lhaped for cleaning the
noHle. tiling dedvice. prou« or probe liner.
and filitf holders.
ZJ:.Z Wash Bottles. Clusa Sample SlOfajie
Cpniainors, Pain Dishes. Crntlualed Cylinder
und IJulj ncu. Pluslic 5 c'"':'- ContuinL'rs.
Funnci and Rubber PcL^-a.i. and
Same i-.s; in Mcthuu 5. Scciirns 2.2.2 Ih
2.Z.A, respectively,
2.3 Anuivsis. Ei»me as in Mnthud 5,
Sunlinr. -.J.
The ri-ngcnts fur
recovery, and analysis are the srime ME lliul
specified in Method S, Sections 3.1. 3.2. nnil
3.3. respectively.
4. Procedure
4.1 Sampling. The complexity of tliia
method is such that, in order to aKuin
reliable results, lestert should be trained UM'
experienced with the lest procedures.
4,1.1 PfL-icsl Prcparaiion Sume nv in
Mtihnd 5, Sttiiun 4.1.1.
4.1-1 Preliminary Determinations. Same us
in Mtuhnd S. Suction 4-l.Z. except use the
dirtcliors nn nozzle size selection and
sampl'nc; lime in this melhod Use of am
nozzle grtiiipr than 0.16 in. in diameter
reyuirt a iflmpling port di?r.c:cr of 6 intlics
Also, the required max'..T>/-- -r.ber of
troyerar points at ar-. ill lie 12.
4.1,2.1 The sizing -- - ,;..,. , jc in-stuck
or maintained a! alack le.n^rralurt during
sampling. The blockage effect of the CSR
sampling assembly will be minimal if tho
crosji-ecctional urea of the snrr.plinf;
assembly is 3 percent or less of
-------
Federal Register / Vo!. 55. No. 74 / Tuesday, April 17.1990 / Rules and Reflations
14267
>
U
U
ec
LLf
39
90
80
70
60
50
40
30
20
10
I I
17 < v < 27 m/s
9 < v < 17 m/3
< 9 m/s
I J L I
8 10
AERODYNAMIC DIAMETER
20
40
mi-Jo
Figure 13. Efficiency envelope for the PM10 cyclone.
BILLMO CODE IUO-SO-C
-------
14270
Federal Register / Vol. 55. No. 74 / Tuesday. April 1~. 1990 / Rules and Regulations
operating parameters of the panicle
genera lion syalfcm.
5-2.2.2 Certify ihe raonodispenity of the
particle,1! for each test either by microscopic
inspection of collected particles on fitter) or
by other suitable monitoring technique* such
as an optical pirlicle counter followed by a
multichannel pulie height analyzer. If (he
proportion of multiple!! and satellites in an
aernpol exceeds 10 percent by mass, the
particle generation system is unacceptable
tor the purpose of Ihin tot. Myllipluts nre
particles thai are agglarm-ralRd. and uteliiies
are particles that are smaller than the
specified size range.
$.2.3 Schematic Drawings. Schematic
drawings of the wind tunnel and blower
lyilem and other information showing
complete procedural detaili of the test
atmosphere generation, verities lion, and
delivery technique! shall be turaiihed with
calibration dcta to the reviewing apenrv
5.Z.4 Plow Measurements. Kleaiure the
cyclone air Dow rites with • dry pa* meter
and a stopwatch, or a calibrated orifice
system capable of measuring flow rales to
within 2 pereenl-
S-2.5 Performance Specification
Procedure. Eatabliph letl particle generator
operation and verify particle size
microscopically. If monodisperily ii lo be
verified by measurement* at Ihe beginning
and the end ol the run rather than by en
integrated sample. lhc»e measurements may
be made at this time.
5,15.1 The cyclone cut SIZE, or DM. of a
cyclone ii defined here ai the particle lize
having • 50 percent probability of
penetration. Determine the cyclone flow 'ate
al which DM ii 10 j*m. A suggested procedure
is to vary the cyclone flow rule while keeping
i constant nar'.icle sizi of 10 ^m. Measure ihc
PM collected in the cydons Im,). the eiut hibr
|rn,l- and Ihe (liter (m,). Culculaie eyc)om<
fffir.ii»nr,y [E,J for each How rale at follows:
m.
>. 100
5.1.5.2. Do three replicates end calculate
inc overage cyclone eflicicncy |E^i.,,,] as
follows:
Whert Ei, En. and Ea are replicate
measurements of E..
5.;.i.3 Calculate the standard deviation
Iff) for the replicate muHsurerrientii of E? «s
(£,'+£,«-»-E.1--
If v exceeds o.io, repeal the replicated runs.
5J15.4 Measure the overall efficiency of
the cyclone and nozzle. E*. at the particle
sizes and nominal gai velocities in Table 2 of
this method using Ihe fallowing procedure.
5.2.3.5 Set the air velocity and panicle
size from one of Ihe conditions in Table 1 ol
Ihti method. Establish isokinetic sampling
cnnditioni and the correct flaw rate in the
cyclone (obtained by procedures in this
•eclion) such thai the Die is 10 pm. Sample
lung enough lo obtain ±5 percent precision
on total collected man ai determined by the
prcciiion and the sensitivity of measuring
technique. Determine separately the nozzle
catch (mn). cyclone catch (m*}, cyclone exit
tube |MJ, and collection filter catch (mi) for
each panicle size and nominal gas velocity in
Table 2 of this method. Calculate overall
efficiency (E,) as follows;
following the procedures described in this
section (or determining efficiency,
X100
5.Z.5.B Do three replicates for each.
combination of git velocity and particle tiza
in Table 2 of this method. Use the equation
below to calculate ihe average overall
efficiency (E^.,.i] for each combination
Where Ei, Ea. and Eo are replicate
measurements of £».
5.2.5.7 Use ike formula in Sechon 5.2-5.3
to calculate er for the replica le
meaiurcments. If o- exceeda 0.10 or if the
particle sizes and nominal gaa vKlocitiei are
not within (he limits specified in Table 2 cf
this method, repeal the replicate rung.
518 Criteria for Acceptance. For each of
ihe three gas stream velocities, plot the Ej..,)
as a function of particle eiie on Figure 8 of
this method. Draw imooih curves through all
panicle sizes. E^,) shall be within Ihe
banded region for all size*, and the £.4.^1
shall be 50 ±0-5 percent al 10 pin.
5 J Cyclone Calibration Procedure. The
purpose of this procedure ii to develop the
relationohip between flow rile, gai viscosity,
gm density, anil Dto.
5.3.1 Calculate Cyclone Flow Rate.
Determine (low rales and DWt for three
different particle size* between S |im and 15
(am. one of which shall be 10 pm. All sizes
must be determined within OJ ^rn. For each
size, use a different temperature within SO "C
{lOfl *F) of ihe itmperalure 91 which the
cyclone is to be used and candaci triplicate
runs. A suggested procedure is to keep the
particle size constant and vary the flow rale.
5.3.1.1. On log-In^ graph paper, plot the
Reynolds number (Re) on the abscissa, and
the square root of ihe Stokes 50 number
|(Sil_y))•*! on the ordinate for each
temperature. Use the following equations lo
compute both values:
Re
9 »
where:
0,^=Cyclone flow rale, cm3/$ec.
p = Caa density, g/cm1,
o^sDiametcr of cyclone inlet, cm.
|itw = Viscosity of gas through the cyclone.
micro poise.
IX,=Aerodynamic diameter of a panicle
having a SO percent probability of
penetration, cm.
3.3.1.2. Use a linear regression analysis to
determine Ihe slope (m) and Ihe Y-inlercept
|b|- Use ihe following formula to dutermine
Q. Ine cyclone flow rate required for a cut
lize of 10 MAI.
0.=
(3000!(K,]-b
- t,!tflm-t.a
'where:
me Slope of the calibration line,
b = y-inlercrpi of the calibration tine.
Q,=Cyclone flow rate for m oil lize of 10
jim. cm1/ see.
d «• Diameter of noizle. cm.
T. a Stack gas temperature, R.
P,™ Absolute stack preisure. in. Hg.
M.=Molecular weight of the Hack gas. 1b/
ib-mole.
K, = 4.077X10-'.
5.3.1.3 Refer to the Method 301A
operators manual, entitled Application Guide
for Source P,\1\* Measurement with Constant
-------
Federal Register / Vol. 55, No. 74 / Tuesday. April 17.
/ Rul»:s and Regulations
14269
y iuch that flow disturl.onctK arr
• K.
1-1.2,-,I In order lo maintain a cut K'.T.e uf
10 j*m in llit: sizing device, (he fluw rule
through the sizing device mu»l b« mainlHinrd
at a cunsiunl. disciple value during the run. IF
the sir.mg device Is u cyclone Ihbt meets thiT
design specifics lions in Fipure 3 of this
me I hod use the equations in Figure 4 of thiii
method to calculate three orifice heitds (all):
uin' nt the average Hack iRmperHliire. nnd the
ulluir two at tempcrniures :r2H "C (^5(1 'Fl
of ilii; average nock tempcrHlure. Usr. all
calculated at the nverupc Black Icmpfrriiture
Mb thr pressure hcuil for (he sample flnw rate
an lonp as the stuck lemperalun? during Ilie
run in within 28 'C (50 "F| of tht- avcro^L-
stack temperature. If (he muck temperature
varies by more than -8 'C (511 *F). thuii une
the appropriate AH.
4.1.2.12 If Ihe iliinp dmcc in n cyclone
(hut clues not meel thr dcsipn specificutiunft
in Fipure 3 of this metliod. use the equations
in Figure 4 of ihis method, cxcepi use Ihc
procedures in Section 5.3 of tin* methnJ li>
dr.ltrmme Q,, ihe correc; cyr.lunn fl«i« rule
fnr i, 10 um size.
4.1.2.Z.3 To iiilecl H nuzzle. use tin:
rqualuijih in Figure 5 of this mtiliud tociilcululi*
4pmm and Apmu for each nozzle Hi nil three
ip.mperHtufES. If the sizing device is a cyclone
lhnl does not meel ihe design specification*
in Figuri: 3 of ihis method, ihr. example
worksheets can be used.
4.1 2 2,4 Correci ihe Method 2 ptiut
rt-Hdinpy Lo Method 201A pilot readings by
multiplying Ihe Method 2 piiol readings by
the j. L| nil re of a ratio of Ihe Method 201A pilol
Cf.cfficii-m to the Method 2 pitol coefficient.
Select the nozzle for which Apml. and Ap,*..
bracket nil of the corrected Method Z pilot
readings. If more than one nozzle metis this
requirement, select Ihe nozzle giving Ihe
greatest symmetry. Note that if the expected
pitol reading for One or more points is near a
limit fcr a chosen nozzle, it may be outside
Ihe limits at the lime of the run.
4.1.:_Z.5 Vary the dwell time, or sampling
lime, at each traverse poinl proportionately
with the point velocity. Use the equation* in
Figure 6 of thij method lo calculate the dwell
lime at the first point and at each subsequent
poinl. II is recommended that the number of
minutes smnpled at each point be roundbd ID
ihe ntareil IS seconds.
4-1-3 Preparation of Collection Train.
Same at in Method S. Section 4.1 J. except
ormI direction! about a gloss cyclone.
4,M Leak-Check Procedure. The sizing
device ii removed before the post-teat leuk-
chcck ID prevent any disturbiincc of the
collected lurnpte prior to analysis.
4.1.4.1 Pretest Leak-Cheek." A pretest leak-
check of the entire sampling train, including
the sizing device, is required. Use the leak-
check procedure in Method 5. Seclion 4.1,4,1
to conduct a pretest leak-check.
4.1.4-2 Leak-Checks During Sample Run.
Same as in Method 5. Section 4 1.4.1.
4.1.4.3 Post-Test Leak-Check. A leuk.
check is required at Ihe conclusion of each
sampling run. Remove the cyclone before the
leak-check lo prevent Ihe vacuum created by
the cooling of the probe fross disturbing the
collected wjmint. und uh« ihe procedure in
Method S. Secnun 4.1.4.3 ir cutidun a pmt-
Irnl Inok-checi.
4,1.5 Method 2U1A Train Oiwrmiuit. Smnr
us in Method 5. Settlor 4 : J except unc the
procedure! in iKlt section lur ieokinelic
sampling und now rale bdiuftinenl. Mainluin
the flow rate c&icaiuled in Secnon 4.1JLM of
ihit melhud throu^lmul the run provided ihe
s;ucii temperature is wiihio 23 'C (SO *F) of
the temperature used lu calculate AH. If slack
tcmpcrHiurifs vary by more than ZB 'C (SO *K).
usn the appropriate AH value ailcuiaied in
Section 4.1-Z-I.l of this method, CulculMle the
dwell lime at each iruverse point as in Figure
ft nf this miHhud.
4,1,6 Calculation of Percent Uukinulic
Ratr und Aerudynamic Cul Size |D»]
Culcutme percent mokmetic rate and LX» (SMI:
Calculaiiont. Scriicm 6 uf this rmrtlmd) 10
dolurrnine whether the test WHS valid, or
another lest ran should be made. If there wai
difficulty in maintaining isokinctic gamplinp
mles within the prescribed range, nr if the IX,
is not in HP proper rnnpe because of source
conditions, the Administrator may !•*•
rur.srlieti for po«i>iblc vm-iunce
•i : Sample Recovery. If a cucciidc
;^ipji:lnr ;6 used, use Ihe manufucturrr h
recommundetl procedure! far BHmpk*
recovery If a cyclone is uaed. u*e the suiue
sample recovery UE Ihul in Method S. Seclion
4.2, except an increased number of anmple
recovery containers is required.
4.Z1 ConraiKff Number J (In-Stuck
Filler). The recovery shall be the same as thai
for Container Number 1 in Method S. Section
4-1
4.2.3 Container Number 3 [Cyclone or
Large I'M Calchj. This step is oplionul- The
anisokinetic error for the cyclone PM ia
theoretically larger than the error for the
PMi. catch. Therefore, adding all the
fractions to gel a total FM catch it not an
accurate aa Method 5 or Method 201.
Disassemble the cyclone and remove the
nozzle to recover the large PM Caleb.
Quantitatively recover the PM from the
interior surfaces of the nozzle and cyclone,
excluding the "turn around" cup and the
interior surfaces of the exit tube. The
recovery shall be.the name as thai for
Container Number : in Method S. Section 41
4.2.4 Container A'u/.iiwr J (PM..).
Quantitatively recover the PM iram all of Ihe
surfaces from the cyclone C7.it to the front
half of the in-«uick filler holder, including tho
"turn oround" cup inside the cyclone and the
••Interior surfaces of Ihe exit lube. The
recovery shall be the same ai thai for
Container Number 2 in Method 5. Section 4.2.
4.2-6 Container Number * (Silica Gel). The
recovery shall be the same ai thai for
Container Number 3 in Method S. Section M.
4.2.7 Impinger Water. Same u in Method
1. Seclion 4-2- under "Impmger Water."
4.3 Analysis. Sume an in Method 5,
Seclion 4.3, except handle Method 201A
Container Number 1 like Container Number 1.
Method 3J1A Container Number* - and 3 like
Container Number Z. and Method 2D1A
Container Number 4 like Container Number X
Ute Figure 7 of this method to record the
weights of PM collected. Us« Figure 5-3 in
Method S, Section 4.3, lo record the volume of '
water collected.
4.4 Quality Control lYucetlurm.. Sume Ufc in
MulhutJ S. Section 4.4.
,1. Calibration
Muinlbin an accurate luburmury log ul >iU
CHlibrations.
S.I Probe Nozzle, Pltul Tube, Meiennj;
Svsiem. Probe Healer Caiibrbtion.
Temperature Caiujes. Leak-check of Mtiennn
Sydttm. and Baromelor Same «« in Method S.
Section 1.1 throuflh 5.7, respectively
S.2 Probe Cyclone and N'uxzic
Combinations. The probe cyclone and nnu.lr
comliiniiliaiis need not be calibrated if bulh
meel de«i>!n specificfltiurf in Hfiure* £ onri 3
lit this method If the nozzles (lu nut mi!«:l
design specifications, then teat the cyclone
and nozzle combinations far conformity with
lierfurmunce specifications (I'S's) in Table 1
of this method. If Ihe cyclune does nol meel
di'bi(ir opi-cifichlions. then the ryli:nne und
nuzzle combiniilion shall conform Hi Ihu PS s
and CHlibrutP the cyclune to dcicrmine the
rclutiuniihip belwucn flow nilh. EUB
viHcooity. and gai drimiy. Usf the
proccdureN in Section 5.2 of thin rntlhud in
conduri PS tcsli and the priiccdun'f in
Section 5.3 of lliis method lu eu libra le the
cyclone. The purpose of (he PS tttts are In
cnntorm thut the cyclone and noiilt
f.ombmjlion bus the desired sharpn«Ni of cut.
Conduct the PS tests in a wind tunnel
described in Section 6.2-1 of this method and
particle generation system described in
Section 5-2J: of this mnihad. Use fjve
sizes and three wind velocities n> listed in
Table 2 o( thin method- A minimum of three
replicate nifiasuremcntj of colluciinn
L-ffidcnc>- shall bt pcrfonnt-d fur eiich of the .
IS conditions listed, for a minimum of 45
measurement!.
5.2.1 Wind Tunnel. Perform ihe
calibration and PS tests In a wind tunnel (or
equivalent leji apparatus) upuble of
establishing and maintaining the required gas
i ere am velocities within 10 percent.
5.12 Particle Generation System. The
particle generation system shu!I be capuble of
producing solid mornxlisrjersrd dye piirticlea
with ihe muss median aerodynamic
diaraplen speciHed in Tiible 2 of this melhud,
Perform the particle size dintributiun
verification on an integrated sample obtained
during lh« sumplins period of each lest. An
acceptable alternative is lo verify the size
distribution of samples obtained before and
' after each letl with both samples required lu
meel the diameter and monodispcnily
requirements for an Acceptable test run.
9,2.2.1 Establish the size of the solid dye
particles delivered lo the tesi section of the
wind tunnel by using the operating
parameter! of Ihe particle genera lion system.
and verify them durinc. the tests by
microscopic examination of rjmpirs of Ihe
.particles collected on a membrane filler. The
panicle size, as established by the operating
parameters of the gcnerolion system, shut! be
•within the tolerance specified in Tuble 2 of
this method. The precision of the particle size
verification technique shall be at least ±0-9
urn. and particle size determined by Ihe
verification technique shall nol differ by more
Than 10 percent from that established by the
-------
14272
Federal Register / Vol. 55. No. 74 / Tuesday, April 17. 1990 / Rules and Regulations
r T. , «»' . »„, }
I M, r. J I Q, J
where <3,=0-0:rr54 for metric units (0.156:5
fur Er.gliih ur.iuj,
fl.3.5 Acceptable Results. The results are
acceptable if I»L» cundilions arc me; The
first is that B.a^fti i. D,i c 11,0 yrr.. The
second ii ihni no sanpling points ore oulside
Apni. and Apmu. ur lhat 80 percent < } <. \2Q
percent ard nc more than one sampling point
if ouisiuc ipmill and ip,,.. If Du is less than
0.0 p*rr.. rcjeu the results and repeat the lest.
7. Bibliography
1. Same as Bibliography in Method 5.
:. McCain. ].U.. |.W. Ra'slsinri. and A.D.
XViMiHmson. Kocumnmndcd Mcihndg!o|;y for
ihe Uuterminalion of Particle Size
Distribution* in Dueled Sourepj, Final Report,
Prepared for the California Air Resources
L'oard by Southern Research Institute. May
19B6.
3. Farthing. W.E.. S,S. Dawes. A.D,
Williamson. J.D. McCain. R.S. Mjrun. and
I \V. Rdc'and. Development of Sampling
Methods for Source PMi. Emissions. Southern
ki-scarch Institute for the Environmental
I'mteciion Apcncy. April 1380. NTIS PS B9
UliOrS. EPA/WM/3-B8-OS6.
4. Application Cuide jnr Source PMm
hlccsurement with Constant Scfrrp.'ing Role,
EPA/GOO/3-68-057.
BILLING CODE ISM-SO-M
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Federal Register / Vol. 55. No. 74 / Tuesday. April IT. 199U / Rules and Regulations 14271
Sampling Rate, for directions in lh« use ol
this equation (or Q in ihe setup calculations.
5.4 C«>*~Hde Impaeior. The purpoin ol
CiiiHiratinpH cascade impiictor is In
determine the empirical constant (STKv).
which is specific to ihe impactcw *nd which
permiiB ihe accurate determination of the cut
size of Ihe irnpHCtor stages it Reid conditions.
It in nnl necessary ID calibrate e»ch
Individual impactor. One* un Imrmctorhai
been calibrated, the calibration data can be
applied io other tmpaciore of identical datipn.
5.4.1 Wind Tunnel Same a* in Section
5.2-1 of this method.
5.4.2 Purticle Generation System. Same at
in Section 5,2.2 of this method
14,3 Hardware Configuration for
Calibrations. An impaction stage constraint
un aerofcul to farm circular or rectangular jets.
which are directed toward a suitable
substrate where the larger aerosol puriictai
are collected- For calibration purposes, threu
stage* of the cascitdti imp«ctor »h«ll tie
discussed and designated calibration Huge*
l. 2, and 3. The first calibration Mage consists
of ihe collection substrate of an impaction
stage and all upstream surface* up to und
including Ihe nozzle. This may include other
preceding impsclor Blugci. The second und
third calibration stages consist of each
respective collection substrate and all
upslrcHm surfaces up to but excluding the
collection substrate of Ihe preceding
calibration aluge. Tail maj include
intervening tmpactor stages which are not
designated at calibration ilayci. The cut sizu.
or Dm. o[ the adjacent calibration singes ahull
differ by o factor of not less then l.S and not
more Ihnn ;,Q, For example, if the first
calibrotion tuge h»f » D*P of 12 um. then tha
D-j of the downstream nagc shall be lielween
6 and 8 jim.
5.4.3.1 It is expected, but not necessary.
that thu complete hardware assembly will be
used in each of the sampling runs of tha
calibration end performance determinations.
Only the first calibration stage rnual be letted
under isokinelic sampling conditions. Tha
second and third calibration itagea must be
calibrated with the collection.substrate of the
preceding calibration stage in place, so thai
g»j flow patterns existing in field operation
will be simulated.
5.4.:.: Each of the PMie siogei should be
calibrated *vith thi type of collection
substrate, viicid material (such ai grease] or
glusi fiber, used in PM« measurements. Note
that most materials used as substrate* ai
elevated temperaturei are not viscid ai
normal laboratory conditloru. Tho tubllnuc
material used for calibrations should
minimize particle bounce, yet b* viscous
•enough to (withstand erosion or deformation
by the tmpactor jets and not interfere wild
the procedure lor measuring the collected
PM.
5.4.4 Calibration Procedure. Eaubliih lest
panicle generator operation and verify
particle size minoscopically. If
monodispenity ii to be verified-by
meiisurcments at the beginning and tho end
of the run rather than hy an integrated
sample, these measurements thai! be mudc at
ihis time. Measure in triplicate the PM
collected by the calibration stage (m) and tha
I'M on all surfaces downstream of the
ve citlibratiuR thi^r |m'l lor «ii ul (hi1
flow rn:i'» and psrlicU me cnnibinKliuni
shown in TuUe i ol Ihii meliiod Tech.niqucr,
of niasi mensurement mny inriuijr t'ut- u»p ol
a dye and ipectrophutometer. Piirtir.lef on thi-
upstream side of a jet plate shall b? included
with the Bubhlrale downilreum, except
nqoliimerBtPt of purlicles. which ihal! be
included with the preceding or upmream
substrate. UM ihe lullowing formula to
lR ihe collection efficiency |E) for auch
Vincotiij- consiant. l.Ofj xiw~"
iKR/'K5!!™* >'10"*micrnp<>ia«;/
5,4.4.1 Uie the formula In Section 4^_5J
of thii mi-thnd lo calculate thn standard
deviation lo1) fur Ihe replicate meaiuremenu.
If a- exceeds C.iO. repeat the replicate runs.
5.4.4,: Use the following formula to
calculate the ft-erape collection efficiency
|E.^] fur each set ol replica te
£„.-(£,-»- E= + E=)/3
where Ei, E«. and Ei are i
meaiuremRnti of E,
5 4 4.3 Upe (he (nllowinp formulu to
calculate Slk for unch E..,.
Stk,
SjiAd,
where;
D — Aerodynamic diameter of the lent
particle, cm (glero^Yn.
O = GHB flow rate through the ulibrmion
mage at inlet candiiions, cm'/MM;.
^i=Ca« viscotily, micropoise.
A = Total CTOBs-scctionnl area of the ji.-li o!
the calibration atOHt. cm".
d, = Diameter of one jet of the tolibrution
stuge. cm.
5-4.4-4 Determine 5tk« for each
calibrnliun stage by plotting f^n VITSUM Stk
on log-log papar. Stkis is the Slk number at SO
percent efficiency. Note that particle.bounre
can cause efficiency to decrease at hiph
vnlues of Slk. Thus. 50 percent efficiency can
occur at multiple values of Stk, The
calibration dnia should clearly indicate the
value of Stka» for minimum particle bounce.
Impactor efficiency versus Slk with minimal
particle bounce ii characterized by a
monutonieatly increasing function with
corulunl or increasing slope with increuiiing
Slk.
S.4.4-5 The Slid, of the first calibration
singe can potentially decrease with
decreasing nozzle size. Therefore.
calibration* should be performed with
enough nozzle sizes to provide a measured
value within 2S percent of any nonJe size
ufted in PMn meaiuremcnta.
5.4.5 Criteria For Acceptance. Plot £„, for
the first calibration Mage vertu* the square
root of the ratio of Stk to Stka* on Figure B of
this method. Draw a smooth curve through all
of the points The curve shall be within the
bended region.
0. Calculation)
8.1 Nomenclature. •
!!„-Moisture fraction of stack, by volume.
dlmeniianlos. _• , ,.
. Ci = Viicothy constunt. SI.IS mierapots*
for *K (51.05 micTopoise for *R).
C, =• Viscoaily constenL IU7Z micmpoiW
*K (0-20? micro|H)ise/-R).
C. = Visi-nnilj" constun:. 53.147 mitriipinse/
frMciiun Oi.
Gi= Viacnaiiy constant 74,143 mieropoisc/
fraction H;O.
UM=l "nlul ryelone flow rale ol standard
conditions, dscm/min IdjcT/inini.
T^^Avprage abnolule lemfMrrnlure uf dry
me:!cr, "K ("RJ.
T, = AvefH(!c absylu't- stuck ym
Icmpt-TBture. *K [*R|,
\'ri»a'= Volume of wati-r vapor In pus
lumpiE (ttundiird conditions). «cm (scr).
Vm Total aumpling time, min.
m^. = Viscosity of mixed cyclone gHi,
micro|ioiic.
H.y = Viscosity of itandurd uir. 1R0.1
micropoisH,
0.2 Anulvuis of Cnicudu Impactor DMu.
Uic the nanulucturcr s rccnnimcndud
prnr.cdurps to nn»\\/7M dnm from cnHCudc
impucton.
6.3 An;ilysii of Cyclone Data Use the
following procedures to analyze dnlu from a
dingle Blufie cyclone,
8.3.1 PM,t Weight Determine the PM
catch in the PM» range from the sum of the
weights obtained from Container Numbers 1
and 3 IMR the acetone blank.
0,3.2 Tcnal PM Weight (optional).
Determine the TM catch for prenter than PMw
from the weight obtained from Container
Number 2 Inti the acetone blank, and add ii
la the f*Mi» weight.
6J.3 PM,i Fraciion. Determine the PMn
fracuun of the total particulBtB wciphl by
dividing the PMu pftrttculule weight by the
total paniculate weight.
6,3.4 Aerodynamic Cm Size, Calculate ihe
Black gui viscosity as followi:
^, - C, 4- C.T, + C,T.«4- C,!,,- &U»,
ft.3.4 1 The PMio flow rate, at actual
cyclone condition*, is calculated a* follows:
tt.3.4.2 CnleuJate the molecular weiphl on
a wot basia of the Hack gai •• fnUowa;
ftj.4 J Calculate the acUuil DM of ths>
cyclnne for the given conditions an follows:
-------
14374
federal Regfoter / Vol. 55. No. 74 / TXiesday. April 17.1B80 f Rules and Regulations
Diameter
(inches)
C.136
0.150
0.164
0.130
O.IS7
0.215
0.233
0.264
0.300
0.3-52
C.33Q
Cone
Angle, 8
[degrees)
4
4
5
6
6
6
Outside
tapec, $
(degrees)
15
15
15
15
15
15
15
15
15
15
15
Straight inle:
length, I
(Inches)
<0.05
<0.05
CO.05
<0.05
<0.05
<0.05
CO.05
CO. 05
<0.05
Toe a I Ui.ig1
L
(inches)
1.970±0.05
1.571*0.05
1.491±0.05
1.45 ±0.35
1.45 10.05
1.45 iO.OS
1.43 tO.05
1.45 ±0.05
1.45 iO.05
Figure 2. Nozzle design specifications,
77
-------
IMPINGER TRAIN
PM 10
SAMPLER
FILTER HOLDER
HEATED PROBE
*n
NOZZLE
*
•STIPE
PfTOTTUaE
DISTILLED WATER EMPTY SILICA GEL
INCLINED
MANOMETER
•n
s.
2
OJ_
X
re
w
at'
<
2-
in
in
7.
o
FLOW CONTROL SYSTEM COARSE
FINE \
.CALIBRATED "•% 4
VACUUM
GAUGE
VACUUM
PUMP
^ INCLINED
"MANOMETER
* DRfGAS
METER
H
to
Ul
Q.
01
>
•o
Figure 1. CSR Sampling Train
ya
£_
S"
tn
a>
3
D-
?
13
O
3
u
76A
fe
U
-------
U276 Federal Register / Vol. 55. No. 74 /Tuesday. April 17, 1990 / Rules and ReyjLationa
Barometric; pressure.
Stack static pressure.
Average stark temperature.
Meter lemperaiurt. lm, T =
Orifice AM., in. II Q =
Has onulvsis:
i',rn- _
••K. + v.rn-
p..- is, 6
Molecular weight of stark gua. dry basis;
MJ=O.-M (?bCOa) + o.32(*.Oi)-*-o.z8
ItrJ.j.VCOf. Ih/ll.mnlP Viieosisy of stack fuw:
Molecular weigh; of iinek gas. we. busisi M. = 152.41 8 + 0.2552 U + 3.23S3X1D-
M.-r4,[1-B..)-lB(B..j= 1W >. =+0.53117 (','J3-)-T4.1«D..=
i|. ... ..i. mirropniio
Absolute stack pressure: Cyclone GJW rale:
, [I. + 400) i n::wg
°' ^ 1 M.P. J " '
Figure 4. Exumple workshei.-! 1. ryrione
law rale and AM.
Orifice prcuure head (AH) needed fur
cyclone Dow rate;
Q, |1-B«) P. | ln M, 1.0U iH»
ii i — i • =
1. + 400 ' P..,
lalcuLle AH for three !cirpcr:;tiin:K Slack viBCuailv. ^
mirropoisp = _
l- f
H.O
• Absolute alack pressure.
p_t> HB -
Average stack temperature.
•„ 'r "
<-.i~>?T t^rwyrstura . i^. T = ..,
s ' • ""A pitot-co«rncient.
tn. it.u
Cvclonc flow rule, fl'/min. .
Q. =
Method 2 pilot coefficient.
Molecular weight of alack gas.
V _
Noizle velocity:
wet buaii.
3.056 Q,
. fl/tec
Maximum and mlnimurn velocities:
O.MS7 + f
0-2WU Q
].].
. fl/sec
i
0 44ST + 0-S600 -
r oi&nQ.**. . 1.
0-S600 - M, =
I .„" i J
election.
S. Example worksheet 2. noale
values:
ucid ™injjT«Mm velocity hnul
Ap... a 1-3036 X 10"
P. M. Iv-
-------
Federal Register / Vol. 55. No. 74 / Tuesday. April 17. iggp / Rules and Regulations
Cyclone Interior Dimensions
14275
0.10 in.
cm
inches
Dimensions (±0.02 cm, ±0.01 in.)
Din
1.27
o.sa
D
4.47
1.76
Der
1.5Q
0.59
B
l.BB
0.74-
H
6.25
174
h
L24
0.88
Z
4.71
1.S5
s
1.57
0.52
Hcup
2,25
0.89
Dcup
4.45
1.75-
D;
1.02
0.4U
Da
1.24
0.49
Figure 3. Cyclone design specifications.
OILUMO COOt
-------
14278 Federal Register / Vol. 55. No. 74 / Tuesday. April 17, ]990 / Rules and Regulations
TABLE 2.—PARTICLE SIZES AND NOMINAL
GAS VELOCITIES FOB EFFICIENCY
Pimcie tit • 7*f9" 9**
lum|' 7 = 1.0 i I5=l.i ! 25^-2.5
5 ±0.5
7=0,S
10 ±.0.5..
14; l.O... L
20- 1.0...
1
'Muss median aerodyn.iniiL (i,.inirliT
BILLING CODE
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Federal Register / Vol. 55. No. 74 / Tuesday. April 17. 1990 / Rules and Regulations 14277
v. M. (v.^p
It. -i- "WiO) Q>
in. II..O
Noiria No.
D H
. F'siw-
io ! in. HjO . ..»™. ......
Inii-erfr rl;ilii:
' r u
liilrM a o.p{Mi:ihoil 2|
I r -
Dial run lime, minutes =
Number of travnrse point" = ,
Ap'i
Ap...
(Tntul run lime)
(Number uf points)
where:
It = dwell linie ni nrsl traverse poinl
minutcj.
an'i = the velocity hcftd HI the [irs! (ravcm:
poinl [from a pruvioui traverse), in. H-0.
Ap'..i»>tlit.' syujre of the average iquure
root of the ilp's (from D previous vuUicity
Irnvcrof-l. In. IliO.
Al miliHf.quent iravcrse poiniE. men surf !hu
vciocily Ap and calculule the dwelt lime
by U5inp the following cqtiHiion:
1,
UP.)1*
'•*. n = Z3.' ' " lalul nurclier of ftumplinfi pdlntB
where: &p.= miiusured vplctclly hcud ul point n. in.
L, = divoll time HI L-Sverse point n. minulu.i. H-0.
a p, =>d»el! lime ul finii iruvunt puinl.
minulL-s.
FipureS. Exnniplt worksheel 3. d«i;U tinm.
Po-n: No,
!
•
f.un no.
Filter no ,
Pon
io
i
~"~T
....... i
AD t 00
1 |
| i
1 4P I
I .... ... .,
1
1 J ....
. ( j
i* ' ^""i
i i ; " • "i " •"
Amount of liquid lost during
Ir^nspart
Acetone blun
Acetone was
L 1 1
i volume, ml (4)
Acetone bliink cone., mg/mg (EquHlian S~«.
Method 5|
Acelone wesh blank, mg (Equation S-S.
Method 5) _,
ConUimrMo,
,
3
Toiai
Less acBlono
bla"* _
Wsigfn ol PM»..
Weighi ol PM,. (mg)
Fmal Tan? Wwgtii
i
1 j
\ i
Figure 7. Method 301 A analysis sheet.
TABLE i. — PERFORMANCE SPECIFICA
TIONS FOR SOURCE PMii, CYCLONES
AND NOZZLE COMBINATIONS
Pinvnew
l. Crtlaetion
affiooncy.
2. Cyclone cut
tat (Off).
Umu
Pwceni..._
Speciha lions
Sucniruu
col lection
efficiency lain
wiinin ciweiope
ipecil«d by
Section 5.2.6
•no Figure a.
•erMynamic
diamaliy.
-------
Federal Rejjisier / Vol. 55. No. 74 / Tuesday. April 17, 1990 / Rule? and Resuiations
14279
>
u
S3
90
80
t M
Ul
$ M
I 40
ff 3D
20
10
5
17 < v < 27 m/»
9 C » < 17 m/s
v < 9 m/s
2 * 6 fl 10 20 40
AERODYNAMIC DIAMETER (pm)
IIU-JI
Figure 3. Efficiency envelope for the PM:B cyclone.
«
90
>
M S3
u
5 70
w
u 60
1 50
^ 4C
10
10
5
17 < v < S7 tn/i
9 < v < 17 m/i
f < 9 m/i
1
0.4 0.6 OJ5 1
1TI1-JL
Figure 9. Efficiency envelope for first calibration sea go,
IFR Doc. 8o-rao3 Fiiod *-io-w; e,*5 om]
*UJMO CODE IHD-fO-C
-------
EPA Pa/llculala
Ruluitmcti Muiliotls
5. 201, ami 201A
Sani|iling Componunis
Figure
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
CONDITIONAL TEST METHOD
Determination Of Condenslble Emissions
From Stationary Sources
1. APPLICABILITY AND PRINCIPLE
1.1 Applicability. This method applies to the determination of condensible
particulate matter (CPM) emissions from stationary sources. It is intended to
represent condensible matter as material that condenses after passing through
an in-stack filter (Note: The filter catch can be analyzed according to
Method 17 procedures). This method may be used in conjunction with Method 201
or 201A if the probes are glass lined. This method may also be modified to
measure material that condenses at other temperatures by specifying the filter
temperature.
1.2 Principle. The CPM is collected in the impinger portion of a Method 17
(Appendix A, 40 CFR Part 60) type sampling train. The impinger contents are
immediately purged after the run with nitrogen (N-) to remove dissolved sulfur
dioxide (SO.) gases from the impinger contents. The impinger solution is then
extracted with methylene chloride (MeCK). The organic and aqueous fractions
are then taken to dryness and the residues weighed. The total of both
fractions represents the CPM.
2. PRECISION AND INTERFERENCE
2.1 Precision. The precisions based on method development tests at a wood i
waste burner and two coal-fired boilers are 13.0 ± 2.1 mg/m3, 3.5 ± 1.1 mg/m3,
and 39.5 + 9.0 mg/m3, respectively.
2.2 Interference. Ammonia (e.g., in sources that use ammonia injection as a
control technique) Interferes by reacting with the hydrogen chloride (HCl) in
the gas stream to form ammonfum chloride (NH4C1) which would be measured as
CPM. The sample may be analyzed for chloride and the equivalent amount of
NHjCl can be subtracted from the CPM weight.
3. APPARATUS
3.1 Sampling Train. Same as in Method 17, Section 2.1, with the following
exceptions noted below (see Figure I). Note: Mention of trade names or
specific products does not constitute endorsement by EPA.
3.1.1 The probe extension shall be glass-lined.
Prepared by Candace Sorrel!, Emission Measurement Branch EMTIC CTM-005
Technical Support Division, OAQPS, EPA March 21, 1990
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EHTIC CTM-005 EMTIC CONDITIONAL TEST METHOD Page 3
4.2.1 Hz Gas. N2 gas at delivery pressures high enough to provide a flow of
20 liters/win for 1 hour through the sampling train.
4.2.2 Hethylene Chloride.
4.2.3 Water. Same as in Section 4.1.
4.3 Analysis. Same as in Method 5, Section 3.3, with the following
additions:
4.3.1 Hethylene Chloride.
4.3.2 Ammonium Hydroxide. Concentrated (14.8 M) NH4OH.
4.3.3 Water. Same as in Section 4.1.
. oS Zo
4.3.4 Phenolphthalein. The pH indicator solution, "M percent in "SO percent
alcohol.
5. PROCEDURE
5.1 Sampling. Same as in Method 5, Section 4.1, with the following
exceptions: ' '"
5.1.1 Place 100 ml of water in the first three Impingers.
5.1.2 The use of silicone grease in train assembly is not recommended.
Teflon tape or similar means may be used to provide leak-free connections
between glassware.
5.2 Sample Recovery. Same as in Method 17, Section 4.2 with the addition of
a post-test N2 purge and specific changes in handling of individual samples as
described below.
5.2.1 Post-test H2 Purge for Sources Emitting SO-. (Note: This step Is
recommended, but is optional. When no or little S02 is present in the gas
stream, I.e., the pH of the Impinger solution is greater than 4.5, purging has
been found to be unnecessary.) As soon as possible after the post-test leak
check, detach the probe and filter from the impinger train. Leave the ice in
the impinger box to prevent removal of moisture during the purge. If
necessary, add more Ice during the purge to maintain the gas temperature below
20'C. With no flow of gas through the clean purge line and fittings, attach
it to the Input of the impinger train (see Figure 2). To avofd over- or
under-pressurizing the Impinger array, slowly commence the N2 gas flow through
the line while simultaneously opening the meter box pump valve(s). Adjust the
pump bypass and N2 delivery rates to obtain the following conditions:
(1) 20 llters/min or AH, and (2) an overflow rate through the rotameter of
less than 2 liters/min. Condition (2) guarantees that the \ delivery system
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EMTIC CTM-OOS EMTIC CONDITIONAL TEST METHOD Page 2
3.1.2 A Teflon fllttr support shall be used.
3.1.3 Both the first and second impingers shall be of the Greenburg-Smith
design with the standard tip.
3.1.4 All sampling train glassware shall be cleaned prior to the test with
soap and tap water, water, and rinsed using tap water, water, acetone, and
finally, MeClL. It is Important to remove completely all silicone grease from
areas that will be exposed to the MeCl2 during sample recovery.
3.2 Sample Recovery. Same as in Method 5, Section 2.2, with the following
additions:
3.2.1 N, Purge Line. Inert tubing and fittings capable of delivering
0 to 28 liters/min of N2 gas to the impinger train fnjra a standard gas
cylinder (see Figure 2). Standard 0.95 cm (3/8-inch) plastic tubing and
compression fittings in conjunction with an adjustable pressure regulator and
needle valve may be used.
3.2.2 Rotaineter. Capable of measuring gas flow at 20 liters/min.
3.3 Analysis. The following equipment is necessary 1n addition to that
listed in Method 5, Section 2.3: . .
3.3.1 Separatory Funnel. Glass, 1-liter:
3,3.2 Weighing Tins. 3iQ-ml.
3.3.3 Drying Equipment. Hot plate and oven with temperature contro;.
3.3.*--SurytlTJ.—t^ml size w-ith Q.Ol il graduations.
3.3.5 Pipits. l-flil.
3.3.6 Ion Chromatograph. Same as in Method 5F, Section 2.1.6.
4. REASENT5
Unless otherwise indicated, all reagents must conform to the specifications
established by the Committee on Analytical Reagents of the American Chemical
Society. When such specifications are not available, use the best available
grade.
4.1 Sampling. Same as In Method 5, Section 3.1, with the addition of
deionized distilled water to conform to the American Society for Testing and
Materials Specification D ll§3-74, Type II.
4.2 Sample Recovery. Same as in Method S, Section 3.2, with the following
additions:
-------
EMTIC CTM-005 EMTIC CONDITIONAL TEST HETHOO Page S
(Note: Do not use this aliquot to determine chlorides since the HC1 will be
evaporated during the first drying step; Section 8.2 details a procedure for
this analysis.)
5.3.2.1 Extraction. Separate the organic fraction of the sample by adding
the contents of Container No. 5 (MeCl?) to the contents of Container No. 4 in
a 1000-ml separatory funnel. After mixing, allow the aqueous and organic
phases to fully separate, and drain off most of the organic/Medz phase. Then
add 75 ml of MeCl, to the funnel, mix well, and drain off the lower organic
phase. Repeat with another 75 ml of MeCl2. This extraction should yield
about 250 ml of organic extract. Each time, leave a small amount of the
organic/HeCl2 phase in the separatory funnel ensuring that no water is
collected in the organic phase. Place the organic extract in a tared 350-ml
weighing tin.
5.3.2.2 Organic Fraction Weight Determination (Organic Phase from Container
Nos. 4 and 5). Evaporate the organic extract at room temperature and pressure
in a laboratory hood. Following evaporation, desiccate the organic fraction
for 24 hours in a desiccator containing anhydrous calcium sulfate. Weigh to a
constant weight and report the results to the nearest 0.1 mg.
5.3.2.3 Inorganic Fraction Weight Determination. Using a hot plate, or
equivalent, evaporate the aqueous phase to approximately 50 ml; then evaporate^
to dryness in a 105'C oven. Redissolve the residue in 100 ml of water. Add "'
five drops of phenolphthalein to this solution, then add concentrated
(14.8 M) NHjQH until the sample turns pink. Any excess NH^OH will be
evaporated during the drying step. Evaporate the sample to dryness in a 105'C
oven, desiccate the sample for 24 hours, weigh to a constant weight, and
record the results to the nearest 0.1 mg. (Note: The addition of NH^OH is
recommended, but Is optional when no or little SOZ is present in the gas
stream, i.e., when the pH of the impinger solution is greater than 4.5, the
addition of NH4OH is not necessary.)
5.3.2.4 Analysis of Sulfate by 1C to Determine Ammonium Ion (NH/) Retained
In the Sample. (Note: If NH4OH is not added, omit this Step.) Determine the
amount of sulfate tn the aliquot taken from Container No. 4 earlier as
described in Method 5F (Appendix A, 40 CFR Part 60). Based on the 1C SO/
analysis of the aliquot, calculate the correction factor to delete the NH4"
retained in the sample and to add the combined water removed by the acid-base
reaction (see Section 7.2).
5.3.3 Analysis of Water and HeCl2 Blanks (Container Nos. 6 and 7). Analyze
these sample blanks as described above 1n Sections 5.3.2.3 and
5.3.2.2, respectively. The sum of the values for the water blank and the
HeCl2 blank must be less than 2 mg or 5 percent of the mass of the CPM
(ma + rar), whichever Is greater. If the sum of the actual blank values Is
greater, then subtract 2 mg or 5 percent of the mass of the CPM, whichever 1s
greater.
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EHTIC CTM-005
erric CONDITIONAL TEST METHOD
Page 4
1s operating at greater than ambient pressure and prevents that possibility of
passing ambient air (rather than N2) through the itnpingers. Continue the
purge under these conditions for 1 hour, checking the rotameter and AH
value(s) periodically. After 1 hour, simultaneously turn off the delivery and
pumping systems.
5.2.1 Sample Handling.
5.2.2.1 Container Nos. 1.2. and 3,
detailed in Method 5, Section 4.2.
If filter catch is to be determined, as
5.2.2.2 Container No. 4 (Impinger Contents). Measure the liquid in the first
three impingers to within 1 ml using a clean graduated cylinder or by weighing
it to within 0.5 g using a balance. Record the volume or weight of liquid
present to be used to calculate the moisture content of the effluent gas.
Quantitatively transfer this liquid into a clean sample bottle (glass or
plastic); rinse each impinger and the connecting glassware, including probe
extension, twice with water, recover the rinse water and add it to the same
sample bottle. Mark the liquid level on the bottle.
5.2.2.3 Container No. 5 (MeCl2 Rinse). Follow tne water rinses of each
impinger and the connecting glassware, including the probe extension with two
rinses of MeCl2; save the rinse products in a clean, glass sample jar. Mark .
the liquid level on the jar.
5.2.2.4 Container No. 6 (Hater Blank). Once during each field test,
500 ml of water in a separate sample container.
pi acs
5.2.2.5 Container No. 7 (MeCl2 Slank). Once during each field test, place in
a separate glass sample jar a volume of MeClz approximately equivalent to the
volume used to conduct the MeCl2 rinse of the impingers.
5.2.2.6 Container No.8 (Acetone Blank).
Section 4.2.
As described in Method 5,
5.3 Analysis. Record the data required on a sheet such as the one shown in
Figure 3. Handle each sample container as follows:
5.3.1 Container Nos.
_3. If filter catch 1s analyzed, as detailed
in Method 5, Section 4.3.
S.3.2 Cental ne^jios.4 and 5. Note the level of liquid in the containers and
confirm on the analytical data sheet whether leakage occurred during
transport. If a noticeable amount of leakage has occurred, either void the
sample or use methods, subject to the approval of the Administrator, to
correct the final results. Measure the liquid In Container No. 4 either
volumetrically to ±1 ml or gravimetrically to ±0.5 g. Remove a 5-ml aliquot
and set aside for later Ion chromatographic (1C) analysis of sulfates.
-------
EMTIC CTH-005
EHTIC CONDITIONAL TEST METHOD
Page 7
7.3 Mass of Inorganic CPU.
- mb + mc
Eq. 2
7.4 Concentration of CPU.
m
•cpm
Eq. 3
sid
8. ALTERNATIVE PROCEDURES
8.1 Determination of NH4" Retained in Sample by Titration.
8.1.1 An alternative procedure to determine the amount of NH/ added to the
Inorganic fraction by titration may be used. After dissolving the inorganic
residue in 100 ml of water, titrate the solution with 0.1 N NH^OH to a pH of
7.0, as indicated by a pH meter. The 0.1 N NH4OH is made as follows: Add"
7 ml of concentrated (14.8 H) NH^QH to- 1 liter of water. Standardize against
standardized O.I N H2SOj and calculate the exact normality using a
procedure parallel to that described in Section 5.5 of Method 6 (Appendix A,
40 CFR Part 60). Alternatively, purchase 0.1 N NH4OH that has been
standardized against a National Institute of Standards and Technology
reference material.
8.1.2 Calculate the concentration of S04" in the sample using the following
equation.
•S04
-48.03 Vt N
100
Eq. 4
where:
N - Normality of the NH4OH, mg/ml.
Vt - Volume of NH4OH titrant, ml.
48.03 • mg/meq.
100 - Volume of solution, ml.
8.1.3 Calculate the CPM as described in Section 7.
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EMTIC CTM-OOS EMTIC CONDITIONAL TEST METHOD Page 6
5.3.4 Analysis of Acetone Blank (Container No. 8). Same as 1n Method 5,
Section 4.3.
6. CALIBRATION
Same as 1n Method 5, Section 5, except calibrate the 1C according to the
procedures in Method 5F, Section 5.
7. CALCULATIONS
Same as in Method 5, Section 6, with the following additions:
7.1 Nomenclature. Same as in Method 5, Section 6,1 with the
following additions.
"cpn
Concentration of the CPM in the stack gas, dry basis, corrected to
standard conditions, g/dscm (g/dscf).
CS04 - Concentration of SO/ in the sample, mg/ml.
mb • Sum of the mass of the water and Medz blanks, mg.
mr • Mass of the NH/ added to sample to form ammonium sulfate, mg.
mi - Mass of inorganic CPM matter, mg.
ma - Mass of organic CPM, mg.
mp - Mass of dried sample from inorganic fraction, mg.
mrc • Mass of dried sample from inorganic fraction corrected for volume
of aliquot taken for 1C analysis, mg.
Vb - Volume of aliquot taken for 1C analysis, ml.
Vje • Volume of impinger contents sample, ml.
7.2 Correction for NH4~ and H20. Calculate the correction factor to
delete the NH4" retained in the sample and to add the combined water removed
by the acid-base reaction based on the 1C SO/.
roc - K CSM Vie Eq. 1
where:
K - 0.020502
j
'V
-------
Thermocouple Checfc
T Valve
UtuWhenPiaing
Hiltogan lluotigti System
Figure 2. Scliemni.\c oT'pnst-teaL niti-o^en purge system.
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EMTIC CTH-005 EMTIC CONDITIONAL TEST METHOD Page a
8.2 Analysis of Chlorides by 1C. At the conclusion of the final weighing as
described in Section 5,3.2.3, redissolve the inorganic fraction in 100 ml of
water. Analyze an aliquot of the redissolved sample for chlorides by 1C using
techniques similar to those described in Method 5F for sulfates. Previous
drying of the sample should have removed all HC1. Therefore, the remaining
chlorides measured by 1C can be assumed to be NH4C1, and this weight can be
subtracted from the weight determined for CPM.
8.3 Air Purge to Remove SO. from Impinger Contents. As an alternative to the
post-test Nz purge described in Section 5.2.1, the tester may opt to conduct
the post-test purge with air at 20 liter/min. Note: The use of an air purge
is not as effective as a N2 purge.
9. BIBLIOGRAPHY
1. DeWees, W.O., S.C. Steinsberger, G.M. Plummer, L.T, Lay, G.D. McAlister,
and R.T. Shigehara, "Laboratory and Field Evaluation of the
EPA Method 5 Impinger Catch for Measuring Condensible Matter from Stationary
Sources." Paper presented at the 1989 EPA/AWMA International Symposium on
Measurement of Toxic and Related Air Pollutants. Hay 1-5, 1989. Raleigh,
North Carolina.
2. DeWees, W.D. and K.C. Steinsberger. "Method Development and Evaluation of
Draft Protocol for Measurement of Condensible Particulate Emissions." Draft
Report. November 17, 1989.
3. Texas Air Control Board, Laboratory Division. "Determination of
Particulate in Stack Gases Containing Sulfuric Acid and/or Sulfur Dioxide."
laboratory Methods forDetermination of Air Pollutants. Modified December 3,
1976.
4. Nothstein, Greg. Masters Thesis. University of Washington Department of
Environmental Health. Seattle, Washington.
5. "Particulate Source Test Procedures Adopted by Puget Sound Air Pollution
Control Agency Board of Directors." Puget Sound Air Pollution Control Agency,
Engineering Division. Seattle, Washington. August 11, 1983.
6. Commonwealth of Pennsylvania, Department of Environmental Resources.
Chapter 139, Sampling and Testing (Title 25, Rules and Regulations, Part I,
Department of Environmental Resources, Subpart C, Protection of Natural
Resources, Article III, Air Resources). January 8, 1960.
7. Wisconsin Department of Natural Resources. Air Management Operations
Handbook. Revision 3. January 11, 1988.
-------
Moisture Determination
Volume or weight of liquid in impingers_
Weight of moisture in silica gel ~
ml or g
9
Sample Preparation (Container No. 4)
Amount of liquid lost during transport
Final volume
pH of sample prior to analysis
Addition of NH4OH required?
Sample extracted 2X with 75 ml MeCl2?
For Tltratlon of Sulfate
Normal i.ty of NH4OH
Volume of sample titrated
Volume of titrant
ml
ml
N
ml
ml
Sample Analysis
Container
number
Weight of Condensible Particulate, mg
Final Weight Tare Weight Weight Gain
4 (Inorganic)
4 i 5 (Organic)
Total
Less Blank
Weight of Condensible Particulate
Figure 3. Analytical data sheet.
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APPENDIX J.3
ALDEHYDES
-------
3-5 Sampling fag ftldahvde &*$ Kjeone Emissions frqB |Wyanarv Sources
(Meshod 00 m
Scope and ABB!{.cation
.his aechod is applicable to the dactnsination of Destruction and Removal
Efficiency (ORE) of formaldehyde, CAS Registry nuabar 50-00-0, and possiblv
o:her aldehydes and ketones Iron stationary sources as specified in the
regulations. The nethodology has been applied specifically co formaldehyde,
however, many Laboratories have extended ch« application co other aldehydes
and kecones. Compounds derivacized with 2,4-dinicrophenyl-hydrarme can be
dececced as lov as 6.4 x 10** Ibs/cu fc (1.8 ppbv) in scack gas over a I hr
sampling period, sampling approximately 43 cu £c.
3,5.2 Suaaarv of Method
3.5.2-1 Gaseous and parcicuiac* pollutants are withdrawn isokine-
ci-cally from an emission source and are collected in squeou* acidic 2 . ^ •
dinicrophenyi-hydrazine. Formaldehyde present In the emissions resets vi:h
:he 2 >-dinicrophenyl-hydrazine co fonn the formaldehyde dinitrophenyihycira-
zone derivative. Th* dinitrophenylhydrazone derivative it extracted, ioiver.:-
exchanged, concentrated, and then analyzed by high performance liquid chroma-
;ography.
3.5.3 Incarfereneaa
3.5.3,1 A decooposition produce of 2,4-dinitrophenyl-hydrazine,
2,^-dinitroanilin*. can b« an analytical interferant if concentrations are
high. 2.4-Dinitroanlitne can coelute with 2>-dinitrophenylhydrarone of
foraaldehydUi und«r high performance liquid chrooutography condition*, which
nay be used for tha analysis. High concentration* of highly-ouygiaatad
compounds, especially acetone, that have the saae retention time or nearly the
saae retention time aa tha dinitrophenylhydrazone of formaldehyde, and that
also absorb ac 360 na, will interfere with the analysis.
3-151
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Formaldehyde, act cant, and 2.4.dinicrosnlllns coneaainatton of the
acidic 2,4-dinicrophenyl-hydrazir.e (DNPH) reagent is frequently
The reigenc BUJC be prepared within five days of use Ln che field and ausc be
scored in an unconcamLnated environment 2och before and after saapling in
order co ninimist blank problem. Son* concentration of aescone contamination
is unavoidable, because ace cone Is ubiquitous in laboratory and field opera-
tions. However, che acetone concaninatton muse be ainiaized
3,5.4 Apparatus and Maeerialj
3-5.4.L A schemacic of cht saapling crain is shown in Figure
3.5-1- This sampling crain configuracion is adapced from EPA Mechod 4
procedures. The sampling crain conaiscs of the following coaponencs: Probe
Nozzle, PicoC'Tube, Differencial Pressure Gauge, Metering System, Baroaecer,
and Gas Density Determination Equipmenc.
3.9.4.1.1 Probe Mottle: Quarcz or glais with sharp, capered (30*
an§L«) leading tdg«. 7h« cap«? shall t>« on ch* outs id* to preserve a cansnar.-
inner dianecer. The nottle shall b* buttonhook or elbow dajign, A range of
nozzle siin suitable for isokinecic saapling should be available in incre-
ments of 0.15 cm(l/U in), e.g.. 0.32 to 1.27 ca (1/8 to 1/2 In), of larger if
higher volume saapling trains are used. Each nozzle shall b* calibrated
according to the procedures outlined in Section 3.5.8.1
3.5.4.1.2 Probe Liner: Borosillcace glass or quartz shall be used
far the prob* liner. The Miter should not allow che ceaperacure in ch* probe
co exceed 120 ± U'C (241 ± 23*F).
3.3,4.1.3 Pltot Tube: The Plcot tub* shall b* Type S, as described
in Section 2.1 of BfA Method 2, or any other appropriate device, The pitot
cube shall be acetched to che prob* co allow constant aonlcorlng of the stack
gas velocity. The i.apace (high pressure) opening plan* of the pltot cube
shall b* even with or above the notzle entry plan (see EPA Method 2. Figure 2-
6b) during sampling. The Type S pitot cub* assanbly shall have a known
coefficient, determined as outlined in Section 4 of EPA Method 2.
3-134
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ThoMnonMM
Form,jkli:liy
-------
3.5.4.1,4 Differencial Pressure Gauge: The differencial press-are
gauge shall b* an inclined manometer or equivalent device as described in
Section 2.2 of E?A Method 2. One manometer shall be ui«d far velocity-head
reading and the other for orifice differential pressure readings.
3.5.4.1.5 Impingeri: The sampling train requires a minimua of four
iapingers, conntcced as shovn in Figure 3,5-I, wieh ground glass (or equiva-
lent) vacuum*cighc ficcinjs. For the first, third, and fourth impingers, use
che Greenburg-Smith design, modified by replacing the tip with * 1.3 cm ir,s:da
diameter (1/2 in) glass cube extending to 1,3 cm (1/2 in) from the bottom of
the flask. For the second irapinger. use a Greenburg-Salth impinger with the
standard tip. Place a thermometer capable of measuring temperature to within
1'C (2*f) at ch« outlet of the fourth impinger for aonitoring purposes.
3.5.4.1.6 Metering System: The) necessary components are a vacuum
gauge, leak-free pump, thermometers capable of ae>a*uring temperature within v
3"C (3.4*F), dry-gas mecer capable of measuring volume co within It, and
re Laced equipment as shown in Figure) 3.5-1. Ac * minimum, che puap should be
capable of 4 cfm fret flow, and che dry few o*cer should have « recording
capacity of 0-999,9 cu fc with a resolution of 0.005 cu ft. Other metering
systems may be used which are capable of maintaining sample volumes co withi-
21. The metering systea may be used In conjunction wish a ptcoc cube co
enable cheeks of isokineclc sampling races.
3,5.4.1.7 Barometer: The baromecer aay be aercury. aneroid, or
other barooflear capable of naaiuring atmogpheric pressure CO within 2.5 no Hg
(O.I in Kg), In aany CAJC«, the) barometric reading aay be obtained from a
nearby SacIon*! Weather Service Station, in which case che station value
(which is ch« absolute baroaetric pressure) is requested and an adJuJCmenc for
elevation differences between the weather station and sampling point is
applied at a race of minuj 2.1 ma H§ (0,1 in Hg) per 30 a (100 ft) elevation
increases (vice versa for elevation decrease).
3.5.4.1.8 Gas Density Oeceruination Equipment: Temperature sensor
and pressure gauge (as described in Sections 2.3 and 2.3 of EPA Method 2). and
3-156
-------
gas analyzer. If necessary (as described in EPA Method 3). Th« temperature
sensor ideally should b» permanently attached co che pieoc cube or saapiing
probe in a flxid configuration such chat cha tip of the sensor extends beyond
the Leading «dge of cha probi sheazh and dots noc couch any cnecal. Alterna-
tively, the sensor may ba attached just prior co uaa in the field, Soce,
however, that If the temperature sensor Is attached in cha fitld, the ser.sor
-Tusc be placed in an intarferenca-fraa arrangement wLch respecc co cha Tvpe S
pi:oc openings (sea EPA Kachod 2, Flgura 2-T), A* a second alternative, if a.
difference of no aora chan It In cha avaraga velocity measurement is to be
incroduced, cha cenparature gauge need noc be attached co cha probe or ?::=:
tuba.
3.5.^,2 Sample Recovery
3.5.4.2.1 Probe Liner: Probe nozzle and brushes; Taflan bristle
brushes with scainlass steal wire handles are required. The probe brush shall
have extensions of stainless steal, Teflon, or inarc material at least js lar.g
as the prob*. The brushes shall ba proparly sized and shaped co brush ouc :he
probe liner, cha probe nozzle, and cha iopingars.
3.5.4.2.2 Wash Botclas: Three wash bottles are required. Teflon or
glass wash boctles ara recooaendad; polyethylene wash bottles should not be
used because organic contaainants »ay ba extracted by exposure co organic
solvents used for saopla recovery.
3.5 4.2.3 CrAduaca Cylinder and/or Balance: A graduated cylinder or
balance is required co aaasura condensad wac*r co ch* nearest 1 ml or 1 g.
Graduated cylinders shall have division not >2 ml. Laboratory balances
capable of weighing to ±0.5 g are required.
3.5.4.2.4 Aober Class Storage Containers: One-liter wide-mouth
amber flint glass bottles with Teflon-lined, caps are required co score
impinger water samples. The beetles must be sealed with Teflon cape.
3-157
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3.5,4,2.5 Rubber Policeman and Funnel: A rubber policnaan and
funnel are raquirsd co aid in che cransfar of material Inco and ouc of
containers In che field.
3.5.4.3 Reagent Preparation
3.5.4.3,1 Bocclea/Capa: Amber 1- or 4-L bocclas with Teflon-Lined
cap* are required for scoring cleaned ONPH toluclon. Additional 4-L boccles
are required co collect waste organic solvents.
3,5.4.3,2 Large Glass Container: Ac laasc one large glass (9 co
16 L) is required for nixing che aqueous acidic DNPH solution,
3,5.4.3.3 Stir Place/Large Stir Bars/Stir Bar RecrLevar: a magnetic
scir place and lat|« sclr bar are required for th« miming of aqueous acidic
DNPH solution. A atlr bar retriever la needed for reaoving th« scir bar fron-r
che large container holding che DNPH solution.
3.5,4,3.4 Buchner Filter/Filter Flask/nicer Paper: A large fiUer
flask (2-4 L) with a buehner filter, appropriate rubber stopper, filter paper.
and connecting cubing arc required foe filtering che aqu*ou* acidic DNPH
solution prior co cleaning.
3.5.4,3.5 Separacory Funnel: AC least on* largo separacory funnel
(2 L) is required for cloaning Che DNPH prior co uio,
3.5.4.3 6 teakarc: Soakers (130 ml. 2SO ml, and 400 •!) aro useful
for holdlng/BJOMuring, organic liquid* whan clvaning che aquooua acidic ONPH
solution and for volghlng DNPH cryecals.
3.5.4.3.7 Punnals: AC leaae ona larga furmol la needed for pouring
cha aqueous acidic DNPH Inco the separator funnel.
3-158
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1.5.4.3.8 Graduated Cylinders; At Lease on* large graduated
cy'.L-der <1 Co 2 L) is required for measuring organic-free reagent water ar.d
acid when preparing the DN?H solution.
3.5-4.3.9 Top-Loading ialanct: A one-place cop loading balance is
needed foe weighing out the DNPH cryscali used ca prepare che aqutous aciiic
DN'PH solution.
3.5.4.3.10 Spatulas:. Spatulas ace needed for weighing ouc ONPH vher.
preparing the aqueous DNPH solution.
3,5.4,4 Crushed Ice: Quantities ranging froa 10-50 lb nay be
necessary during a sampling run, depending upon aablenc temperature. Samples
which have been taken oust be stored and shipped cold; sufficient ice for this
purpose oust be allowed.
35.5 ^§agents
3.5.5.1 Reagent grade chemicals shall b* used in all tests.
Unless otherwise indicated, it is intended that all reagents shall conform :s
ch* specifications of the Committee on Analytical Reagents of th« Aaerican
Chemical Society, where such specifications are available. Other grades nay
be used, providad It la first ascertained chat the reagent is of sufficiently
high purity ce perait its use without lessening the accuracy of the detersir.a-
clan.
3.5.5.2 Organic-free reagent water: All references to water ir.
:his method refer to organic-free reagent water, as defined in Chapter One.
3.5.5.3 Silica Gel; Silica gel snail be indicating type, 6-16
mesh. If the silica gel has been'used previously, dry at 173*C (350"F) for 2
hours before using, New silica gel nay be used as received. Alternatively,
other typea of d»siceants (equivalent or better) nay be used.
3-159
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3.5.5.i. 2,4-dinicrophenylhydraaina (DNPH), [2.4- (OjN)2CgHa;
The quantity of water nay vary from 10 Co 30%.
3.5.5.<*.l The 2,4-dinL=rophenylhydrazine reagent must be prepared •.-
:he Laboracory within five days of sampling us* in che field. Preparation of
DNPH can also be done in che field, vtch coniideracion of appropriate proce-
dures required for safe handling of solvent in che field. When a container of
prepared DNPH reagent is opened in che field, che concencs of the opened
container should be used within 48 hours. All laboratory glassware must be
washed with detergent and wacer and rinsed with wecer, mechanol, and oechyier.e
chloride prior co use.
NOTE; DNFH crystals or DNPH solucion should be handled vich plascic gloves
ac all does with proopc and extensive use of running water in case
of skin enposur*
3.3.3.4.2 Preparation of Aqueous Acidic DNPH Derivaclxing Reagent:
Each batch of DKPH reagent should be prepared and purified within five days of
sampling, according to the procedures described below.
NOTE: Reagent boccles for storage of cleaned DNPH derivaelzlng solucion
ousc be rinaed vlch aceconlerile and dried before use. Baked
glassware is noc essential for preparaclc- £ DNPH reagent. The
glassware auat not be rinsed with acec;-; .t an unaccepcable concen-
craclon of acetone concaatnaclon will be introduced. If field
proparaclon of DKPH is porforaed. caution ouat be exercised In
avoiding acetone contamination.
3.3.5.^.2.1 Place an 8 L container under a fuae hoed on a
magnetic stlrrer. Add a large stir bar and fill the container half full of
organic-free reagent vaeer. Save che eopcy beetle fro* che organic*free
reagent water. Stare che stirring bar and adjuat che stir race eg be aa face
as possible. Using a graduated cylinder, uasure 1.4 ml of concentrated
hydrochloric acid. Slowly pour the acid into the stirring water. Fuoes nay
be generated and che wacer may become warm. Weight che DNPH crystals on a
3-160
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one-place balance (see Table 3.5-L £or approximate amounts) and add ;o :;-.e
stirring acid solution. FLU =he 8-L container to the 8 • L. mark wish organic-
free reagent water and stir overnight. If all of the DNPH crystals have
dissolved overnight, add addi.ci.onal DNPH and stir for cwo acre hours,
Continue the process of adding DNPH with additional stirring until a saturated
solution has been formed. Filter the DNPH solution using vacuum filtration.
Gravity filtration may be used, but a ouch longer tine Is required. Store -'-a
filtered solution in an amber bottle ac room temperature.
3.5,5.4.2.2 Within five days of proposed use, place about 1,6 1
of the DNPH reagent in a 2-L saparatory funnel Add approximately 200 ml of
rcathyiene chlorida and 3copper the funnel. Vrap the stopper of the funnel
with paper towels to absorb any leakage. Invert and vent tha funnel. Then
shake vigorously foe 3 minutes. Initially, the funnel should.be vented
frequently (every 10 -15 sec). After che layers have separated, discard che'
lower (organic) layer.
3,5-5.4.2.3 Excraec tha DNPH a second time with nechylene
chloride and finally with cyclohexane. When the cyclohexane layer has
separated froo the DNPH reagent,the cyclohexane layer will be che cop layer i-
che separatory funnel. Drain che lower layer (the cleaned extract DNPH
reagent solution) into an amber bottle chac has been rinsed with aceconicri'.e
and allowed co dry.
3.5,5.it.3 Quality Control: Take cvo aliquots of che extracted DNPH
reagent. The size of the aliquocs is dependent upon che exact stapling
procedure vued, buc 100 •! is reasonably represencaclve. To ensure that the
background In Che reagent is acceptable for field use. Analyze on* aliquot of
che reagent eccording co che procedure of Method 8315. Save che ocher a 11quo:
of aquiouj acidic DNPH for uaa aa a aathod blank «han the analysis Is per-
formed.
3.3.5.4.4 Shipment co che Field: Tlghcly cap che bottle containing
extracted DNFH reagent usting a Teflon-lined ctp. Seal che beetle with Teflo-
3-161
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Table 3.5-1
APPROXMIATE AMOUNT OF CRYSTALLINE DNPH USED
TO PREPARE A SATURATED SOLUTION
Aoounc of Moiicure in DNPH
Weight Required per 8 L of Solution
10 weighc percent
15 weight percent
30 weight percent
31 8
33 g
S
40
Table 3.5-2
INSTRUMENT DETECTION LIMITS Aim REAGENT CAPACITY
FOR FORMALDEHYDE ANALYSIS1
AnaLyta
Oacacclon Limit, ppbv3 Reagent Capacity, ppmv
Formaldehyde
Acecaldahyde
Acrolein
Ace tone/Prop ionaldehyd*
Butyraldahyda
Methyl achyl kecenc
Valaraldahyda
I aovalar aldehyde
Hexaldehyd*
Banxaldahydfl
o Vn-/p-Tolu*ld*hyd«
Dim«thylb«n*ald«hyd«
1.8
1.7
1.5
1.5
1.3
1.5
1.5
1.4
1.3
1.4
1.3
1.2
66
70
73
75
79
79
84
84
88
84
89
93
L0xyganac«d coopound* in addition ce foraaldahyda *ra Included for
comparison with form*ldahyda; ancaniion of th« aachodology ce other compounds
Li ponibl*.
JDacaccion lialci art dacamlnad in to 1 vane. Than values charafora
rapraianc cha opcloua capability of cha methodology.
3-162
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cape. After che boccle is labeled, cha boccle nay be placed in a. friction-::;?
can (painc can or equivalent) containing a 1-2 inch layer of granulated
charcoal and scored ac ambienc temperature uncLl use.
3.5.3.i.-.L If che DNPH reagenc has passed che Qualicy Cor.:rol
criteria, che reagenc may be packaged co meec necessary shipping requirements
and senc co che sampling area. It che Quality Control criteria are r.o: 3e:r
che reagenc solution may be re-extracced or the solution may be re-prepared
and che excraccion sequence repeated.
3-5.5,4.4.2 If che DNFH raagenc is not used in che field within
five days of excraccion, an aliquoc may be taken and analyzed as described 1-
-lechod OOllA. If che reagenc meets the Quality Control requirements, che
reagenc may be used. If che reaganc does not oeec che Quality Control
requirements, che reagenc muse be discarded and new reagenc must be prepared
and cascad.
3.5 3 4.5 Calculation of Acceptable Concencracions of Inpuricies Lr.
DMPH Reagenc: The accepcable impurlcy concencraclon (AlC. wg/al) Is calc-la:
ed from che expected analyce concencracion In che saapled gas (EAC, ppbv). :he
volume of air chac will be saapled ac standard condition! (SVOL, L); che
formula weight of che analyce (FV, g/aol). and che volume of DNPH reagenc :!-,a:
will be used in che ImpInger§ (RVOL. ml):
AlC - 0.1 x [EAC x SVOL X FU/22.
-------
disposal purposes. 2,&-dini:roph«nylhydrazine is a flammable solid whan drv,
so -Jacer should not be evaporated from the solution of che reagent.
3.5.5-5 Field Spike Standard Preparation to prepare a formalde-
hyde field spiking scandard ac 4,01 ng/al, use • 500 ^1 syringe co transfer
0.5 ml co 37% by weight of formal shyde (401 mg/ml) co a 50 ml voluoecric
flask concaining approximately 50 ol of nechanol. Dilute co 50 ol with
mechanol.
3.5.5.6 Hydrochloric Acid, HCL; Reagenc grade hydrochloric acid
(approximacaly 12N) is required for acidifying che aqueous DNPH solucion.
3.5.3.7 Hechylene Chloride. CH2C1Z: MechyLene chloride (suitable
for residue and pesclcid* analysis, CC/HS, HPLC, CC, Speccrophocoaecry or
equivalent) Is required for cleaning che aqueous acidic DNPH solucion, rinsing
glassware, and recovery of saople erains,
3.5.5.8 Cyclohexane, C(HU: Cyclohexane (HPLC grade) is required
Cor cleaning che aqueous acidic DNPH solucion.
NOTE: Do not us* spectroanalyzed grades of cyclohexane if this sampling
methodology is extended co aldehydes and kecones vich four or oore
carbon aeons.
3.5.5.9 Mechanol. CH,OH: Nachanol (HPLC grade or equlvelenc) is
required for rinsing gluavare.
3.3.3.10 Aceconltrlle, CH,CN: \cetonltrile (HPLC grade or equiva-
lane) is required for rinsing glassware.
3.5.5.11 Formaldehyde, HCHO: Analytical grade or equivalent
formaldehyde is required for preparation of standards. If other aldehydes or
ketones are used, analytical grade or equivalent is required.
3-16-
-------
Sample CoILgc.ci.oP- Preservation. *r.4Handling
3.5.6-1 Because of the complexity of this nechoa, field personnel
should be :rained in and experienced with the case procedures in order ;a
obtain reliable results
3.5.6.2 Laboratory Pr«paracion;
3 5.6.2.L All che components shall be maintained and calibrated
according to che procedure described in APTD-0576, unless ochervise specified.
3,5.6.2.2 Weigh several 200 co 300 g portions of silica gel in
aircighc containers co che nearest 0.5 g. Record on each container che :ota'.
veighc of che lilica gel plus containers. As an alternative co preweighing
che silica gel, 1C may instead be weighed directly in che Lapingar or sampling
holder Juac prior co craln assembly.
3.5.6.3 Preliminary Field Decenninaclons:
3.5.6.3.1 Select che sampling site and che mlnlmua number of
sampling point according co EPA Method 1 or ocher relevant criteria. Deter-
mine che stack pressure, temperature, and range of velocity heads using EPA
Method 2. A leak-cheek of che plcoc linea according co EPA Method 2, Section
3.1, must be performed. Determine che stack gas no is cure concenc using EPA
Approximation Heched 4 or Let elcernacivas co eecabllah flscleacas of Isokine-
tic sampling-rate sectings. Determine che acack gas dry molecular weight, as
described in EPA Kechod 2, Section 3.6. If integrated EPA Method 3 sampling
is used for aelacular weighc determination, che incegraced beg sample shall be
taken simultaneously wich. and for the same cotal length of time as, the
sample run.
3.5.6.3.2 Select a nozzle size based on the range of velocity heads
so that is noc necessary co change che nozzle size In order co maintain
isokinecic sampling races below 28 L/nin (1.0 cfa). During che run, do no;
3-165
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change the nozzle. Ensure thac che proper differencial pressure gauge is
chosen for the range of velocicy heads encountered (see Section 2.2, of EPA
Method 2).
3.5- 6.3,3 Select a suicable probe Uner and probe length 10 chac All
iraversa points can be saapled. Tor large stacks, co reduce che lengch of the
probe, consider sampling from opposite sides of the stack,
3,5.6.3.4 A minimum of 45 ft1 of staple volune Ls required for -he
determination of Che Destruction and Removal Efficiency (DRE) of formaldehyde
from incineration systems (45 fcj is equivalent to one hour of sampling at
0,73 dscf). Additional sample volume shall be collected as necessitated by
the capacity of the ONFH reagent and analytical detection limit constraints.
To determine the minimum sample volume required, refer co sample calculations
in Section 10.
3.5-6.3.5 Determine the total lengch of sampling time needed to
obtain the identified minimum volume by comparing the anticipated average
sampling rate with the volume requirement. Allocate the SUM time co all
:raverse pointa defined by EPA Method 1. To avoid timekeeping errors, cha
length of time sampled ac each traverse point should be an integer or an
integer plus 0.5 min.
3.5.6.3.6 In aoaa circumstances (e.g., batch eyelet) it may be
necessary co sample for ahorter times at the traverse points and co obtain
smaller gas-volu** sample*. In these cases, careful documentation muse be
maintained la ordar to allov accurate calculation of concentration*.
3.5.6.4 Preparation of Collection Train:
3.5.6.4.1 During preparation and assembly of che sampling train,
keep all openings where contamination can occur covered with Teflon film or
aluminum foil until juac prior to assembly or until sampling is about to
begin.
3-166
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3,5.6.4,2 PLacf 100 ml of cleaned DNPH solution in each of :he :irs:
:vo Lapi.igers , .and Leave che :hird impinger empty. If additional capacity -.5
required for high expected concentrations of formaldehyde in the stack $as ,
200 si of DNPH per inpinger may be used or additional iapingers may be used
for soap ling. Transfer approximately 200 eo 300 g of pre-weighed silica jel
from its container :o che fourth impinger. Care should be taken ;o ensure
chac che silica gel is not entrained and carried out from the iapinger ^ur:.-,z
sampling. Place the silica gel container Ln a clean place or later use ir, :-e
saaple recovery. Alternatively, the weight of the silica gel plus impir.ger
may be determined co the nearest 0.3 g and recorded.
3.5.6.4.3 With a glass or quartz liner, install the selected r.oz=Le
using a VUon-A 0-ring with stack temperatures are <260'C (500'F) and a wover.
glass-fiber gasket when caaperacures are higher. See APTD-0576 (Rom, -572)
for details. Other connection systems utilizing either 316 stainless steel or
Teflon ferrules may be used. Hark the probe with heat-resistant cape or by
some other method to denote the proper distance into cha stack or duct" for"
each sampling point,
3.5.6.4.4 Assemble the train a* shown in Figure 3.5-1. During
assembly, do not use any silicane grease on ground-glass Joints upstream of
the impingers. Use Teflon cape. If required. A very light coating of
silicone grease may be used on ground-glass Joints downstream of che
impingers, but che silicone grease should be limited co che outer portion (see
APTD-0576) of che ground-glass Joints co minimize stlicone grease contamina-
tion. If necessary, Teflon cap* may be used co seal leaks. Connect ail
temperature sensors Co an appropriate pocenclomecer/display unic. Check al'.
temperature sensors ae ambient cemperatures.
3.5.6,4.3 Placa crushed lea all around che iapingers.
3.5.6 4 6 Turn on and sac che probe heating system ac che desired
operating temperature. Allow time for the temperature co stabilize.
3-167
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3.5.6.5 Leak-Check Procedural:
3,5.6.5,1 Pre-test Le«k Check
3.5.6.5.1.1 After che stapling train has been Assembled, :urn on
and sec the probe heating system at the desired operating temperature. Allow
= i.ne for :he temperature no stabilize. If a Vlcon-A o-rlng or och«r leak-free
connection La used Ln assembling Che probe nozzle to che probe liner, leak -
check :he :raln at che stapling lice by plugging che nozzle and pulling a 381
nun Hg (15 in Hg) vacuum.
N'QTE: A lower vacuua may be used, provided chat che lover vacuum Is noc
exceeded during cht test.
3,3.6,5,1.2 If an asbestos scrlng Is uaed, do noc connect che
probe co che train during che leak cheek. Irucead. leak-cheek the crain by
first aEcaching a carbon-filled laak check implngar co the tnlec and then
plugging che inlec and pulling a 381 ma Hg (IS in Hg) vacuua, (A lower vacuua
any be used if chii lover vacuua is noc exceeded during che ceic.) Naxc
eonnecc che probe Co che train and leak-check ac about 25 am Hg (1 in Hg)
vacuum, Alternatively, leak-check che probe with che resc of che stapling
=rain in one step ac 381 on Hg (1) in Hg) vacuua. Leakage race* in excess of
(a) <*\ of the average stapling race or (b) X).00057 «s/min (0.02 cfa), are
unacceptable,
\*
3.3.6.3.1.3 The following leak cheek instructions for che
sampling crain detected In ADFT-0576 and APTD-0381 may be helpful. Scare che
poop with che fina-adjuac valve fully open and coarse-valve completely closed
Partially open che coarse-adjuac valve and slowly close che fine-adjust valve
until the deaired vacuum If reached. Do Q0Jt reverie direction of the fine-
adjust valve, as liquid will back up into the crain. If Che deaired vacuum is
exceeded, either perform che leak check ac this higher vacuua or end the leak
3-168
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3. 5.6, 5. L. 4 When che Leak check is completed, first slowly reao-.-e
che plug froa the inlet to the probe. W*hen the vacuum drops to 127 ma (5 L-.'
Hj or less, immediately close che coarse -adjust valva. Switch off che puapir.g
system and reopen the fine-adjust valve. Do not reopen the fine-adjus; valve
ur.cil ;he coarse-adjust valve has been closed co prevent the liquid in :he
L.Tipingers from being forced backward in che sampling Line and silica gel frcs
being entrained backward into che third impingec.
\
3.5.6.5.2 Laak Checks During Sampling Run:
3,5.6,5.2.1 If, during the sampling run, a component change
(i.e.. iorplnger) becomes necessary, a leak check shall be conducted iaaediare-
ly after the interruption of sampling and before che change is oade. The leak
check shall be dan* according co cha procedure described In Section 3.5.6.5.1
excepc chac 1* shall ba done at a vacuum greater Chan or equal co the maximum
value recorded up co chae point in ch« teec. If che leakage cate is found to
ba no greacer Chan 0.00057 m'/nin (0.02 cfa or &% of cha average saopling rate
(whichever is less), cha re«ulcs are acceptable. If a higher leakage race is
obtained, cha caacar muse void che sampling run.
MOTE: Any correccion of the sample volume by calculation reduces the
integrity of che pollutant concentration data generated and oust be
avoidad.
3.5.6.S.2.2 Iimadlacely after a eonponenc change and before
sampling is reinitiated, a leak check similar co a pre-teet leak check muse
also ba conducted.
3.9.6.3.3 Post teat Leak Check:
3.5.6.3.3.1 A leak check is mandatory at cha conclusion of each
sampling run. The Leak cheek ahaLl ba dona with cha laaa proceduree at the
pre-caic leak check, excepc chat cha posc-teac laak check shall ba conducted
ac a vacuua greacer than or equal to cha maxinua value reached during the
saapling run. If cha leakage rate is found to ba no graacar than 0.00057
3-L69
-------
sVmin (0.02 cfm) or <.* of ch« average sampling eat* (whichever is less). :he
results are acceptable. If, however, a higher laakage race is obtained, the
:escer shall record the Leakage race and void th* sampling run.
3.5.6.6 Sampling Train Optracion:
3.5.6.6,1 During che sampling run, maintain an isoklnecic sampling
rate to within 101 o£ true isokinetic, below 20 L/ain (1.0 cfm). Maintain a
temperature around che probe of 120'C (24g» ± 25'F).
3.5.66.2 for each run, record the dac* on a daca sheet such ai che
one shown. In. Figure 1.5-2. &e sure Co c«cocd che initial dry -gam meter
reading, Rtcord che dry-gas meter reading* ac ehe beginning and end of each
sampling elm* tncremenc. when changes in flow races arc oad«, before and after
each leak theek, and whan laapLing 10 halcad. Taka oehar readings required by
Figure 2 ac Itasc onca ac each • ample poine during «ach C!BM irvcteoenc and
additional readings when significant adjusca«ncs 20% variation In velocity
head readings) necassicac* additional adjuacoancs in flev race, Laval and
zero che manomecer. Because che nanoaacer Level and zero nay drlfc due to
vibrations and tamperacure changes, oake periodic checks during che traverse
3.5,6.6.3 Clean che stack access pores prior Co che cest run to
eliminate che change of saapling deposited oaeerial. To begin sampling.
remove che notzle cap, verify chat che filter and probe heaclng systems are a.-.
the specified tenperacure, and verify chae che picoc cube and probe are
properly positioned. Position eh* nozzle ae the firsc traverse point, with
the tip pointing directly into the gas screaa. Immediately start che pump and
adjust che flow co isokineclc conditions, Monographs, which aid in che rapid
adjustment of the isokinetie saapling rate without excessive computations , are
available. These nomographs are designed for use when che Type S picoc tube
coefficient is 0,84 ± 0.02 and che stack gas equivalent dens ley (dry molecular
weight) Is equal co 29 + 4. AFTD-0976 details the procedure for using che
nomographs. If che stack gas molecular weight and the pltot tube coeff icier:
steps are caken co compensate for the deviations,
3-170
-------
I Ma
Cf
PUTi
AatbMM
AMumd MoMiM* X
. rn(ti}
Natxte OlwnM«, cm Qn|-
. an He 0n
fa* Mo.
Vrtoojy
'«.o
-fi
ACIOM
I«Oto«l
Jo
tMMMflQ
•cm
A«y Avtj
I-' i I'M I i 1 . 'l ' I' i I I il I).I I .1 Sin .'I
-------
3.5-6.6.4 U"hen the scack it under iLgni.fi.canc negative pressure
(equlvalenc Co che heighc of che impinger scam), cake car* co close che
coarse-adjusc valve before inserting che probe Lnco che scack In order ;o
prevent Liquid from backing up chrough che crain. If necessary, che puap say
be :urned on with che coarse•adjust valve closed.
3.5.6.6-5 When che probe is in postcion, block off che openings
around che probe and scack access pore co prevenc unrapresencaclve dtlucior. of
:he gas screaa.
3.5.6.6.6 Traverse che scack cross seccion, as required by EPA
Mechod I, being careful noc co bump che probe nozzle inco che scack walls when
sampling near che walls or when removing or inserting che probe chrough che
access pore, in order co ninimize che chance of excraccing deposiced material.
3.3.6.6.7 During che cesc run. oake periodic adjustments co keep che
temperature around eh« probe ac che proper lavala. Add sore ica and, if
necessary, sale, Co aaincain a cenperacure of <20'C (6S*F) ac che silica gel
ouclee. Also, periodically check che level and zero o£ che manometer.
3,5.6.6,8 A single crain shall be used for che encire sampling rur.,
except in cases where sLoultanaous saapling is required in cvo or more
separace ducca or ac evo or nore different locations wichin che sane duct, or
in cases where equipewnc failure necessicaces a change of crains. An addition-
al train or additional erains nay also be used for saapling when che capacicy
of a single ecain is exceeded.
e
3.9.6.6.9 When evo or aere crains are used, separace analyses of
coaponencs from each crain shall be performed. If aulciple crains have been
used because che capacity of a single crain would b« exceeded, firsc iapingers
from each crain aay be coabined, and second iaptngers froa each crain Bay be
combined.
3-172
-------
3.5.6.6.10 AC che end of che sampling run, cutn off :he coarse
acijusc valve, reoove qhe probe and nozzle from che scack, cum off she puap,
record :he final dry gas oecer reading, and conduce a pose-case leak check.
Also, leak check che picoc lines AS described in EPA Method 2. The lines
pass ;his leak check in order qo validaca che velocity-head data.
3.5.6.6.11 Calculate percent isokinericicy (see Mechod 2) to
determine whether che run wax valid or another case should be made,
3.5.7 Sample tUeoyfry
3.5.7.1 Preparation:
1.5.7.1.1 Proper cleanup procedure begins ** soon as che probe is
removed from the stack ac che end of che sampling period. Allow che probe co
cool. When che probe can be handled safaly. wipe off all external parciculace
matter near che dp of che probe nozzle and place a cap over che tip ca ~
prevent losing or gaining parciculace matter. Do nor cap che probe tip
tightly while che sampling craln Is cooling because a vacuum will be creazec
drawing liquid from che impingen back through che sampling craln,
3.5-7.1.2 Before moving che lampIIng crain co che cleanup sice,
remove che probe fronj cha laapUng craln and cap the open outlet, being
careful noc co lei* any condansaca chac aighc be present. Remove che umbili-
cal cord from che laac loplnger and cep che impinger. If a flexible line is
used, lee any condensed water or liquid drain Into che iaplngars. Cap off any
open impinger inlet* and ouclacs. Ground glaas scoppers, Teflon caps or caps
of ocher Inarc aacarials may ba used co seal all openings.
3,5,7,1.3 Transfer che probe and Impinger assembly co an area chac
Is clean and procaccad from wind so chac che chances of eoncaalnacing or
losing che sample ara minimized.
3.5.7.1.4 Inspect cha train before and during disassembly, and noce
any abnormal conditions.
3-173
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3.5-7.L,5 Save a portion of all washing solution (mechylene chlo-
ride, water) used for cleanup as a blank. Transfer 200 ml of each solution
directly from che wash boctle being used and place each In a separate,
^relabeled sample container,
3.5.7.2 Sample Containers:
3.5.7.2.1 Container I: Probe and Imp Inger Catches. Using a
graduated cylinder, measure to che nearest ml, and record the volume of ;he
solution in the first three impingers Alternatively, the solution may be
weighed to che nearest 0.5 g. Include any condensact in the probe in this
determination. Transfer the iopinger solution from che graduated cylinder
into the aaber flint glass boctle. Taking care chat dust on che outside of
the probe or other exterior surfaces does not get Into the saaple. clean all
surfaces to which the sample is exposed (Including the probe nozzle, probe
fitting, probe liner, first iaplnger, and iaplnger connector) with mechylene. „
chloride. Us* laas than 500 ml for che entire wash (230 ml would be better,
if possible). Add the washing ro the sample container.
3.5.7.2.1.1 Carefully remove che probe nozzle and rinse the
inside surface with nethylene chloride from a wash boccla. Brush with a
Teflon bristle brush, and rinse until the rinsa shows no visible particles or
yellow color, aftar which aaka a final rinja of the inaida surface. Brush and
rinsa tha insida parts of the Swagelok fitting with oachylena chlorida in a
similar way.
3.5.7.2.1.2 Rinse che probe liner with mathylena chlorid*. Uhlle
squirting eh* •a.thylena chloride into tha uppar and of cha probe, tile and
rotata tha proba so ehaC all insida surfaces will ba watted with mathylene
chlorida. Lac cha MChylana chlorida drain froa tha lower and Inco cha sample
container. Tha tester may use a funnel (glass or polyechylena) eo aid in
transferring tha liquid washes to the container, follow cha rinse with a
Teflon brush. Hold cha proba in an inclined position, and squire machylene
chioeida inco cha uppar and as cha proba brush is baing puahad with a twisting
action through cha proba. Hold che sample container underneath tha lower end
3-174
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of che probi, and cacch any aechylen* chloride, water, and paniculate aa::er
that is brushed Iron che proba- Run che brush through che probe three cLaes
or acre. 'Jlch scainlass steel or other aecal probes, run the brush through ;-
che abo^a prescribed Banner at lease six times since chare may be snail
crevices in which particulace aaccer can b* entrapped. Rinse Che brush v-;;h
mechylene chloride or wacer, and quantitatively collect these washing in ;'-e
sanpla container. After che brushing, make a final rinse of che probe as
described above.
NOTE: Two people should clean che probe in order to ninimize saapie
losses. Between sampling runs, brushei auac be kepe clean and free
from contamination.
3.5.7.2,1,3 Rinse che inside surface of each of the first three
inpingars (and connecting cubing) three separate rises. Use a inall portion
of nechylene chloride for each rinse, and brush each surface co which the
sample is exposed wich a Teflon bristle brush co ensure recovery of fine "
particulat* natter. Uecer will b* required for che recovery of che iiapir.gers
in addlcion co ch* specified quantity of methylane chloride. There will be a:
lease cuo phase* in che iorpingers This two-phase mixture does noc pour veil,
and a significant amounc of che impinger cacch will be left on che walls, The
use of wacer as a rlns* makes che recovery quantitative. Hake a final rinse
of each surface end of ch* brush, using both toechylene chloride and wacer.
3.5.7.2.L.4 Afcer all mechylene chloride and wacer washing and
particulate maccer haw been collected in the saaple container, tighten the
lid so ch* solvent, w*cer, and DNPH reagent will noc leak out when the
container Li shipped to th* laboratory. Mark th* height of the fluid level :o
determine whecher leakage occurs during transport. Seal ch* container wish
Teflon cap*. Label th* container clearly to identify ics concents.
3.5.7.2.I.5 If th* first cwo impingers at* to b* analyzed
separately to check Cor breakthrough, separate ch* concents and rinses of the
two impingers into individual containers. Care oust b* taken co avoid
physical carryover fro« th* first laplnger co che second. Th* foraaldehyde
3-175
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hydrazone is a solid which floats and froths on cop of the impingar solution.
Any physical carryover of collected moisture into che second impingar will
a breakthrough assessment.
3,5,7,2,2 Concainar 2: Sanpla Blank. Prapara a blank by using an
amber fiinc glass container and adding A voluaa of DNPH raaganc and nechylene
chloride equal co eha cocal voluaa In Concainar 1. Process cha blank in che
saae manner as Concainar 1.
3,3.7,2.3 Concainar 3: Silica Cal. Note cha color of che indicat-
ing silica gal to determine whether ic has been completely sptnc and make a.
notation of its condition. The iopinger containing tha silica gal nay be used
as a saapla transport container with both ends iaaled with cighcly fleeing
caps or plugs. Ground-glass stoppars or Teflon caps maybe ujad. Tha silica
gal iapinger should Chan ba Labalad. covered vlch aluminum fell, and packaged
on ica for transport co cha laboratory. If tha silica gal la removed froa ch*
implngar, tha cascar uy as a • funnal Co pour cha silica gal and a rubber
policeman co remove cha silica gal fro* cha impingar. Ic la noc necessary ~o
remova cha small aaounc of dust particles chac aay adhere co cha inplnger wall
and ara difficult co raoova. Sinca cha gain in waighc is co ba ujad for
moiscura calculations, do noc use water or othar liquid! co transfer cha
silica gal. If a balanca la available in cha fiald, cha spanc silica gal (or
s LI Lea gal plus inplngar) aayba weighed ce che naarasc 0.3 g.
3.S.7.2.& Saa^la concalnara should ba placed in a cooler, cooled by
(although noc in contact with) ice. Saaple containers auit ba placad verti-
cally and, sine* thay ara flajs, protected froa braakaga during shlpaanc.
Samples should b« coolad during shLpaanc mo they will ba received cold ac che
laboratory.
3-175
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3.5,8 Calibration
3,5,8,1 Probe Nozzle, Probe nozzles shall be calibrated before
-heir initial use in ctxa field. Using a micrometer, oeas-ura che ins ids
ciane-er of :ha nozzla co che nearest 0,025 too (0,001 in). Hake measurements
a: :hree separace places across cha diameter and obcain cha average of the
measurements. The difference bacueen cha high and low numbers shall no:
exceed 0.1 ma (0.004 Ln). whan che nozzles become nicked or corroded, ;hey
shall be replaced and Calibrated before use. Each nozzla ausc be pemaner.;!y
and uniquely idanclfied.
3.5-9,2 Pitot Tube: The Type S picot cube assembly shall be
caUbraced according co che procedure outlined Ln Secclon 4 of EPA Method 2.
or assigned a nominal coefficient of 0.94 if Lc Ls noc visibly nicked or
corroded and if ic oeecs design and incerconponent spacing specificaclons.
3.5.8.3 Metering System
3.5.8.3.1 Before its initial use Ln cha field, che metering syscen
shall be calibrated according co che procedure outlined in APTD-Q576. Insraac
of physically adJuseing che dry-gas macar dial readings co correspond co the
wac-cesc ma car readings, calibration faccors may be used co correct che gas
meter dial reading! aacheaaclcally to the proper valuea. Before calibrating
:he mecering lyscaa, Lc ia suggested that a leak check be conducted. For
metering sysceu having diaphraga puaps, the neraal leak check procedure will
noc detect leakages wlch th« punp. Far these cases, the following leak check
procedure will apply: aaka • can-islnuce calibration run ac 0.00057 a'/ain
(0.02 cfa). Ac the end of che run. take the difference of the oeaaured wat-
:esc and dry*g«J o«cer volunes and divide che difference by 10 to gee che leak
race. The leak cat* should nee exceed 0.00097 n'/Bin (0.02 cfa),
3.5.8.3.2 Afc«c «*ch field use, check the calibration of the
me coring syscaa by performing three calibration run* ac • single intermediate
orifice setting (based on che previous field east). See the vacuua at cha
raaximua value reached during the case series. To adjuac che vacuua, insert a
3-177
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valve between tha wec-tast meter and "he inlec of cha metering system,
Calculate the average value of the calibration factor. If che calibration has
changed by more che 5%, recalibrate che nicer over che full range of orifice
settings, as outlined in APTD-0576.
3.5.8-3.3 Leak check of metering system: The portion of the
sampling train from the pump Co che orifice tneter (see Figure i) should be
leak checked prior co initial use and afcer each shipment. Leakage after :he
pump will result In Lets volume being recorded than ii actually sampled. Use
:he following procedure: Close the oaln valve on che meter box. Insert a
one-hole rubber stopper with rubber cubing attached Into cha orifice exhaus:
pipe. Disconnect and "enc che low side of the orifice manometer. Close off
;he low side orifice cap. Pressurize che system Co 13 • 18 ca (5 • 7 in)
water column by blowing Into the rubber Cubing. Pinch off cha cubing and
observe che nanometer for 1 mln. A loss of pressure on che manometer indi-
cates a leak In the actor box. Laaks muse be corrected.
NOTE.; If che dry-gaa-«ecer coefficient values obtained before and after a
test series differ by >3«, either the test series must be voided or
calculation! for test series nut be performed using whichever oacer
coefficient value (i.e., before or after) gives che lower value of
cocal sample volume.
3.5.8.4 Prob* Heater: The probe heating syacea oiut be calibrated
before its initial use in the field according to the procedure outlined in
APTD-0576. Probes constructed according to APTO-0381 need net be calibrated
if che calibration curvet• in APTD-0576 art used.
3.9.8.3 Te«p«rature gauges: Each thermocouple must be permanently
and uniquely marked on cha casting. All Mtcury-in-flaas reference chermoae-
ters oust conform co ASTH E-l 63C or 63F spec ii;'cat ions. Thermocouples should
be calibrated in the laboratory with and without the use of extension leads.
If extension leade »rm ug«4 fn rho field, che charsecsupls rsidlr.;: £= :hs
aobienc air temperatures, with an; without che extension lead, must be noted
3-178
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and recorded. Corraccion is necessary if =he use of an extension Lead
produces a change >L.5».
3.5, 8.5,1 Impinger and dry-gas meter thermocouples: For che
thermocouples used co measure che temperature of che gas Leaving che impir.ger
crain. chree-poirvc calibracLon ac ice water, room air, and boiling .'a:er
temperatures is necessary. Accept the chermocoupl.es only if rhe readings a:
all three temperatures agree co ±2C (3.6*F) with those of the absolute va'._e
of che reference chermometer.
3.53-5-2 Probe and stack thermocouple: for che thermocouples use-
co indicate che probe and stack camperacures, a chree-poLnc calibracion a: .:-.
wacar. boiling water, and hoc oil bach camperacurei tausc b« performed. Use :;
a poinc AC room air temperature is recommended. The thermometer and thermo-
couple muse agree co within 1.5% AC each of che calibration points. A
calibration curve (equation) may be constructed (calculated) and che daca
extrapolated co cover che entire cemperacure range suggested by the manufac^
curer.
3.5.9.6 Barometer: Adjust che barometer initially and before eacr
cast series co agree co within ±2.5 ma Hg (O.I in Hg) of che mercury baro.ieze:
or che correct baromecric pressure value reported by • nearby National -«a:r.r.-
Service Scacion (saae altitude above sea level),
3.5.3.7 Trlple
-------
3.3-9,1 Calculation of Total. Formaldehyde: To deearmlne che :oca!
formaldehyde t>n m&, u" th« following equation:
[g/mole aldehyde |
Total mg formaldehyde - Cd x 7 x DF x ___^ ___ ^_^ ___ x LOJ mg/wg
(g/moie DNPH
where;
C4 - measured concentration of DNPH • formaldehyde derivative, wg/ai
V - organic excracc volume ml
DF - dLluclon factor
3.5.9.2 Formaldehyde concentration in stack gas:
Determine the formaldehyde concentration in the stack gas using :he
following equation:
Ct - K [total formaldehyde, eg] V-UU)
where;
K - 33.31 ft1/*1 if '.<.u) i* expressed in English units
- 1.00 m'/B1 if V«uui li "Pressed in metric units
7a(lM, - volume of gas sample a measured by dry gas mecer,
corrected to standard conditions, deem (dscf)
3.3.9.3 Average Dry Gas Hater Temperature and Average Orifice
Pressure Drop are obtained from the data sheet.
3.3.9.4 Dry Gaa Volume): Calculate V.<,n) and adjust for leakage,
if necessary, vising the aquation in Section 6.3 of EPA Method 3.
3.3.9.3 Volusw of Water Vapor and Moisture Content. Calculate che
volume of water vapor and moiscure content from equations 5-2 and 3-3 of EPA
Method 5.
3 . 5 ,10 Decimil;
To determine the minimum sample volume to be collected, use the following
sequence of equations.
3-180
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3.5.10.1 From prior analysis of cha waste feed, cha concentration
of formaldehyde (FORM) introduced Lnco cha combustion syscen can b« calculat
ed. The degree of destruction and removal efficiency chat is required is
-o ie:eroiin« the amounc of FORM allowed Co be present in che effluen:. Thi
r.c say be expressed a*
FORM Mass - [ (VF) (FORK cone) (100 • 1DRE) j /100
where :
-F - mass flow race of waste feed per h, g/h (Ib/h)
FORM - concencraclon of FORM (we I) Introduced into ihe
combustion process
ORE - percanc Destruction and Removal Efficiency required
Max FORM - mass flow raca (g/h [lb/]) of FORM aaicced froo :r.e
combust ion sources
3.5,10.2 The average discharge concentration of cha FORM in che
effluent gas is determined by comparing the Max FORM with the volumetric fl^w
race being exhausted froo the source. Voluaatric flow race data are available
as a rasulc of preliminary EPA Method 1 - 4 determinations:
Max FORK cone - [Max FORM Mass] / DV,(t(,U)
where:
DT*ftntd) - volumetric flow raca of exhaust gas, dscm (dscf)
FORM cone - anticipated concentration of cha FORM in the
exhaust gas strau, g/dscm (Ib/dscf)
3,3.10.3 In aakini this calculation, in is reco«B«ndad that a
safety oargin of ae lease ten be Included.
[10LRM x 10 / FORM cone] - V^
where:
detectable amount of FORM in anclce sup I Ing train
oilniauB dry standard voluae to be collected at dry-
gas oe ear
3-181
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3.5.10.^ The following analytical detection UnUs *nd DNPH Reajer.:
Capacity (based °n a total volume of 200 ml in cwo implngers) must also be
considered in determining a volume to be sampled.
3.5.11 Quality C_o_ntrp_l
3.5-11.1 Stapling: Sec EPA Manual 600/fc-77-Q2b for Method 5
quality control.
3,3.11.2 Analysis: The quality assurance program required for :his
me chad includes che analysis of che field *nd aechod blanks, procedure
validations, and analysis of field spikes. The assessment of combustion daca
and positive identification and quantisation of formaldehyde arc dependent on
the integrity of che samples received and che precision and accuracy of the
analytical methodology. Quality assurance procedures for this aechod are
designed eo aonicor the performance of the analytical methodology and to .
provide the required information Co take corrective action if problem are
observed In laboratory operations or in field ssapling activities.
3-5.11.2,1 Field Blanks: Field blanks must be submitted uich
the samples collected at each sampling sice. The field blanks include the
sample bottles containing allquocs of sample recovery solvents, nethylene
chloride and water, and unused DNPH reagenc. At a oinimua, one complete
sampling train will be assembled in the field staging area, taken co the
sampling are. and leak-checked AC che beginning and end of che testing (or for
the tame total nuaber of clMi MM che accu«l •••plinf train). The probe of
the blank train sjuic be heated during che saaple teat. The train will be
recovered oj If it were an actual test saaple. No geseouj saaple will be
passed through eh* blank soapLing train.
3.3.11.2.2 Method Blank*: A. OMChod blank onuc be prepared for
each set of analytical operations, to evaluate contamination and artifacts
that can be derived from glassware, reagents, and saaple handling in the
laboratory.
3-182
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3.5-11.2.3 Field Spike: A field spike is performed by ir.;:3iuc.
ing 200 uL of *^e Field Spike Standard inco an iapinger containing 200 sii 3f
DN'PH solution. Standard inipinjer recovery procedures are followed and the
spike is used as a check on field handling and recovery procedures, An
aliquot of tha field spike standard Is retained in the labora:ory for deriva-
uizacion and comparative analysis.
3,5.12 Kacjnod Performance
3 5.12.1 Mechod performance evaluation: The expecced method
performance parameters for precision, accuracy, and detection limits are
provided in Table 3.5-3.
Addition of a Filter to the Formaldehyde Sampling Train
As a check on tha survival of particulate material through cha impinger
system, a filter can be added co the impinger train alchar after the second^
impinger or after tha third impinger Since cha impingars are in an ice bath
chore is no reason co haae cha fileer ae this poinc.
Any suitable medium (e.g., paper, organic membrane) may ba uaad for the f-..:er
if the material conforms co cha following specifications:
I) cha filter has at lease 931 collection efficiency (<3% penetration:
far 3 wffl dloceyl phchalaca smoke particles, Tha filcar efficiency
cost shall ba conducted In accordance with ASTM standard aachod
02986-71. Tasc dac* from cha supplier's quality control program are
sufficient for, chl• purpose.
2) tha filter has a low aldehyde blank value «0.013 mg formaldeh-
yde/cm1 of filter area). Before cha test series, determine the
average formaldehyde blank value of aC lease chraa filters (from :he
lot to ba used for sampling) using tha applicable analytical
procedures.
3-183
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Table 3.5-3
EXPECTED METHOD PERFORMANCE FOR FORMALDEHYDE
Para»«c«r Precision1 Accuracy2 Dataction Liaic1
Matrix: Dual craini ilSt RPD ±201 L.5 x. 10*' lb/£=3
(1.8 ppbv)
p*re*nc dlff*r*ne* Hale'for dual crain*.
2Liolc Cor fi*Ld split* r«cov«rl«i.
}Th« low»r rtporting limit having !«»• than It probability of falsa pesitiva
daciccion.
3-L84
-------
Recover ch« exposed filter into a saparaea ci«an container and return -_r-.e
concaintr .over Lc« co che laboratory for analysts, If ch« filcer U btLr.»
analyzed for foraaldihyde, che fLLcer nay be r*covtred inco a concainir or
DN'PH reagenc for shlpaenc back co ;h« laboracory. If ch* filctr is baing
examined for tha preienc* of particulace rsattrlai, thfl filcer nay be r
inco a clean dry eoncalnar and recurned co che Laboracory.
3-185
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3 >6 ftnalvsis for ftldahvdes fnd Kaeonaj fry High Performance
(HPLC) I'M* -hod OQI1
3,6.1 SS9P* and AppLteacLen
3.6,1-1 Method OOllA covers the determination of free fowaldehvde
in che aqueous samples and leachacas and derived aldahydei/ketones collected
by Method 0011.
Compound Name CAS No,*
Formaldehyde 50-00-0
Acetaldahyde 75-07-0
• Chemical Abscrect Service! Registry Nuab*r
3.6.1.2 Heehed CQllA La a high parfonunce liquid chroaacographi;
(HPLC) mechod opciraized for che dacarmlnaclon of formaldehyde and acecaldehyce
in aqueous «rwt,rorjn«ncal macttces and leachacei of solid saaples and acack
samples collected by Mechod 0011. When this aechod Li used co analyze
unfaailiar sample macrLces, compound Idencif icacLon should be supported by a:
lease one addi'Lonal qualitative cechnique A gas chroaacograph/oass spec-
:rofflecer (CC/MS) nay be uied for Che qualltaclv* confiraaeton of results fror
:he target analytes, uaing Che excracc produced by this aethod.
3.6.1. J Th« MChod detection liaics (HDL) are Lilted in Tables
3.6-1 and 3.6-2. The HDL for a specific sample may differ from chat listed,
depending upon the nature of interference! in che sample natrlx and the aaour:
of saaple used in che procedure.
3.6.1.& the extraction procedure for solid samples is siailar :o
chac specified Ln Method 1311 (1). Thus, a single saaple nay be extracted to
measure che analytas included in che scope o£ ocher appcopfkaE* aachuuf. The
analyst Is allowed che flexibility to select chroaatographic conditions
3-196
-------
Table 3.6-1
HIGH PERFORMANCE LIQUID CHROHATOGRAPHY CONDITION'S
AND METHOD DETECTION LIMITS L'SINC SOLID
SORBENT EXTRACTION
Analyse Rectncion TLm«
(ainue«i)
Fonnaldshyda 7 ,1
HPLC conditions: R«ven« pha«« C13 column, <*, 6 x 250 ma; Uocraeic elu;ia:
using BiCh«nol/w*Cir ('5:25, v/v); flo« c*c« 1.0 mL/oin. : d«ceecor 360 r.-s,
* After correction for laboracory blank.
Table 3.6-2
HIGH PERFORMANCE LIQUID CHROHAtOCRAfHY COKDITIONS
AND METHOD DETECTION LIMITS USING METXYL1.VE
CHLORIDE EXTRACTION
Analyca Rac«ncion TioM
(mlmicai)
Fonuldahyd* 7.1
Acacaldanyd* 8.6
HDL
(Mg/D*
7.2
171*
HPLC condLcLons: R«v«rit phA«« CIS eoluon. 4.6 x 230 oa; Lseeracic «lu;ion
using a«ch«noL/VAC«r (75:23, v/v); flow r«c« 1.0 aL/«in. ; daciccor 360 no.
Lneluda rctgcnc blank concancraclona of approxlmactly 13 ug/"_
formaldahyd* and 130 w£/L acaealdahyda.
3-187
-------
appropriate for che simultaneous measurement of contaminations of :hes* ar.alv
res
3.6.1.5 This method is restricted co use by, or under che supervi-
sion of analyses experienced in che use of chfomatography and in che incarprt-
zacion of chronacograas. Each analyse oust d*«onscrace ch* ability co
generate acceptable results with chls o«chod.
3.1.1.6 Th* coxLcicy or carcinegenlcity of each raagenc usad in
:his nachod has rvoc b««n practsaly daflnad; hov*v«r. «ach chamical compound
should b« created as a pocencial htalch hazard. From chis vlawpoinc, exposure
:o :hese chemicals nuic be reduced co cht lowest possible Laval by whatever
T.eans available. The labocacory is responsible for maintaining a current
awareness file of OS HA regulations regarding ch« safe handling of che chemi-
cals specified in chis MChod. A reference file of aacerial safecy daca
sheets should also b« ttad* available Co all personnel involved in che chemical
analysis. Additional references co laboratory safety are available,
3.6.1.7 Foruldehyda ha* been tentatively classified as a knour. or
suspected, human or oajmalian carcinogen.
3.6.2 Suamarv of Mechad
3.6.2.1 Envlrenaencal Liquid! and Solid Leachaces
3.6.2.1.1 For waatea coaprlaed of soIIda or for aquaoua wastes
concaining significant aaeunts of solid material, eh* aqueous phase, if any.
is separated frost v jjlid phase and stored for later analysis. If neces-
sary, che particle also of che solid* in che waste is reduced. The solid
phase is extracted with an aoount of extraction fluid equal to 20 ciaes che
weight of ch* solid phase of the vases. A special extractor vessel is used
when cesting for volatile*. Following extraction, the aqueous extract is
separated from the solid phase by filtration employing 0.6 to 0.8 Mm glass
fiber filter*.
3-L88
-------
3.6,2,1,2 If coapacLble (i.e., multiple phases will noC fora on
combination). Che initial aqueous phase of che waste is added co cha aqueous
«x;rac=, and chose Liquids are analyzed cogecher. If incompatible, ;he
liquids are analyzed separately and cha results are machemacicalLy combir.ed -
_';iie_Id_a "o'luae 'JeLghced average concentration.
3,6.2,1.3 A measured volume of aqueous staple or an appropriate
amount of solids leachata is buffered co pH 5 and derivaclzed wi;h 2.--
diruurophenylhydrazine (DNPH), using either che solid sorbenc or che nechyiere
derivacizacion/axcracclon opcion. If che solid sorbenc option is used, the
derivative is extracted using solid sorbenc cartridge*, followed by elucior.
-irh echanol. If :he methylene chloride opcion is used, the derivacive is
extracted wtch methylene chloride. The me thylane chloride extracts are
concentrated using che Kuderna-Danish (K-D) procedure and solvent exchanged
into oethanol prior co HPLC analysis. Liquid chromatographic conditions are
described which permit the separation and measuremenc of formaldehyde in che
extract by absorbance detection ac 360 run. , ..^
3.6.2.2 Scack Cas Samples Collected by Method 0011
3.6.2,2.1 The entire saaple returned to the laboratory is excrac:ed
wich mechylene chloride and cha methylene chloride extract is brought up co a
known voluoa. An aliquot, of cha m«chylene chlorld* excract is solvent
exchanged and concentrated or diluted as necessary,
3.6,2.2.2 Liquid chromatographie eondlclona are described that
permit che separation and Matureoanc of formaldehyde in the extract by
absorbance detection ac 360 nn.
3.6.3 Ineerferencee
3.6,3.1 Method Interferences may be caused by contaminanti in
solvents, reagenes. glassware, and other saople processing hardware that lead
:o discrete artifacts and/or elevated baselines in cha chrosutograos. All of
3-189
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aaeerials muse be routinely demonstrated co be free froa interferences
under the condition* of che analysis by analyzing laboratory reagent blanks.
3.6,3.1,1 Glassware nust be scrupulously cleaned. Clean all
glassware as soon as possible after use by.rinsing with che last solvent used
This should be followed by detergent washing with hoc water, and rinses vi:h
:ap water and distilled water. It should then be drained, dried, and heated
in a laboratory oven at 130'C for several hours before use. Solvent rinses
with nathanol nay be substituted for the oven heating. After drying and
cooling, glassware should be stored in a clean environment Co prevent any
accumulation of dust or other contaminants.
3,6.3,1.2 The use of high purity reagencs and solvents helps to
minimize interference problem*. Purification of solvents by distillation in
all-glass systems may b« required.
3.6.3,2 Analysis far formaldehyde Is especially complicated by its
ubiquitous occurrence In che environment.
3.6.3.3 Matrix Interferences nay be caused by contaminants chac
are coextraeted from the sample. The extent of matrix ineerferences will vary
considerably froa source co source, depending upon che nature and diversity of
che matrix being sampled. No interferences have been observed in the matrices
studied ae a result of using solid sorbene extraction u opposed Co liquid
extraction. If interferences occur in subsequent samples, some additional
cleanup may be necessary.
3.6,3.4 The extent of interference* that may be encountered using
liquid chroejaeographlc techniques has not been fully assessed. Although the
HPLC conditions described allow for • resolution of the specific compounds
covered by this method, other oacrlx components may Interfere.
3.6.4 Aooaracxia and Materials
3.6.4.1 Reaction vessel - 250 ml Florence flask.
3-190
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3.6,6.2 Separatory funnel - 205 aL. vi:h Teflon stopcock
3.6,4.3 Kuderna-Danish (K-D) apparatus.
3.6,6i.3.1 Concentrator cube - 10 ml graduated (Konces K- 570050-102:
or equivalent). A ground glass stopper is used to prevent evaporation of
ex:rae;s.
3.6.4.3.2 Evaporation flask • 500 ol (Koneei K-570001 • 5QP or
equivalent). Accach co concentrator tube with springs, clamps or equivalent
3,6.^.3,3 Snyder column - Three ball nacro (Konces K-503000-012'. =:
equivalent).
3,6.4,3.4 Snyder column - TWO ball macro (Koncas K-56900L-0219 or
equivalent)-
3.6.4.3.5 Springs - 1/2 inch (Kontes K-662750 or equivalent).
3.6.4.4 VlalJ • 10, 25 ml, glass with Teflon lined screw caps or
crimp cops.
3.6.4.5 Boiling chips • Solvent extracted with methylene cKloritte
approximately 10/40 oesh (silicon carbide or equivalent).
3.6.4.6 Balance • Analytical, capable of accurately weighing to
:he nearest 0.0001 g.
3.6.4.7 pH oecer • Capable of measuring ca the nearest 0.01 uni:s
3.6.4.8 High perfomunce liquid chromacograph (nodular)
3.6.4.8.1 Puvpinc syscea • Isocratic, vlch conatanc flow control
capable of 1.00 al/aln.
3.6.4.8.2 High pressure injection valve vlch 20 j*L loop.
3.6,4.8.3 Coluon • 250 mm x 4,6 m ID, 5 na particle size, C18 (or
equivalent).
3,6.4.8.4 Abierbanc* dececcor • 360 na.
3-191
-------
1,6.4,8.5 Strip-chars recorder compatible with dececcor • Use o: a
data system for measuring p«ak areas and recencion times Ls reconuaended
3.6,4.9 Glass fiber filter paper.
3.6,4.10 Solid sorbenc cartridges • Packed vLch 500 og CLB Oaker
or equivalent).
3.6.4.11 Vacuum manifold • Capable of simultaneous extraction, a: •_;
to 12 samples (Supelco or equivalent) .
3, 6, ^. 12 Sample reservoirs - 60 ml capacicy (Supelco or equiva-
lent) .
j
3.6,4.13 Pipec - Capable of accurately delivering 0-10 ml solution
(Plpetnan or equivalent).
3.6.4.14 tfacer bach • Heaced, wtch concentric ring cover, capable
of temperature control ((±) 2'C). The bath should be ujed under a hood,
3.6.4.15 Volumetric Flasks • 250 or 500 al.
3.6,5
3.6.5.1 Ree.fent grade chemtcala shall be used In all tests
Unlen otherwise Indicated, Lc is intended ehac all reagents shall conform to
the specification* of the Conic tee on Analytical Reagents of the Aaerlcan
Chemical Society, where euch specifications) are available. Other grades nay
bo used, provided it la fine ascertained that the reagent ia of sufficiently
high purity to perait ita uce without lessening the accuracy of the determina-
tion.
36.5.2 Organic -free water • All references to water in this
method refer to organic -free reagent water, as defined in Chapter I SV-846.
3-192
-------
3.6.5,3 Mechylene chloride. CHjClj • HPLC grade or equivalent
3.6.5.4 Methanol, CH5OH - HPLC grade or equivalent
3.6.5.5 EchanoL (absolute) , CHjCH2OH - HPLC grade or equivalent.
3.6.5.6 2.4-Dinicrophenylhydrazine (DNPH) (701 fJ/V)), '2,--
in organic- Eree r«aganc water.
3.6.5.7 Formalin (37.6 percent (w/w)), fornaldehyde in organic-
free reagent wacer.
3.6.5.3 Acetic acid (glacial), CH3C02H.
3.6,5.9 SodLua hydroxide solutions NaOH, 1.0 N and 5 N.
3.6,5.10 Sodiua chloride. NaCl. . ^
3,6.5.11 Sodium sulfice solucion, Na,SOJr 0.1 H.
3.6.5.12 Hydrochloric Acid, HCl. 0.1 N.
3.6.3.13 Extraction fluid - Dlluci 64.3 ml of 1.0 N NaOH and 5.7 •:
glacial acecic acid to 900 al with organic -free reagent water. Dilute co 1
licer wich organic -fre« reagent water. The pH should be 4.93 ± 0.02.
3.6,3.14 Stock standard tolutiona
3.6.3.14,1 Stock formaldehyde (approximately 1.00 ag/al) • Prepare
by diluting 263 itl fonalln to 100 al with organic -fraa reagent water,
3.6.5.14.1.1 Standardization of formaldehyde stock solution •
Transfer a 25 oL aliquot of a 0.1 M NajSO, solution to a beaker and record ;h
pH. Add a 25.0 ml aliquot of the fornaldehyda stock solution (Section
3.6.3.14.1) and record tha pH. Tltrace this aUture back to the original pH
3-193
-------
using 0.1 N HC1. The formaldehyde concentration is calculated using the
fallowing equation:
Concentration (mg/ml) - 30.03 x (N HCl) x (al HC1) 23,0
where :
S HCl - Normality of HCl solution used
ml HCl - ml of standardized HCl solution ui«d
30 03 - KV of formaldehyde
3.6.5.14.2 Stock formaldehyde and acecaldehyde - Prepare by adding
265 nL formalin and 0.1 g acecaldehyda to 90 ml of water and dlluce to 100 ml
The concentration of acecaldehyde in this solution is 1.00 og/ml. Calculate
the concentration of formaldehyde in this solution using the results of -he
assay performed In Section 3.6.5.14.1.1.
3.6.5.16.3 Stock standard solution* must be replaced after six
months, or sooner. If coeparlion with check standards indicates a problon.
3.6.5.15 Reaction Solutions
3.6.5.15.1 DNPH (1.00 ug/U • Dissolve U2.9 ng of 70% (w/v) reagen:
in 100 ml absolute ethanol. Slight heating or sonicatlon nay be necessary to
effect dissolution.
3.6,5.15.2 Ac«uta buffer (5 N) Prepar* by neutralizing glacial
acetic acid to pH 5 with 3 H NaOH solution. Dtlut* to standard volume with
3.6.5.13.1 Sodiua chloride solution (saturated) Prepare by mixing
of che reagent grada solid with water.
3.6,6 Saanla CoIleeelQn. Preservation, and Handling
3.6.6.1 See the introductory material to this Chapter, Organic
Analyses, Section 4.1 of SU-846.
3-194
-------
3.6.6.2 Environmental liquid and laachata samples ousc b« re friz-
eraced ac VC, and must be derivatized wlchin 5 days of sample collection ar.d
ar.alyzed wiehln 3 days of derivatizacion.
3.6.6.3 Stack gas samples collected by Machod 0011 muse be
refrigerated ac ^*C. Ic is recommended chat samples be extracted wUhin 30
days of collection and chat excracts b* analyzad within 30 days excrac-lcm.
3.6.7 Procedure
3,6.7.1 Extraction of Solid Saaplea
3.6,7,1.1 All solid samples should be homogeneous, «*hen che sample
is noc dry. decermina the dry weight of the aaapU, using a representative
aliquot.
3.6.7.1.1.1 Decerainacion of dry weight • In certain cases,
results are desired based on a dry weight basis. When such data Is desired,
or required, a portion of sample for dry veighc determination should be
weighed out at the Sam* tine as che portion used for analytical detaraina:i
•ARNINC: The drying oven should be contained in a hood or vented. Signifi-
cant laboratory contaatoation may result froa drying a heavily
contaainated haiardous waste i ample.
3.6.7,1.1,2 Is»edlately after weighing the saople for extraction,
weigh 5-10 | of the saaple Into a tared crucible. Determine the I dry weight
of che saarple by drying overnight at lOS'C. Allow to cool in a desiccator
before weighing:
t dry weight - | of drv aample x 100
g of saaple
3.6.7.1.2 Measure 23 g of solid into a 300 al bottle vleh a Teflon
lined screw cap or crlop top, and add SOO ml af extraction fluid (Section
3.6,5.13). Extract the solid by rotating the bottle at approximately 30 rpn
3-195
-------
for 18 hours- Filter che excract :hcough glass fiber paper and scare in
sealed bottles ac ^*C, Each ml of extract represents 0.050 g solid,
3,6.7.2 Cleanup and Separation
3.6.7.2.1 Cleanup procedures may noc be necessary for a relatively
clean sample matrix. The cleanup procedures recommended In this method have
been used for the analysis of various sample types. If particular circua-
scances demand che use of an alternative cleanup procedure, che analys; r.us:
daceraine che elucion profile and demonstrate ehac che recovery of formalde-
hyde is no leas chen 85» of recoveries specified in Table 3.6-3. Recovery .7a-
be lower for samples which form emulsions,
3.6.7.2.2 If che staple is noc clean, or che complexity is unknown,
che encire iample should be ctncrifuged ac 2500 rpo for 10 minutes. Decanc
che supernacanc liquid froa the centrifuge botcle, and filter through glass
fiber filter paper inco « container which can be tightly sealed.
3.6.7.3 Derivacizacion
3.6.7.3.1 For aqueous samples, measure: a SO co 100 ml aliquot of :r.
sanple. Quantitatively transfer the sample aliquoc co the reaction vessel
(Section 3.6.4.L).
3.6,7.3.2 For solid saoples, I co 10 oil of leachace (Section
3.6.7.1} will usually b« required. The aaoxinc used for a particular sample
•use be determined through preliminary experiaentf.
3-196
-------
Table 3.6-1
SINCU QPERATQH ACCllACY AND FIECISIQH
US ISC SOLID SORILVT EXTRACTION
Analyse
"ormald«hyd«
Matrix
Type
Reegene
'••car
Final
Effluene
Phenol
formaldahydi
Sludg.
Average
Ptrcinc
R«cov«ry
86
90
I
93
Standard SpU« Su^bir
D«vtaclon Range of
?treene (af/L) Ar.aL-.-sts •
9.4 IS-L<»30 ;5
'.1,0 46.S-L4JO Li
U-'O 457-1430 15 ;
-------
S'oce: For all reactions, che coe*l volume of che aqueous Layer should be
adjusted co 100 ml wi:h water.
3.6.7.3.3 Derlvacizacion and axcraccLon of che derivative can be
accomplished using cha solid sorbent (Saccion 3.6,7.3.4) or methylane chloride
option (Section 3.6.7.3.5).
3.6.7.3,4 Solid Sorbenc Opclon
3.6.7.3.4.1 Add 4 ml of acecata buffar and adjust che pH co 5.0 -
0.1 wich glacial aceclc acid or 5 N NiJH. Add 6 al of DNPH reagent, seal che
container, and place on a wrist-accion shaker for 30 minutes
3.6.7,3.4.2 Assemble cha vtcuua manifold *nd connect to a water
aspirator or vacuum puap Aasenbl* solid sorbant cartridges containing a
rainimua of l.S g of CIS «orbanc, uJing connactori supplitd by cha manufaccur-^
er, and attach cha sorbanc crtln co cht vacuum unlfold. Condition each
cartridge by passing 10 ml dilute acetate buffar (10 ml 5 N acetate buffer
dissolved in 290 ml water) through the sorbanc cartridge train.
3.6.7.3,4.3 Reaove ch« reaction vessel froa che shaker and add 10
•nl saturated NaCl solution to the vessel,
3.6.7.3.4.4 Add the reaction solution to the sorbenc train and
apply a V«CUUB so that that solution is drawn through the cartridges at a race
of 3 co 5 ml/aln. ReIeMe che vacuum after the solution has passed through
che sorbent.
3.6.7.3.4.3 Eluce each cartridge train with approximately 9 ml of
absolute echanol, directly Into a 10 al volumetric flask. Dilute che solution
co volume with absolute ethanol, mixed thoroughly, and place in • tightly
sealed vial until analyzed.
3-198
-------
3.6.7.3. 5 ttechylene Chloride Option
3.6.7.3.5.1 Add 5 D of acetate buffer and adjusc the pH :o 5,0 *
3.5 vi;h glacial acetic acid or 5 N NaOH. Add 10 al a! DNPH reagent, seal :hs
container, and place on a wrist-action shaker for I hour,
3.6,7.3.5.2 Extract che loluclon wish three 20 oi portions of
TiechyLene chloride, using a 250 ml separacory funnel, and combine che aethy-
Lene chloride layers. If an emulsion forms upon extraction, remove che en:ire
emulsion and centrifuge ac.2000 rpm for 10 ainutas. Separate the layers and
proceed wich che nexc extraction.
3.6.7,3.5.3 Assemble a Kudern*-Danish (K-D) concentrator by
attaching a 10 ml concentrator cube to a 500 al evaporator flask Uash she K-
D apparatus with 25 oi oC extraction solvent co complete the quantitative
transfer.
3.6.7.3.5.4 Add one co two clean boiling chips to the evapora:; ?
flask and attach a three ball Snyder column. Preset the Snyder colunn by
adding about I ml methylene chloride eo the cop. Plae* Che K-D apparatus on a
hot water bach (80-90'C) so chat eh* concentrator cub* Is partially Laaersad
in the hoc water and the entire lower rounded surfae* of the flask'is bathed
wich hoe vapor. Adjust che vertical position of eh* apparatus and ch* wacer
ceoperatur*. as required, eo coaplete eh* concentration in 10-15 ain. Ac :he
proper rate of distillation eh* balls of ch* column will actively chatter. bu=
cha chaabers will nee flood with condensed solvent. Uh*n ch* apparent vol^ae
of liquid reaches 10 al, reaove ch* K-D apparatus and allow It to drain and
cool for a leeet 10 Bin.
36.73.5-5 Prior eo liquid chroaa to graphic analysis, ch* solver.:
muse be exchanged co nechanol. The analyse Bust ensure quantitative transfer
of ch* extract concentrate. The exchange Is performed a* fellows:
3-199
-------
3,6.7,3.5,5.1 Following jC-D concentration of th* neehylana chloride
sxcracc co < 10 nl using ch« macro Snyder coluan, allow the apparatus co cool
and drain for at lease 10 ainucis.
3.6 " "* 5.5.2 MoaencarLly remove the Snyder column, add 5 »1 of ;he
.nechanel. a -.= . - oed, or boiling chip, and accaeh ch» aicro Snydar
coluan. Concentrate the extract using I al of nechanol co prewec the Snyder
coluan. Place Chi K-D apparatus on ch* wacar bach so chac ch« concincracar
rubi is partially lcua*rscd In cha hoc water. Adjuse ch« vcrclcal posicion o:
che apparacus and eh* wactr c«np«racur*, ai raqulnd, co complect concancra-
:ion. AC ch* proper -: < of dlscLllacion ch* balls of ch* column will
acciv«ly chacctr. : j chambers will nor flood. '-"h*n ch* apparent voLuae
of liquid rtac- ... reaovi ch* K-D apparatus and allow it Co drain and
cool for ac l*asc *0 minuets.
3.6.7.3.5.5.3 R*«ov* ch* Snyd*r coluam and rlnj* ch* flask and ics"
lou*r Joinc wish 1-2 ml of m*chanol and add co conc*ncracor cub*. A 5-al
syring* is r*coaa*nd*d for chls op*racion. Adjvuc ch* axcraec volua* co 10
nl. Scoppar ch* conc*ncr*cor cub* and scor* r*fri|*rac*d ac 4*C if furcher
processing will noc b* p*rfom*d ism*diac*ly. If ch* extract will b* scored
longer Chan cvo days, le should b* transferred co a vtal wlch a teflon-lined
screw cap or crlap cop. Proceed wich liquid chronacographic analysis if
furchar claanup is noc required.
3.6.7.4 Extraction of Stack Gas SaapUs Collected by Mechod 0011
3,6.7.4.1 MSJMUT* th* aquaous volua* of ch* saapl* prior co excrac-
clon (for swiscur* d*e*nilnacion In cas* ch* volua* was noc taeasured in che
field). Four th* saapl* into a separacory funn«l and drain ch* »*chyl*n*
chloride into a voluaMtrle flask,
3.6.7.4.2 Extract ch* aqueous solution with eve or chree allquocs of
nechylan* chloride. Add ch* methylen* chlorIda axcraccs co ch* volua*cric
flask.
3-200
-------
3.6.7.4.3 Fill che volumetric flask co cha Una vich nethylene
chloride. Mix well and remove an aliquoc.
3.6.7 a.4 if high levels of formaldehyde are presenc. che extract
can be diluted wi'h mobile phase, otherwise che extract muse be solvent
exchanged as described in Section 3.6.7.5.3.3. If low levels of formaldehyde
are presenc, cha sample should be concentrated during cha solvent exchange
procedure,
3.6,7.5 Chromacographic Conditions
Column: CIS, 220 mm x <*. 6 mm ID, 5 pa particle size
Mobile Phase: mechanol/wacer. 75:25 O/v), isoeratlc
Flow Rate: 1.0 ml/min
UV Dececcor: 360 run
Injeccion Volume: 20 j»l
3.6.7.6 Calibration
3.6,7,6.1 Establish liquid cnromatographic operating parameters :o
produce a recencion cine equivalent to that Indicated in Table 3.6-1 for the
solid sorbent options, or in Table 3.6-2 for methylene chloride option.
Suggested chrooatographlc condition! art provided In Section 3.6.7,5. Prepare
derivacized calibration standard* according co the procedure in Section
3.6.7.6.1.1. Calibrate the chroaatographic ayatea using che external standard
technique (Section 3.6.7.4.1.2).
3.6.7.6.1,1 Preparation of calibration standards
3.6,7.6.1.1.1 Prepare calibration standard solutions of formalde-
hyde and acetaldehyda In water froa tha stock standard (Section 3.6.5.1^.2)
Prepare these solutions ac the following concentrations (in pg/al) by serial
dilution of che stock standard solution: 50, 20. 10. Prepare additional
calibration standard solutions ac che following concentrations, by dilution of
the appropriate 30, 20. or 10 itg/al standard: S, 0.3, 2, 0,2. I, 0.1.
3-201
-------
3,6.7,6,1,1.2 Process each calibration standard solution through
che derivasization opcion used for sanple processing (Section 3.6,7.3.4 or
3.6.7,3.5) .
3.6.7.6.1.2 External standard calibration procedure
3.6.7.6.1.2.1 Analyze each derlvatized calibration standard using
the chromatographic conditions listed in Tables 3.6-1 and 3,6-2, and tabulate
peak area against concentration injected. The results nay be used to prepare
calibration curves for formaldehyde and acetaldehyde.
3.6.7.6.1.2.2 The working calibration curve must be verified on
each working day by the measurement of one or more calibration standards. If
the response for any analyte varies from the previously established responses
by more the 10*. the test oust be repeated using a fresh calibration standard
after it is verified that the analytical systea is in control. Alternatively,
a new calibration curve may be prepared for that compound. If an autosaapler
Ls available, it is convenient to prepare a calibration curve dally by
analyzing standards along with test samples.
3.6.7.7 Analysis
3.6.7.7.1 Analyze samples by HPLC, using conditions established in
Section 3.6.7.6.1. Tables 3.6*1 and 3.6-2 list the retention times and MDLs
that were obtained under these conditions. Other HPLC columns, chromatogrtph-
ic conditions, or detectors may be used if the requirements for Section
3.6.8,1 are net, or if the data are within che limits described in Tables
3.6-1 and 3.6-2.
3.6.7.7.2 The width of the retention tine window used to make
identifications should be based upon measurements of actual retention time
variations of standards over the course of a day. Thrasi :iaes the standard
deviation of a retention time for a compound can be used to calculate a
SuSg"ited window size; however, the experience of the analyst should weigh
heavily in the interpretation of the chromatograas.
3-202
-------
3.6.7.7.3 [f the peak area exceeds ehe Linear range of the calibra-
tion curve, a smaller staple volume should be m«d. Alternatively, che final
solution may be diluted with echanol and reanalyzed.
3.6.7.7.4 If che peak area measurement is prevented by che presence
of observed interferences, further -cleanup is required, However, none of che
3600 method series have been evaluated for "his procedure.
3.6.7.8 Calculations
3.6.7.9.1 Calculate each response factor ae follows (moan value
based on 5. points):
concentration of standard
RF - atea of the signal
mean - RF - RF -
3.6.7.8.2 Calculate che concentration of formaldehyde and aeecalde>
hyda as follows:
Mg/nl - (RF) (area of signal) (concentration factor)
where;
Final velum* of extract
concentration factor -
Initial sample (or Leachate) volume
NOTE: For iolld samples, a dilution factor BUJC be included in che equa-
tion Co account for the weight of the sanple used.
3.6.7.8.3 Calculate the total weight of formaldehyde in the stack
gas sample as followa:
3-202
-------
cotal ng/ml - (RF) (area of signal) (concentration factor)
where:
Final Volume of Extract
concentration factor -
Initial Extract Volume
3.6,8 OualL:v Cop'rol
3.6,8.1 Refer to Chapter One of SU-8^6 for guidance on quality
control procedures.
3.6.9 Mechod_ Performance
3.6'.9.1 The HDL concentrations listed in Table 3.6-1 were obtained
using organic-free water and solid sorbenc extraction. Similar results were
achieved using a final affluent and sludge leachace. The HDL concentrations
listed in Table 3.6-2 were obtained using organic*free water and oechylene
chloride extraction. Similar results were achieved using representative *
matrices.
3.6.9.2 This method has been tested for linearity of recovery from
spiked organic-free wacer and has been demonstrated co be applicable over the
range from 2 x HDL to 200 x HDL.
3.6.9.3 In a single laboratory evaluation using several spiked
matrices, the average recoveries presented In Tables 3.6-3 and 3.6-<* were
obtained using solid sorbent and aethylene chloride extraction, respectively
The standard deviations of che percent recovery are also Included in Tables
3.6-3 and 3.6-4.
3.6.9.4 A repreeentacive chroaatograa is presented in
Figure 3.6-1.
3-204
-------
3 . 6 . 10 Reference^
1. Fadaral Ragtscar, 1986, 51, 40643-40652; Novtnbar 7.
2, EPA MachodJ 6010. 7000, 7041, 7060, 7131. 7421, 7470. 7740, and
7841, Jesc Methods got gvaLuattng Solid Uaica:
Methods. SU-846, Third Edlcion. S«pc§ib*r 1938. Office of Solid
'.'asce and Emergency Reiponse, U.S. Environaencal Protection Agir.c;/.
Uashlngcon. D.C. 20460.
3-205
-------
able
SINGH OPERATOR ACO.TUCY AND PRECISION
USING KRHYUNt CHLOIIOI EXTRACTION
AnaLyc*
Foramidthyd*
AC*C*ldahyd«
HmcrU
Typt
J":r
Ground-
v«c«r
liquid*
££"
Ground*
w«car
Liquids
(2 cyp««)
Solid*
Ptreinc
R*cov«ry
X
9L
92.5
69 6
iQ.l
13.1
44.0
SI. A
S candied
D«vl*cion
p»rc«nc
P
2.3
1,2
16. 3
1.2
10. 9
20.2
2.7
SpUt Nuabtr .
fUngt a f
50- LOGO 9 i
50 6
2SO 12
SO. 1000 9
SO 12 - —
230 12
O.lO-l.O- 12
Spll* tr*nf* La unlea of
x * Av*r«g* cceev«cy «xp*ecid for ehia iM
p - Av«ea|« »t*nd»rd d*vl»cton trp«ct»d Cot
taeiiod.
3-206
-------
Figure 3,6-1
f * JO Mi/l SOUT1QM
A °A
* ActtilMijrit
3-20?
-------
METHOD 00 1U
«y UTS* gftffltmMCI gouta
,ua.
•;• a",
r 9
2.!
:•«"«•, H
-mm*
Z.2 C
'V
c. d nrrqet a< wM
JT9 9«'.wff
git •<(* tens ae«
JO
•yltl
7,3,4,2
rj.4j
'"'•MMnflfl *HMI|
Ti*.* MM N*
74.4.1
«iM
«luM It
: i:: ::i : i
"•' :•: :: .r
« • ::t-; :; :
ti :i :::;•.•-
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. :s .r
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M.S.3
3-208
-------
METHOD 001 LA
«•::«•
7 !-'.' 2
2.1
7.5.1.2.1
v
' I.' *«8l»I*
••'
a»ti MA
-------
APPENDIX J.4
PAH
-------
METHOD 0010
MODIFIED METHOD 5 SAMPLING TRAIN
»
1.0 SCOPE AND APPLICATION
l.l This method Is applicable to the determination of Destruction and
Removal Efficiency (ORE) of semi volatile Principal Organic Hazardous Compounds
(POHCs) from Incineration systems (PHS, 1967). This method also may be used
to determine particulate emission rates from stationary sources as per EPA
Method 5 (see References at end of this method).
2.0 SUMMARY OF METHOD
2.1 Gaseous and particulate pollutants are withdrawn from an emission
source at an 1sok1net1c sampling rate and are collected In a multlcomponent
sampling train. Principal components of the train Include a high-efficiency
glass- or quartz-fiber filter and a packed bed of porous polymeric adsorbent
resin. The filter Is used to collect ov^anlc-laden partlculate materials and
the porous polymeric resin to adsorb semi volatile organic species.
Semi volatile species are defined as compounds with boiling points >100*C.
2.2 Comprehensive chemical analyses of the collected sample are
conducted to determine the concentration and Identity of the organic
materials.
3.0 INTERFERENCES
3.1 Oxides of nitrogen (NOX) are possible Interferents 1n the
determination of certain water-soluble compounds such as dloxane, phenol, and
urethane; reaction of these compounds with NO* In the presence of moisture
will reduce their concentration. Other possibilities that could result In
positive or negative bias are (1) stability of the compounds In methylene
chloride, (2) the formation of water-soluble organic salts on the resin In the
presence of moisture, and (3) the solvent extraction efficiency of water-
soluble compounds from aqueous media. Use of two or more Ions per compound
for qualitative and quantitative analysis can overcome Interference at one
mass. These concerns should be addressed on a compound-by-compound basis
before using this method.
4.0 APPARATUS;AND MATERIALS
4.1 Sampling train;
4.1.1 A schematic of the sampling train used In this method Is
shown In Figure 1. This sampling train configuration Is adapted from EPA
Method 5 procedures, and,,,as such, the majority of the required equipment
0010 - 1
Revision
Date September 1986
-------
o
o
I—
o
I
ISJ
T*mpn«HM Senior
Type Piioi Tuba
Rncifculalion Pump
Thermameleit
Impingm* l Ice Balh
Chech Vilne
Vwuivn Line
Oiy Gai Meier An light Piimp
oo
Figure I, Modi I ted Mi-1 hod 5 Sampling Train.
-------
is identical to that used In EPA Method 5 determinations. The new
components required are a condenser coll and a sorbent module, which are
used to collect semlvolatlle organic materials that pass through the
glass- or quartz-fiber filter In the gas phase.
4.1.2 Construction details for the basic train components are given
in APTD-0581 (see Martin, 1971, In Section 13.0, References); commercial
models of this equipment are also available. Specifications for the
sorbent module- are provided 1n the following subsections. Additionally,
the following subsections list changes to APTD-0581 and Identify
allowable train configuration modifications.
4.1.3 Basic operating and maintenance procedures for the sampling
train are described 1n APTD-0576 (see Rom, 1972, In Section 13.0,
References). As correct usage 1s Important in obtaining valid results,
all users should refer to APTD-0576 and adopt the operating and
maintenance procedures outlined therein unless otherwise specified. The
sampling train consists of the components detailed below.
4.1.3.1 Probe nozzle; Stainless steel (316) or glass with
sharp, tapered (30* angle) leading edge. The taper shall be on the
outside to preserve a constant 1.0. The nozzle shall be buttonhook
or elbow design and constructed from seamless tubing (If made of
stainless steel). Other construction materials may be considered
for particular applications. A rangt of nozzle sizes suitable for
isokinetic sampling should be available In increments of 0.16 cm
(1/16 1n.)» e.g., 0.32-1.27 en (1/8-1/2 fn.), OP larger If higher
volume sampling trains are used. Each nozzle shall be calibrated
according to the procedures outlined in Paragraph 9.1.
4.1.3.2 Probe liner; BorosHlcate or quartz-glass tubing with
a heating system capable of maintaining a gas temperature of 120 +
H*e (248 + 25*F) at the exit end during sampling. (The tester may
opt to operate the equipment at a temperature lower than that
specified.) Because the actual temperature at the outlet of the
probe Is not usually monitored during sampling, probes constructed
according to APTD-0581 and utilizing the calibration curves of APTD-
0576 (or calibrated according to the procedure outlined in APTD-
0576) are considered acceptable. Either boroslHcate or quartz-
glass probe liners may be used! for stack temperatures up to about
480"C (900'F). Quartz liners shall be used for temperatures between
480 and 900*C (900 and 1650*F). (The softening temperature for
boroslHcate is 820*C (1508*F)f and for quartz 1500'C (2732*F).)
Water-cooling of the stainless steel sheath will be necessary at
temperatures approaching and exceeding 500*C.
4.1.3.3 Pi tot tube; Typt S, as described in Section 2.1 of
EPA Method 2, or other appropriate devices (Yollaro, 1976). The
pi tot tube shall be attached to the probe to allow constant
monitoring of the stack-gas velocity. The Impact (high-pressure)
opening plane of the pi tot tube shall be even with or above the
nozzle entry plane (see EPA Method 2, Figure 2-6b) during sampling.
The Type S pi tot tube assembly shall have a known coefficient,
determined as outlined 1n Section 4 of EPA Method 2.
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Date September 1986
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4.1.3.4 D1fferent 1 a1 pressure gauge; Inclined manometer or
equivalent device as described InSection2.2 of EPA Method 2. One
manometer shall be used for velocity-head (4P) readings and the
other for orifice differential pressure (iH) readings.
4.1.3.5 Filter holder; Boroslllcate glass, with a glass frit
filter support and a sealing gasket. The sealing gasket should be
made of materials that Mill not Introduce organic material Into the
gas stream at the temperature at which the filter holder will be
maintained. The gasket shall be constructed of Teflon or materials
of equal or better characteristics. The holder design shall provide
a positive seal against leakage at any point along the filter
circumference. The holder shall be attached Immediately to the
outlet of the cyclone or cyclone bypass.
4.1.3.6 Filter heating system; Any heating system capable of
maintaining a temperature of 120 + 14'C (Z48 + 25'F) around the
filter holder during sampling. ~ Other temperatures may be
appropriate for particular applications. Alternatively, the tester
may opt to operate the equipment at temperatures other than that
specified. A temperature gauge capable of measuring temperature to
within 3*C (5.4*F) shall be Installed so that the temperature around
the filter holder can be regulated and monitored during sampling.
Heating systems other than the one shown In APTD-0581 may be used.
4.1.3.7 Organic sampling nodule! This unit consists of three
sections. Including a gas-conditioning section, a sorbent trap* and
a condensate knockout trap. The gas-conditioning system shall be
capable of conditioning the gas leaving the back half of the filter
holder to a temperature not exceeding 20*C (6B'F). The sorbent trap
shall be sized to contain approximately 20 g of porous polymeric
resin (Doha and Haas XAD-2 or equivalent) and shall be Jacketed to
maintain the Internal gas temperature at 17 + 3*C (62.5 * 5.4'F).
The most coanonly used coolant Is Ice water from the tnplnger Ice-
water bath, constantly circulated through the outer Jacket, using
rubber or plastic tubing and a peristaltic pump. The sorbent trap
should be outfitted with a glass well or depression, appropriately
sized to accomodate a snail thermocouple In the trap for monitoring
the gas entry temperature. The condensate knockout trap shall be of
sufficient size to collect the condensate following gas
conditioning. The organic module components shall be oriented to
direct the flow of condensate foraed vertically downward from the
conditioning section, through the adsorbent media, and into the
condensate knockout trap. The knockout trap 1s usually similar 1n
appearance to an empty Inplnger directly underneath the sorbent
module; It may be oversized but should have a shortened center stem
(at a mlnlnun, one-half the length of the normal Implnger stems) to
collect a large volume of condensate without bubbling and
overflowing Into the Implnger train. All surfaces of the organic
module wetted by the gas sanple shall be fabricated of boroslllcate
glass, Teflon, or other Inert materials. Commercial versions of the
0010 - 4
Revision
Date September 1986
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complete organic module are not currently available, but may be
assembled from commercially available laboratory glassware and a
custom-fabricated sorbent trap. Details of two acceptable designs
are shown In Figures 2 and 3 (the thermocouple well Is shown In
Figure 2).
4.1.3.8 Implnqer train; To determine the stack-gas moisture
content, four 500-mL Impingers, connected In series with leak-free
ground-glass Joints, follow the knockout trap. The first, third,
and fourth Implngers shall be of the Greenburg-Smlth design,
modified by replacing the tip with a 1.3-cm (l/2-1n.) I.D. glass
tube extending about 1.3 cm (1/2 In.) from the bottom of the outer
cylinder. The second Implnger shall be of the Greenburg-Smlth
design with the standard tip. The first and second Implngers shall
contain known quantities of water or appropriate trapping solution.
The third shall be empty or charged with a caustic solution, should
the stack gas contain hydrochloric add (HC1). The fourth shall
contain a known weight of silica gel or equivalent deslccant.
4.1.3.9 Metering system: The necessary components are a
vacuum gauge, leak-free pump, thermometers capable of measuring
temperature to within 3*C (S.4*F), dry-gas meter capable of
measuring volume to within IS, and related equipment, as shown In
Figure 1. At a minimum, the pump should be capable of 4 cfm free
flow, and the dry-gas meter should have a recording capacity of
0-999.9 cu ft with a resolution of 0.005 cu ft. Other metering
systems capable of maintaining sampling rates within 101 of
Isold net1 city and of determining sample volumes to within 21 may be
used. The metering system must be used in conjunction with a pltot
tube to enable checks of 1sok1net1c sampling rates. Sampling trains
using metering systems designed for flow rates higher than those
described In APTD-05B1 and APTD-0576 may be used, provided that the
specifications of this method are met.
4.1.3.10 Barometer: Mercury, aneroid, or other barometer
capable of measuring atmospheric pressure to within 2.5 mm Hg (0.1
in. Hg). In many cases the barometric reading may be obtained from
a nearby National Weather Service station, In which case the station
value (which Is the absolute barometric pressure) Is requested and
an adjustment for elevation differences between the weather station
and sampling point Is applied at a rate of minus 2.5 mm Hg (0.1 In.
Hg) per 30-m (100 ft) elevation Increase (vice versa for elevation
decrease).
4.1'. 3.11 Gas density determination equipment; Temperature
sensor and pressure gauge (asdescribedIn Sections 2.3 and 2.4 of
EPA Method 2), and gas analyzer, If necessary (as described 1n EPA
Method 3). The temperature sensor Ideally should be permanently
attached to the pltot tube or sampling probe In a fixed
configuration such that the tip of the sensor extends beyond the
leading edge of the probe sheath and does not touch any metal.
0010 - 5
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September1986
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-S
un
1
E
I
4
o
u
oc
a
i
7
0010 - 6
Revision 0
Data September 1986
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Flo*
He I wriing Sprint] -
8 mm Glm Cooling Coil
o
O
o ya
ttt (ft
r» <
A —
Ffiitdl SlMnteu SicH Diic
28/12 Brfl Jowl
Glw W«im Jacket
16 mm Solv Se«l Joint
(rt« ?8/l?Snckel Jomll
Figure 3. Adsorlieni Sampling System.
-------
Alternatively, the sensor may be attached Just prior to use In the
field. Note, however, that 1f the temperature sensor Is attached in
the field, the sensor must be placed 1n an Interference-free
arrangement with respect to the Type S pi tot tube openings (see EPA
Method 2, Figure 2-7). As a second alternative, If a difference of
no more than IX in the average velocity measurement Is to be
Introduced, the temperature gauge need not be attached to the probe
or pltot tube.
4.1-3.12 Callbratlpn/fleld-preparatlon record: A permanently
bound laboratory notebook" in which duplicate copies of data may be
made as they are being recorded, Is required for documenting and
recording calibrations and preparation procedures (I.e., filter and
silica gel tare weights, clean XAD-2, quality assurance/quality
control check results, dry-gas meter, and thermocouple calibrations,
etc.). The duplicate copies should be detachable and should be
stored separately In the test program archives.
4.2 Sample Recovery;
4.2.1 Probe liner: Probe nozzle and organic module conditioning
section brushes; nylon bristle brushes with stainless steel wire handles
are required. The probe brush shall have extensions of stainless steel,
Teflon, or Inert material at least as long as the probe. The brushes
shall be properly sized and shaped to brush out the probe liner, the
probe nozzle, and the organic module conditioning section.
4.2.2 Wash bottles: Three. Teflon or glass wash bottles are
recommended; polyethylene wash bottles should not be used because organic
contaminants nay be extracted by exposure to organic solvents used for
sample recovery.
4.2.3 Glass saaple storage containers: Chemically resistant,
boroslllcate amber and clear glass bottles, 500-mL or 1,000-mL. Bottles
should be tinted to prevent action of light on sample. Screw-cap liners
shall be either Teflon or constructed so as to be leak-free and resistant
to chemical attack by organic recovery solvents. Narrow-mouth glass
bottles have been found to exhibit less tendency toward leakage.
4.2.4 Petrl dishes: Glass, sealed around the circumference with
wide (I-in.) Teflon tape, for storage and transport of filter samples.
4.2.5 Graduated cylinder and/or balances: To measure condensed
water to the nearest 1 ml or I g. Graduated cylinders shall have
subdivisions not >2 »L. Laboratory triple-bean balances capable of
weighing to +0.5 g or better are required.
4.2.6 Plastic storage containers: Screw-cap polypropylene or
polyethylene containers to store silica gel.
4.2.? Funnel and rubber policeman: To aid in transfer of silica
gel to co "alner (not necessary If silica gel is weighed 1n field).
0010 - 8
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Date September 19B6
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4.2.8 Funnels: Glass, to aid 1n sample recovery.
4.3 Filters: Glass- or quartz-fiber filters, without organic binder,
exhibiting at least 99.951 efficiency «0.051 penetration) on 0.3-um dlocty]
phthalate smoke particles. The filter efficiency test shall be conducted In
accordance with ASTM standard method 02986-71. Test data from the supplier's
quality control program are sufficient for this purpose. In sources
containing S0£ or S0|, the filter material must be of a type that 1s
unreactlve to SO? or $63. Reeve Angel 934 AH or Schlelcher and Schwell 13
filters work well under these conditions.
4.4 Crushed Ice: Quantities ranging from 10-50 1b may be necessary
during a sampling run, depending on ambient air temperature.
4.5 Stopcock grease: Solvent-insoluble, heat-stable slUcone grease.
Use of s11Iconegrease upstream of the module 1s not permitted, and amounts
used on components located downstream of the organic module shall be
minimized. SlUcone grease usage 1s not necessary If screw-on connectors and
Teflon sleeves or ground-glass Joints are used.
4.6 Glass wool: Used to plug the unfrltted end of the sorbent module.
The glass-wool fiber should be solvent-extracted with methylene chloride In a
Soxhlet extractor for 12 hr and a1r-dr1ed prior to use.
5.0 REAGENTS
5.1 Adsorbent resin; Porous polymeric restn (XAD-2 or equivalent) 1$,
recommendedThese resins shall be cleaned prior to their use for sample
collection. Appendix A of this method should be consulted to determine
appropriate precleaning procedure. For best results, resfn used should not
exhibit a blank of higher than 4 rag/kg of total chromatographable organic*
(TCO) (see Appendix B) prior to use. Once cleaned, resin should be stored In
an airtight, wide-mouth amber glass container with a Teflon-lined cap or
placed In one of the glass sorbent modules tightly sealed with Teflon film and
elastic bands. The resin should be used within 4 wk of the preparation.
5.2 Silica flel; Indicating type, 6-16 mesh. If previously used, dry at
175*C (35Q*F) for Z hr btfore using. New silica gel nay be used as received.
Alternatively, other types of deslccants (equivalent or better) may be used,
subject to the approval of the Administrator.
5.3 Implnger solutions; Distilled organic-free water (Type II) shall be
used, unless sampling Is Intended to quantify a particular Inorganic gaseous
species. If sampling Is Intended to quantify the concentration of additional
species, the 1mplnger solution of choice shall be subject to Administrator
approval. This water should be prescreened for any compounds of Interest.
One hundred ml will be added to the specified fmplnger; the third Inpfnger In
the train may be charged with a baste solution (1 N sodium hydroxide or sodium
acetate) to protect the sampling pump from acidic gases. Sodlun acetate
should be used when large sample volumes are anticipated because sodium
hydroxide will react with carbon dioxide In aqueous media to fora sodium
carbonate, which may possibly plug the 1mplnger.
0010 - 9
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Date September 1986
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5.4 Sample recovery reagents;
5.4.1 Methylene chloride: 01st1lled-1n-glass grade Is required for
sample recovery and cleanup (see Note to 5.4.2 below).
5.4.2 Methyl alcohol: Distilled-ln-glass grade 1s required for
sample recovery and cleanup.
NOTE: Organic solvents from metal containers may have a high
-residue blank and should not be used. Sometimes suppliers
transfer solvents from metal to glass bottles: thus blanks shall
be run prior to field use and only solvents with low blank value
«0.001X) shall be used.
5.4.3 Water: Water (Type II) shall be used for rinsing the organic
module and condenser component.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1 Because of complexity of this method, field personnel should be
trained In and experienced with the test procedures In order to obtain
reliable results.
6.2 Laboratory preparation;
6.2.1 All the components shall be maintained and calibrated
according to the procedure described In APTD-0576, unless otherwise
specified.
6.2.2 Weigh several 200- to 300-g portions of silica gel in
airtight containers to the nearest 0.5 g. Record on each container the
total weight of the silica gel plus containers. As an alternative to
prewelghlng the silica gel, It my Instead be weighed directly In the
Implnger or sampling holder Just prior to train assembly.
6.2.3 Check filters visually against light for Irregularities and
flaws or plnhole leaks. Label the shipping containers (glass Petrl
dishes) and keep the filters 1n these containers at all times except
during sampling and weighing.
6.2.4 Desiccate the filters at 20 + 5.6*C (68 + 10'F) and ambient
pressure for at least 24 hr, and weigh at Intervals of"at least 6 hr to a
constant weight (I.e., <0.5-og change froa previous weighing), recording
results to the nearest 0.1 mg. During each weighing the filter must not
be exposed for more than a 2-m1n period to the laboratory atmosphere and
relative humidity above 501. Alternatively (unless otherwise specified
by the Administrator), the filters My be oven-dried at 105'C (220*F) for
2-3 hr, desiccated for 2 hr, and weighed.
0010 - 10
Revision 0
Date September1986
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6.3 Preliminary field determinations;
6.3.1 Select the sampling site and the minimum number of sampling
points according to EPA Method 1 or as specified by the Administrator.
Determine the stack pressure, temperature, and range of velocity heads
using EPA Method 2. It 1s recommended that a leak-check of the pilot
lines (see EPA Method 2, Section 3.1) be performed. Determine the stack-
gas moisture content using EPA Approximation Method 4 or Its alternatives
to establish estimates of Isoklnetlc sampling-rate settings. Determine
the stack-gas dry molecular weight, as described In EPA Method 2, Section
3.6. If Integrated EPA Method 3 sampling 1s used for molecular weight
determination, the Integrated bag sample shall be taken simultaneously
with, and for the same total length of time as, the sample run.
6.3.2 Select a nozzle size based on the range of velocity heads so
that It 1s not necessary to change the nozzle size 1n order to maintain
Isoklnetlc sampling rates. During the run, do not change the nozzle.
Ensure that the proper differential pressure gauge Is chosen for the
range of velocity heads encountered (see Section 2.2 of EPA Method 2).
6.3.3 Select a suitable probe liner and probe length so that all
traverse points can be sampled. For large stacks, to reduce the length
of the probe, consider sampling from opposite sides of the stack.
6.3.4 A minimum of 3 dscm (105.9 dscf) of sample volume 1s required
for the determination of the Destruction and Removal Efficiency (DRE) of
POHCs from Incineration systems. Additional sample volume shall be
collected as necessitated by analytical detection limit constraints. To
determine the minimum sample volume required, refer to sample
calculations 1n Section 10.0.
6.3.5 Determine the total length of sampling time needed to obtain
the Identified minimum volume by comparing the anticipated average
sampling rate with the volume requirement. Allocate the same time to all
traverse points defined by EPA Method 1. To avoid timekeeping errors,
the length of time sampled at each traverse point should be an Integer or
an Integer plus one-half Bin.
6.3.6 In some circumstances (e.g., batch cycles) It may be
necessary to sample for shorter times at the traverse points and to
obtain smaller gas-sample volumes. In these cases, the Administrator's
approval must first be obtained.
6.4 Preparation of collection train;
6.4.1 During preparation and assembly of the sampling train, keep
all openings where contamination can occur covered with Teflon film or
aluminum foil until Just prior to assembly or until sampling Is about to
begin.
0010 - 11
Revision
Date September 1986
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6.4.2 Fill the sorbent trap, section of the organic module with
approximately 20 Q of clean adsorbent resin. While filling, ensure that
the trap packs uniformly, to eliminate the possibility of channeling.
When freshly cleaned, many adsorbent resins carry a static charge, which
will cause clinging to trap walls. This may be minimized by filling the
trap In the presence of an antistatic device. Commercial antistatic
devices Include Model-204 and Model-210 manufactured by the 3H Company,
St. Paul, Minnesota.
6.4.3 If an Implnger train Is used to collect moisture, place 100
ml of water In each of the first two Impingers, leave the third Implnger
empty (or charge with caustic solution, as necessary), and transfer
approximately 200-300 g of prewelghed silica gel from Its container to
the fourth Implnger. More silica gel may be used, but care should be
taken to ensure that It Is not entrained and carried out from the
Implnger during sampling. Place the container In a clean place for later
use in the sample recovery. Alternatively, the weight of the stUca gel
plus Implnger nay be determined to the nearest 0.5 g and recorded.
6.4.4 Using a tweezer or clean disposable surgical gloves, place a
labeled (identified) and weighed filter In the filter holder. Be sure
that the filter Is properly centered and the gasket properly placed to
prevent the sample gas strean from circumventing the filter. Check the
filter for tears after assembly Is completed.
6.4.5 When glass liners art used, Install the selected nozzle using
a VUon-A 0-r1ng when stack temperatures are <260*C (500'P) and a woven
glass-fiber gasket when temperatures are higher. See APTD-0576"(Rom,
1972) for details. Other connecting system utilizing either 316
stainless steel or Teflon ferrules say be used. When aetal liners are
used. Install the nozzle as above, or by a leak-free direct mechanical
connection. Nark the probe with heat-resistant tape or by some other
method to denote the proper distance Into the stack or duct for each
sampling point.
6.4.6 Set up the train as 1n Figure 1. During assembly, do not use
any sllicone grease on ground-glass Joints that are located upstream of
the organic nodule. A very light coating of stHcone grease may be used
on all ground-glass Joints that are located downstream of the organic
module, but it should be Halted to the outer portion (see APTD-0576) of
the ground-glass Joints to nlnlmlze si 11cone-grease contamination.
Subject to the approval of the Adn1n1strator, a glass cyclone nay be used
between the probe and the filter holder when the total partlculate catch
Is expected to exceed 100 ng or when water droplets are present in the
stack. The organic Module condenser oust be maintained at a temperature
of 17 + 3*C. Connect all temperature sensors to an appropriate
potentioieter/dlsplay unit. Check all temperature sensors at ambient
temperature.
6.4.7 Place crushed Ice around the implngers and the organic module
condensate knockout.
0010 - 12
Revision
Date September 1986
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6.4.8 Turn on the sorbent module and condenser coll coolant
redrculatlng pump and begin monitoring the sorbent module gas entry
temperature. Ensure proper sorbent module gas entry temperature before
proceeding and again before any sampling Is Initiated. It Is extremely
Important that the XAD-2 resin temperature never exceed 50*C (122*F),
because thermal decomposition will occur. During testing, the XAD-2
temperature must not exceed 20'C (68*F) for efficient capture of the
semi volatile species of Interest.
6.4.9 Turn on and set the filter and probe heating systems at the
desired operating temperatures. Allow time for the temperatures to
stabilize.
6.5 Leak-checkprocedures
6.5.1 Pre-test leak-check:
6.5.1.1 Because the number of additional tntercomponent
connections In the Seml-VOST train (over the MS Train) Increases the
possibility of leakage, a pre-test leak-check 1s required.
6.5.1.2 After the sampling train has been assembled, turn on
and set the filter and probe heating systems at the desired
operating temperatures. Allow time for the temperatures to
stabilize. If a VIton A 0-r1ng or other leak-free connection 1s
used In assembling the probe nozzle to the probe Hner, leak-check
the train at the sampling site by plugging the nozzle and pulling a
381-mm Hg (15-ln. Hg) vacuum.
(NOTE: A lower vacuum may be used, provided that It 1s not exceeded*
during the test.)
6.5.1.3 If an asbestos string Is used, do not connect the
probe to the train during the leak-check. Instead, leak-check the
train by first attaching a carbon-filled leak-check Implnger (shown
in Figure 4) to the Inlet of the filter holder (cyclone, If applic-
able) and then plugging the Inlet and pulling a 381-nn Hg (15-ln.
Hg) vacuum. (Again, a lower vacuum may be used, provided that It 1s
not exceeded during the test.) Then, connect the probe to the train
and leak-check at about 25-m Hg (l-1n. Hg) vacuum; alternatively,
leak-check the probe with the rest of the sampling train 1n one step
at 381-mn Hg (15-ln. Kg) vacuua. Leakage rates In excess of 41 of
the average sailing rate or X.00057 nH/min (0.02 cfo), whichever
is less, are unacceptable.
6.5.1.4 The following leak-check Instructions for the sampling
train described In APTD-0576 and APTD-0581 may be helpful. Start
the pump with fine-adjust valve fully open and coarse-adjust valve
completely closed. Partially open the coarse-adjust valve and
slowly close the fine-adjust valve until the desired vacuum Is
reached. Do not reverse direction of the fine-adjust valve; this
will cause water to back up Into the organic module. If the desired
vacuum Is exceeded, either leak-check at this higher vacuum or end
the leak-check, as shown below, and start over.
0010 - 13
Revision 0
Date September 1986
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Lftk T«t1ng
ti/u r**
Joint
M/lf
ActlvttM
Ffgyrt 4. Leak-chtck fnpfngtr.
0010 - 14
Rtvlslon
September 1986
-------
6.5.1.5 When the leak-check Is completed, first slowly remove
the plug from the Inlet to the probe, filter holder, or cyclone (If
applicable). When the vacuum drops to 127 mn (5 1n.) Hg or less,
Immediately close the coarse-adjust valve. Switch off the pumping
system and reopen the fine-adjust valve. Do not reopen the fine-
adjust valve until the coarse-adjust valve has been closed. This
prevents the water In the Implngers from being forced backward Into
the organic module and silica gel from being entrained backward Into
the th1rd~1mp1nger.
6.5.2 Leak-checks during sampling run:
6.5.2.1 If, during the sampling run, a component (e.g., filter
assembly, Itnplnger, or sorbent trap) change becomes necessary, a
leak-check shall be conducted Immediately after the Interruption of
sampling and before the change 1s made. The leak-check shall be
done according to the procedure outlined 1n Paragraph 6.5.1, except
that 1t shall be done at a vacuum greater than or equal to the
maximum value recorded up to that point In the test. If the leakage
rate Is found to be no greater than 0.00057 oP/nln (0.02 cfm) or 41
of the average sampling rate (whichever Is less), the results are
acceptable, and no correction will need to be applied to the total
volume of dry gas metered. If a higher leakage rate Is obtained,
the tester shall void the sampling run. (It should be noted that
any "correction" of the sample volume by calculation by calculation
reduces the Integrity of the pollutant concentrations data generated
and must be avoided.)
6.5.2.2 Immediately after a component change, and before"
sampling 1s reinitiated, a leak-check similar to a pre-test leak-
check must also be conducted.
6.5.3 Post-test leak-check:
6.5.3.1 A leak-check Is mandatory at the conclusion of each
sampling run. The leak-check shall be done with the sane procedures
as those with the pre-test leak-check, except that 1t shall be
conducted at a vacuum greater than or equal to the maximum value
reached during the sampling run. If the leakage rate Is found to be
no greater than 0.00057 oH/mln (0.02 cfm) or 41 of the average
sampling rate (whichever ts less), the results are acceptable, and
no correction need be applied to the total volume of dry gas
metered. If, however, a higher leakage rate Is obtained, the tester
shall either record the leakage rate, correct the sample volume (as
shown In the calculation section of this method), and consider the
data obtained of questionable reliability, or void the sampling run.
6.6 Sampling-train operation;
6.6.1 During the sampling run, maintain an Isoklnetlc sampling rate
to within 101 of true Isoklnetlc, unless otherwise specified by the
Administrator. Maintain a temperature around the filter of 120 + u'C
(248 + 25*F) and a gas temperature entering the sorbent trap at a naxloua
of 20TC (68*F).
0010 - 15
Revision 0
Date September 1986
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6.6.2 For each run, record the data required on a data sheet such
as the one shown In Figure 5. Be sure to record the Initial dry-gas
meter reading. Record the dry-gas meter readings at the beginning and
end of each sampling time Increment, when changes In flow rates are made
before and after each leak-check, and when sampling Is halted. Take
other readings required by Figure 5 at least once at each sample point
during each time Increment and additional readings when significant
changes (201 variation In velocity-head readings) necessitate additional
adjustments In flow rate. Level and zero the manometer. Because the
manometer level and zero may drift due to vibrations and temperature
changes, make periodic checks during the traverse.
6.6.3 -Clean the stack access ports prior to the test run to
eliminate the chance of sampling deposited material. To begin sampling,
remove the nozzle cap, verify that the filter and probe heating systems
are at the specified temperature, and verify that the pi tot tube and
probe are properly positioned. Position the nozzle at the first traverse
point, with the tip pointing directly Into the gas stream. Immediately
start the pump and adjust the flow to 1sok1net1c conditions. Nomographs,
which aid 1n the rapid adjustment of the Isoklnetlc sampling rate without
excessive computations, are available. These nomographs are designed for
use when the Type S pi tot-tube coefficient Is 0.84 + 0.02 and the stack-
gas equivalent density (dry molecular weight) Is equal to 29 + 4. APTD-
0576 details the procedure for using the nomographs. If the stack-gas
molecular weight and the p1tot-tube coefficient are outside the above
ranges, do not use the nomographs unless appropriate steps (Shlgehara,
1974) are taken to compensate for the deviations.
6.6.4 When the stack Is under significant negative pressure
(equivalent to the height of the 1mp1nger stem), take care to close the
coarse-adjust valve before Inserting the probe Into the stack, to prevent
water from backing Into the organic module. If necessary, the pump may
be turned on with the coarse-adjust valve closed.
6.6.5 When the probe Is In position, block off the openings around
the probe and stack access port to prevent unrepresentative dilution of
the gas streaa.
6.6.6 Traverse the stack cross section, as required by EPA Method 1
or as specified by the Administrator, being careful not to bump the probe
nozzle Into tht stack walls when sampling near the walls or when removing
or inserting tht probe through the access port, in order to minimize the
chance of extracting deposited eatenal.
6.6.7 During the test run, make periodic adjustments to keep the
temperature around the filter holder and the organic module at the proper
levels; add more Ice and, If necessary, salt to maintain a temperature of
<20*C (68*F) at the condenser/silica gel outlet. Also, periodically
check the level and zero of the manometer.
0010 - 16
Revision
Date September 1986
-------
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6.6.8 If the pressure drop across the filter or sot-bent trap
becomes too high, making isoklnetic sampling difficult to maintain, the
fllter/sorbent trap may be replaced In the midst of a sample run. Using
another complete filter holder/sorbent trap assembly 1s recommended,
rather than attempting to change the filter and resin themselves. After
a new fllter/sorbent trap assembly Is Installed, conduct a leak-check.
The total paniculate weight shall Include the summation of all filter
assembly catches.
6.6.9 A single train shall be used for the entire sample run,
except in cases where simultaneous sampling is required in two or more
separate ducts or at two or more different locations within the same
duct, or in cases where equipment failure necessitates a change of
trains. In all other situations, the use of two or more trains will be
subject to the approval of the Administrator.
6.6.10 Note that when two or more trains are used, separate
analysis of the front-half (if applicable) organic-module and impinger
(If applicable) catches from each train shall be performed, unless
identical nozzle sizes were used on all trains. In that case, the front-
half catches from the Individual trains may be combined (as may the
Impinger catches), and one analysis of front-half catch and one analysis
of impinger catch may be performed.
6.6.11 At the end of the sample run, turn off the coarse-adjust
valve, remove the probe and nozzle from the stack, turn off the pump,
record the final dry-gas meter reading, and conduct a post-test leak-
check. Also, leak-check the pi tot lines as described-in EPA Method 2.
The lines must pass this leak-check In order to validate the velocity-
head data.
6.6.12 Calculate percent isoklneticity (see Section 10.8) to
determine whether the run was valid or another test run should be made.
7.0 SAMPLE RECOVERY
7.1 Preparation?
7.1.1 Proper cleanup procedure begins as soon as the probe 1s
removed from the stack.at the end of the sampling period. Allow the
probe to cool. Mien the probe can be safely handled, wipe off all
external parti cutate natter near the tip of the probe nozzle and place a
cap over the tip to prevent losing or gaining partlculate matter. Do not
cap the probe tip tightly while the sampling train is cooling down
because this will create a vacuum In the filter holder, drawing water
from the implngers Into the sortent module.
7.1.2 Before moving the sample train to the cleanup site, remove
the probe from the sample train and cap the open outlet, being careful
not to lose any condensate that might be present. Cap the filter Inlet.
0010 - 18
Revision 0
Date September 1986
-------
Remove the umbilical cord from the last 1mp1nger and cap the Implnger.
If a flexible line Is used between the organic module and the filter
holder, disconnect the line at the filter holder and let any condensed
water or liquid drain Into the organic module.
7.1.3 Cap the filter-holder outlet and the Inlet to the organic
module. Separate the sorbent trap section of the organic module from the
condensate knockout trap and the gas-conditioning section. Cap all
organic module openings. Disconnect the organic-module knockout trap
from the implnger train Inlet and cap both of these openings. Ground-
glass stoppers, Teflon caps, or caps of other Inert materials may be used
to seal all openings.
7.1.4 Transfer the probe, the filter, tht organic-nodule
components, and the Implnger/condenser assembly to the cleanup area.
This area should be clean and protected from the weather to minimize
sample contamination or loss.
7.1.5 Save a portion of all washing solutions (methanol/methylene
chloride, Type II water) used for cleanup as a blank. Transfer 200 ml of
each solution directly from the wash bottle being used and place each In
a separate, prelabeled glass sample container.
7.1.6 Inspect the train prior to and during disassembly and note
any abnormal conditions.
7.2 Sample containers;
7.2.1 Container no. 1: Carefully remove the filter froo the filter
holder and place 1t In Us Identified Petrl dish container. Use a pair
or pairs of tweezers to handle the filter. If It 1$ necessary to fold
the filter, ensure that the partlculate cake Is Inside the fold.
Carefully transfer to the Petrl dish any partlculate natter or filter
fibers that adhere to the filter-holder gasket, using a dry nylon bristle
brush or sharp-edged blade, or both. Label the container and seal with
l-1n.-w1de Teflon tape around the circumference of the lid.
7.2.2 Container no. 2: Taking care that dust on the outside of the
probe or other exterior surfaces does not get Into the sample,
quantitatively recover partlculate matter or any condensate froa the
probe nozzle, probe fitting, probe Hner, and front half of the filter
holder by washing these components first with methanol/nethylene chloride
(1:1 v/v) Into a glass container. Distilled water may also be used.
Retain a water and solvent blank and analyze fn the same manner as with
the samples. Perform rinses as follows:
7.2.2.1 Carefully remove the probe nozzle and clean the Inside
surface by rinsing with the solvent mixture (1:1 v/v nethanol/-
methylene chloride) from a wash bottle and brushing with a nylon
bristle brush. Brush until the rinse shows no visible particles;
then make a final rinse of the Inside surface with the solvent mix.
Brush and rinse the Inside parts of the Swage1ok fitting with the
solvent mix 1n a similar way until no visible particles remain.
0010 - 19
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Date September 1986
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7.2.2.2 Have two people rinse the probe liner with the solvent
mix by tilting and rotating the probe while squirting solvent Into
Us upper end so that all Inside surfaces will be wetted with
solvent. Let the solvent drain from the lower end Into the sample
container. A glass funnel may be used to aid In transferring liquid
washes to the container.
7.2.2.3 Follow the solvent rinse with a probe brush. Hold the
probe 1n an Inclined position and squirt solvent Into the upper end
while pushing the probe brush through the probe with a twisting
action; place a sample container underneath the lower end of the
probe and catch any solvent and particulate matter that 1s brushed
from the probe. Run the brush through the probe three times or more
until no visible particulate matter Is carried out with the solvent
or until none remains 1n the probe liner on visual Inspection. With
stainless steel or other metal probes, run the brush through In the
above-prescribed manner at least six times (metal probes have small
crevices In which partlculate matter can be entrapped). Rinse the
brush with solvent and quantitatively collect these washings In the
sample container. After the brushing, make a final solvent rinse of
the probe as described above.
7.2.2.4 It Is recommended that two people work together to
clean the probe to minimize sample losses. Between sampling runs,
keep brushes clean and protected from contaalnation.
7.2.2.5 Clean the Inside of the front half of the filter
holder and cyclone/cyclone flask, 1f used, by rubbing the surfaces
with a nylon bristle brush and rinsing with methanol/methylene
chloride (1:1 v/v) alxtura. Rinse each surface three times or more
1f needed to remove visible paniculate. Make a final rinse of the
brush and filter holder. Carefully rinse out the glass cyclone and
cyclone flask (1f applicable). Brush and rinse any partlculate
material adhering to the Inner surfaces of these components Into the
front-half rinse sample. After all solvent washings and partlculate
matter have been collected In the sample container, tighten the lid
on the sample container so that solvent will not leak out when It 1s
shipped to the laboratory. Hark the height of the fluid level to
determine whether leakage occurs during transport. Label the
container to Identify Us contents.
7.2.3 Container no. 3: The sorbent trap section of the organic
module nay be used as a sample transport container, or the spent resin
may be transferred to a separate glass bottle for shipment. If the
sorbent trap Itself 1s used as the transport container, both ends should
be sealed with tightly fitting caps or plugs. Ground-glass stoppers or
Teflon caps nay be used. The sorbent trap should then be labeled,
covered with alumlnua foil, and packaged on Ice for transport to the
laboratory. If a separate bottle Is used, the spent resin should be
quantitatively transferred froa the trap Into the clean bottle. Resin
that adheres to the walls of the trap should be recovered using a rubber
policeman or spatula and added to this bottle.
0010 - 20
Revision 0
Date September 1966
-------
7.2.4 Container no. 4: Measure the volume of condensate collected
In the condensate knockout section of the organic module to within +1 ml
by using a graduated cylinder or _by weighing to within +0.5 g using a,
triple-beam balance. Record the volume or weight of 11quid present and
note any discoloration or film 1n the liquid catch. Transfer this liquid
to a prelabeled glass sample container. Inspect the back half of the
filter housing and the gas-conditioning section of the organic module.
If condensate Is observed, transfer It to a graduated or weighing bottle
and measure the volume, as described above. Add this material to the
condensate knockout-trap catch.
7.2.5 Container no. 5: All sampling train components located
between the high-efficiency glass- or quartz-fiber filter and the first
wet Implnger or the final condenser system (Including the heated Teflon
line connecting the filter outlet to the condenser) should be thoroughly
rinsed with methanol/methylene chloride (1:1 v/v) and the rinsings
combined. This rinse shall be separated from the condensate. If the
spent resin Is transferred from the sorbent trap to a separate sample
container for transport, the sorbent trap shall be thoroughly rinsed
until all sample-wetted surfaces appear clean. Visible films should be
removed by brushing. Whenever train components are brushed, the brush
should be subsequently rinsed with solvent mixture and the rinsings added
to this container.
7.2.6 Container no. 6: Note the color of the Indicating silica gel
to determine If It has been completely spent and make a notation of Its
condition. Transfer the silica gel from the fourth Implnger to Its
original container and seal. A funnel may make It easier to pour the
silica gel without spilling. A rubber policeman may be used as an aid 1n
removing the silica gel from the Implnger. It Is not necessary to remove
the small amount of dust particles that may adhere strongly to the
Implnger wall. Because the gain In weight 1s to be used for moisture
calculations, do not use any water or other liquids to transfer the
silica gel. If a balance Is available In the field, weigh the container
and Its contents to 0.5 g or better.
7-3 Implnger water;
7.3.1 Make a notation of any color or film In the liquid catch.
Measure the liquid In the first three Implngers to within +1 ml by using
a graduated cylinder or by weighing It to within +0.5" g by using a
balance (If one Is available). Record the volume or weight of liquid
present. This Information Is required to calculate the moisture content
of the effluent gas.
7.3.2 Discard the liquid after measuring and recording the volume
or weight, unless analysis of the Implnger catch Is required (see
Paragraph 4.1.3.7). Amber glass containers should be used for storage of
Implnger catch, If required.
7.3.3 If a different type of condenser 1s used, measure the amount
of moisture condensed either volunetrlcally or gravlnetrlcally.
0010 - 21
Revision 0
Date September 1986
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7.4 Sample preparation for shipment; Prior to shipment, recheck all
sample containers to ensure that thecapsare well secured. Seal the lids of
all containers around the circumference with Teflon tape. Ship all liquid
samples upright on 1ce and all paniculate filters with the partlculate catch
facing upward. The partlculate filters should be shipped unrefrlgerated.
8.0 ANALYSIS
8.1 Sample preparation:
8.1.1 General: The preparation steps for all samples will result
tn a finite volume of concentrated solvent. The final sample volume
(usually In the 1- to 10-mL range) Is then subjected to analysis by
GC/MS. All samples should be Inspected and the appearance documented.
All samples are to be spiked with surrogate standards as received from
the field prior to any sample manipulations. The spike should be at a
level equivalent to 10 times the MOL when the solvent Is reduced In
volume to the desired level (I.e., 10 nL). The spiking compounds should
be the stable Isotoplcally labeled analog of the compounds of Interest or
a compound that would exhibit properties similar to the compounds of
Interest, be easily chromatographed, and not Interfere with the analysis
of the compounds of Interest. Suggested surrogate spiking compounds are:
deuterated naphthalene, chrysene, phenol, nitrobenzene, chlorobenzene,
toluene, and carbon-13-labeled pentachlorophenol.
8.1.Z Condensate: The "condensate" Is the moisture eg 11ecjed In.
the first Implnger following the XAO-Z module. Spike the condensate with
the surrogate standards. The volume Is measured and recorded and then
transferred to a separatory funnel. The pH Is to be adjusted to pH 2
with 6 N sulfurlc add, 1f necessary. The sample container and graduated
cylinder are sequentially rinsed with three successive 10-mL altquots of
the extraction solvent and added to the separatory funnel. The ratio of
solvent to aqueous sample should be maintained at 1:3. Extract the
sample by vigorously shaking the separatory funnel for 5 rain, After
complete separation of the phases, remove the solvent and transfer to a
Kuderna-Danlsh concentrator (K-D), filtering through a bed of precleaned,
dry sodium sulfate. Repeat the extraction step two additional times.
Adjust the pH to 11 with 6 M sodium hydroxide and reextract combining the
add and base extracts. Rinse the sodium sulfate Into the K-D with fresh
solvent and discard the deslccant. Add Teflon boiling chips and
concentrate to 10 ml by reducing the volume to slightly less than 10 ml
and then bringing to volume with fresh solvent. In order to achieve the
necessary detection limit, the sample volume can be further reduced to 1
ml by using a micro column K-0 or nitrogen blow-down. Should the sample
start to exhibit precipitation, the concentration step should be stopped
and the sample redlssolved with fresh solvent taking the volume to some
finite amount. After adding a standard (for the purpose of quantltatlon
by GC/MS), the sample 1s ready for analysis, as discussed in Paragraph
8.2.
0010 - 22
Revision 0
Date September 1986
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8.1.3 Inplnger: Spike the sample with the surrogate standards;
measure and record the volume and transfer to a separatory funnel.
Proceed as described 1n Paragraph 8.1.2.
8.1.4 XAO-2: Spike the resin directly with the surrogate
standards. Transfer the resin to the all-glass thimbles by the following
procedure (care should be taken so as not to contaminate the thimble by
touching It with anything other than tweezers or other solvent-rinsed
mechanical hording devices). Suspend the XAO-2 module directly over the
thimble. The glass frit of the module (see Figure 2) should be 1n the up
position. The thimble is contained In a clean beaker, which will serve
to catch the solvent rinses. Using a Teflon squeeze bottle, flush the
XAO-2 Into the thimble. Thoroughly rinse the glass module with solvent
Into the beaker containing the thimble. Add the XAD-2 glass-wool plug to
the thimble. Cover the XAD-2 1n the thimble with a precleaned glass-wool
plug sufficient to prevent the resin from floating Into the solvent
reservoir of the extractor. If the resin 1s wet, effective extraction
can be accomplished by loosely packing the resin in the thimble. If a
question arises concerning the completeness of the extraction, a second
extraction, without a spike, Is advised. The thimble Is placed In the
extractor and the rinse solvent contained In the beaker Is added to the
solvent reservoir. Additional solvent 1s added to make the reservoir
approximately two-thirds full. Add Teflon boiling chips and assemble the
apparatus. Adjust the heat source to cause the extractor to cycle 5-6
times per hr. Extract the resin for 16 hr. Transfer the solvent and
three 10-mL rinses of the reservoir to a K-D and concentrate as described
1n Paragraph 8.1.2.
8.1.5 Paniculate filter (and cyclone catch): If participate
loading Is to be determined, weigh the filter (and cyclone catch, if
applicable). The partlculate filter (and cyclone catch, If applicable)
1s transferred to the glass thimble and extracted simultaneously with the
XAO-2 resin.
8.1.6 Train solvent rinses: All train rinses (I.e., probe,
Implnger, filter housing) using the extraction solvent and methanol are
returned to the laboratory as a single sample. If the rinses are
contained In more than one container, the Intended spike Is divided
equally among the containers proportioned from a single syringe volume.
Transfer the rinse to a separatory funnel and add a sufficient amount of
organic-free water so that the nethylene chloride becomes Immiscible and
Us volume no longer Increases with the addition of more water. The
extraction and concentration steps are then performed as described In
Paragraph 8.1.2.
8.2 Sampleanalysis;
8.2.1 The primary analytical tool for the measurement of emissions
from hazardous waste Incinerators is GC/MS using fused-slllca capillary
GC columns, as described In Method 8270 In Chapter Four of this manual.
Because of the nature of GC/MS Instrumentation and the cost associated
0010 - 23
Revision
Date September 1986
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with sample analysis, prescreenlng of the sample extracts by gas
chromatography/flame lonlzatlon detection (GC/FID) or with electron
capture (GC/ECD) Is encouraged. Information regarding the complexity and
concentration level of a sample prior to GC/MS analysis can be of
enormous help. This Information can be obtained by using either
capillary columns or less expensive packed columns. However, the FID
screen should be performed with a column similar to that used with the
GC/MS. Keep 1n mind that GC/FID has a slightly lower detection limit
than Gt/MS and, therefore, that the concentration of the sample can be
adjusted either up or down prior to analysis by GC/MS.
8.2.2 The mass spectrometer will be operated In a full scan (40-
450) mode for most of the analyses. The range for which data are
acquired In a GC/HS run wlU be sufficiently broad to encompass the major
ions, as listed In Chapter Four, Method 8270, for each of the designated
POHCs In an Incinerator effluent analysis.
8.2.3 For most purposes, electron lonlzatlon (El) spectra will be
collected because a majority of the POHCs give reasonable El spectra.
Also, El spectra are compatible with the NBS Library of Mass Spec--a and
other mass spectral references, which aid 1n the Identification . ocess
for other components In the Incinerator process streams.
8.2.4 To clarify some Identifications, chemical lonlzatlon (CI)
spectra using either positive Ions or negative Ions will be used to
elucidate molecular-weight Information and simplify the fragmentation
patterns of some compounds. In no case, however, should CI spectra alone
be used for compound Identification. Refer to Chapter Four, Method 8270,
for complete descriptions of GC conditions, MS conditions, and
quantitative and quantitative Identification.
9.0 CALIBRATION
9i1 Probe nozzle; Probe nozzles shall be calibrated before their
Initial use In the field. Using a ralcr iter, measure the Inside diameter of
the nozzle to the nearest 0.025 on (0...1 In.). Hake measurements at three
separate places across the diameter and obtain the average of the
measurements. The difference between the high and low numbers shall not
exceed 0.1'mn (0.004 In.). When nozzles become nicked, dented, or corroded,
they shall be reshaped, sharpened, and recalibrated before use. Each nozzle
shall be permanently and uniquely Identified.
9.2 Pi tot tube; The Type S pitot tube assembly shall be callbratec
according to the procedure outlined In Section 4 of EPA Method 2, or assignee
a nominal coefficient of 0.84 If It Is not visibly nicked, dented, or corrode*
and 1f It meets design and Intercomponent spacing specifications.
0010 - 24
Revision 0
Date September 1986
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9-3 Metering system;
9.3.1 Before Its Initial use 1n the field, the metering system
shall be calibrated according to the procedure outlined in APTD-0576.
Instead of physically adjusting the dry-gas meter dial readings to
correspond to the wet-test meter readings, calibration factors may be
used to correct the gas meter dial readings mathematically to the proper
values. Before calibrating the metering system, H Is suggested that a
leak-check be conducted. For metering systems having diaphragm pumps,
the normal Teak-check procedure will not detect leakages within the pump.
For these cases the following leak-check procedure Is suggested: Make a
10-mln calibration run at 0.00057 m3/m1n (0.02 cfm); at the end of the
run, take the difference of the measured wet-test and dry-gas meter
volumes and divide the difference by 10 to get the leak rate. The leak
rate should not exceed 0.00057 m3/m1n (0.02 cfm).
9.3.2 After each field use, the calibration of the metering system
shall be checked by performing three calibration runs at a single
Intermediate orifice setting (based on the previous field test). The
vacuum shall be set at the maximum value reached during the test series.
To adjust the vacuum, Insert a valve between the wet-test meter and the
Inlet of the metering system. Calculate the average value of the
calibration factor. If the calibration has changed by more than 51,
recalibrate the meter over the full range of orifice settings, as
outlined 1n APTD-0576.
9.3.3 Leak-check of petering system That portion of the samplJng
train from the pump to the orifice meter (see Figure 1) should be leak-
checked prior to Initial use and after each shipment. Leakage after the
pump will result In less volume being recorded than Is actually sampled.
The following procedure Is suggested (see Figure 6): Close the main
valve on the meter box. Insert a one-hole rubber stopper with rubber
tubing attached Into the orifice exhaust pipe. Disconnect and vent the
low side of the orifice manometer. Close off the low side orifice tap.
Pressurize the system to 13-18 cm (5-7 1n.) water column by blowing Into
the rubber tubing. Pinch off the tubing and observe the manometer for l
mln. A loss of pressure on the manometer Indicates a leak (n the meter
box. Leaks, if present, must be corrected.
NOTE: If the dry-gas-meter coefficient values obtained before and after
a test series differ by >5I, either the test series shall be
voided or calculations for test series shall be performed using
whichever meter coefficient value (I.e., before or after) gives
the lower value of total sample volume.
9.4 Probe heater: The probe-heating system shall be calibrated before
Us Initial use In the field according to the procedure outlined In APTD-0576.
Probes constructed according to APTD-0581 need not be calibrated If the
calibration curves 1n APTD-0576 are used.
0010 - 25
Revision
Date September 1986
-------
RUBBER ORIFICE
STOPPER
BY PASS VALVE
VACUUM
GAUGE
O
I
MAIN VALVE CLOSED
AIR TIGHT
PUMP
i/t O
e»
c*
Figure 6. Leah check ol meter box.
00
on
-------
9.5 Temperature gauges; Each thermocouple must be permanently and
uniquely marketTbn the casting; all mercury-ln-glass reference thermometers
must conform to ASTH E-l 63C or 63F specifications. Thermocouples should be
calibrated (n the laboratory with and without the use of extension leads. If
extension leads are used In the field, the thermocouple readings at ambient
air temperatures, with and without the extension lead, must be noted and
recorded. Correction 1s necessary If the use of an extension lead produces a
change >1.5X.
9.5.1 Implnger, organic «odule, and dry-gas meter thermocouples:
For the thermocouples used to measure the tenperature of the gas leaving
the 1mp1nger train and the XAO-2 resin bed, three-point calibration at
Ice-water, room-air, and boiling-water temperatures Is necessary. Accept
the thermocouples only if the readings at all three temperatures agree to
+Z*C (3.6*F) with those of the absolute value of the reference
thermometer.
9.5.2 Probe and stack thermocouple: For the thermocouples used to
indicate the probe and stack temperatures, a three-point calibration at
Ice-water, boiling-water, and hot-oil -bath temperatures must be
performed; It 1s recommended that room-air tenperature be added, and that
the thermometer and the thermocouple agree to within 1.51 at each of the
calibration points. A calibration curve (equation) may be constructed
(calculated) and the data extrapolated to cover the entire temperature
range suggested by the manufacturer.
9.6 Barometer; Adjust the barometer Initially and before each test
series to agree to within +-25 mm Hg (0.1 In. Hg) of the mercury barometer or
the corrected barometric pressure value reported by a nearby National Weather
Service Station (same altitude above sea level).
9.7 Triple-beam balance; Calibrate the triple-beam balance before each
test series, using Class-S standard weights; the weights roust be within +0.51
of the standards, or the balance must be adjusted to meet these limits.
10.0 CALCULATIONS
10.1 Carry out calculations. Round off figures after the final
calculation to the correct number of significant figures.
10.2 Nomenclature;
An » Cross-sectional area of nozzle, m2 (ft2).
• Water vapor In the gas stream, proportion by volume.
C
-------
La > Maximum acceptable leakage rate for a leak-check, either pre-test
or following a component change; equal to 0.00057 m3/m1n (0,02
cfm) or 41 of the average sampling rate, whichever Is less.
LI * Individual leakage rate observed during the leak-check conducted
prior to the "1tn" component change (1 « 1, 2, 3...n) m3/ni1n
(cfm).
In - Leakage rate observed during the post-test leak-check, m3/m1n
(cfm).
M{| * Stack-gas dry molecular weight, g/g-mole (Ib/lb-mole).
MH » Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-mole).
pbar • Barometric pressure at the sampling site, mm Hg (In. Hg),
Ps - Absolute stack-gas pressure, mn Hg (In. Hg).
Pstd * Standard absolute pressure, 760 mm Hg (29.92 In. Hg).
R - Ideal gas constant, 0.06236 an Hg-m^/K-g-mole (21.85 In.
Hg-ft3/'R-1b~nole).
Tm « Absolute average dry-gas meter temperature (see Figure 6), K
CR).
Ts • Absolute average stack-gas temperature (see Figure 6), K (*R).
Tstd • Standard absolute temperature, 293K (528'R).
Vic • Total volume of liquid collected In the organic nodule condensate
knockout trap, the 1rap1ngers, and silica gel, ml.
Vm a Volume of gas sample as measured by dry-gas meter, dscm (dscf),
vm(std) " Volume of gas sample measured by the dry-gas meter, corrected
to standard conditions, dscm (dscf).
vw(std) * Volume of water vapor In the gas sample, corrected to standard
conditions, sen (scf).
Vs * Stack-gas velocity, calculated by Method 2, Equation 2-9, using
data obtained from Method 5, ra/sec (ft/sec).
Wa • Weight of residue 1n acetone wash, rag.
1 m Dry-gas-meter calibration factor, dlaenslonless.
AH * Average pressure differential across the orifice meter (see
Figure 2), on HjO (1n. HjO).
0010 - 28
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^ - Density of water, 0.9982 g/mL (0.002201 Ib/mL).
B - Total sampling time, m1n.
8} =• Sampling time Interval from the beginning of a run until the
first component change, mln.
81 » Sampling time Interval between two successive component
changes, beginning with the Interval between the first and
second changes, mln.
Bp a Sampling time Interval from the final (n*h) component change
until the end of the sampling run, mln.
13.6 » Specific gravity of mercury.
60 * sec/mln.
100 a Conversion to percent.
10.3 Average dry-gas-meter temperature and average orifice pressure
drop; See data sheet (Figure 5, above).
10.4 Dry-gas volume! Correct the sample measured by the dry-gas meter
to standard conditions [20'C, 760 mm Hg [68*F, 29.92 In. HgJ) by using
Equation 1: -
Tstd Pbar * 4H/U'6 'bar
where:
0.3858 K/nn Hg for metric units, or
l7.64*R/1n. Hg for English units.
It should be noted that Equation 1 can be used as written, unless the leakage
rate observed during any of the mandatory leak-checks (I.e., the post-test
leak-check or leak-checks conducted prior to component changes) exceeds La.
If Lp or LI exceeds La, Equation 1 must be modified as follows:
a. Case I (no component changes made during sampling run): Replace vm
In Equation 1 with the expression:
vm -
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b. Case II (one or more component changes made during the sampling
run):Replace Vra 1n Equation 1 by the expression:
Vm ' (4 - La)8, - : (L, - L.JB, - (Lp - la).p
and substitute only for those leakage rates (LI or Lp) that exceed
10.5 Volume of water vapor;
vw(std) " vl
Pw RTstd
"w rstd
where:
K? « 0.001333 m3/«L for metric units, or
K2 " 0.04707 ft3/tL for English units.
10.6 Moisture content;
V
»s -
w(std)
B
NOTE; In saturated or Mater-droplet-laden gas streams, two calculation;
of the moisture content of the stack gas shall be made, one fror
the Inplnger analysis (Equation 3) and a second from the
assumption of saturated conditions. The lower of the two value;
of By, shall be considered correct. The procedure for determining
the moisture content based upon assumption of saturated condition;
Is given In the Note to Section 1.2 of Method 4. For the purpose;
of this method, the average stack-gas temperature from Figure <
may be used to make this determination, provided that the accuracj
of the in-stack temperature sensor is H*C (2*F).
10.7 Conversion factors;
Froi To Multiply by
P 0.02832
gr/ftj 15.43
Ib/ft* 2.205 x 10'3
g/«J 35.31
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10.8 Isoklnetlc variation:
10.8.1 Calculation froa raw data:
TOO Te[K,F,^ + (Vm/Tj (
s i ic mm
I (4)
where;
K3 = 0.003454 mm Hg-m3/mL-K for metric units, or
«3 = 0.002669 In. Hg-ft3/mL-'R for English units.
10.8.2 Calculation for Intermediate values:
TsVm(std)Pstd100
v TsVm(std>
4 P V A
where:
K4 » 4.320 for metric units, or
1(4 - 0.09450 for English units.
10.8.3 Acceptable results: If 90S £ I <; 1101, the results are
acceptable. If the results are ION In comparison with the standard and
I Is beyond the acceptable range, or If I Is less than 90S, the
Administrator may opt to accept the results.
10.9 To determine the minimum sample volume that shall be collected, the
following sequence of calculations shall be used.
10.9.1 From prior analysis of the waste feed, the concentration of
POHCs Introduced Into the combustion system can be calculated. The
degree of destruction and removal efficiency that 1s required Is used to
determine the maximum amount of POHC allowed to be present In the
effluent. This may be expressed as:
(WF) (POHC, cone) (100-IDRE)
. Max POHC, Mass (6)
100 100
where:
WF « mass flow rate of waste feed per hr, g/hr (Ib/hr).
POHC| * concentration of Principal Organic Hazardous Compound (wt I)
introduced Into the combustion process.
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ORE = percent Destruction and Removal Efficiency required.
Max POHC • mass flow rate (g/hr [lb/hr]) of POHC emitted from the
combustion source.
10.9.2 The average discharge concentration of the POHC In the
effluent gas Is determined by comparing the Max POHC with the volumetric
flow rate being exhausted from the source. Volumetric flow rate data are
available as a result of preliminary Method 1-4 determinations:
Max POHCj Mass
- Max TOHC1 cone (7)
DVeff(std)
where:
Dveff(std) ' volumetric flow rate of exhaust gas, dscm (dscf).
POHCi cone • anticipated concentration of the POHC In the
exhaust gas stream, g/dscm (Ib/dscf).
10.9.3 In making this calculation, it 1s recommended that a safety
margin of at least ten be Included:
LDLPOHC X l°
roHC1 cone
VTBC
where:
LOLpQHC " detectable amount of POHC 1n entire sampling train.
NOTE: The whole extract from an XAD-2 cartridge 1s seldom If ever,
Injected at once. Therefore, If allquotlng factors are
Involved, the IDLpgHC 1s not tnc sane as tne Analytical (or
column) detection limit.
•Inlmum dry standard volume to be collected at dry-gas
meter.
10.10 Concentration of any given POHC In the gaseous emissions of a
combustion process;
1) Multiply the concentration of the POHC as determined In Method 8270
by the final concentration volume, typically 10 mL.
CPOHC (ug/mL) x sample volume (ml) • amount (ug) of POHC In sample (9)
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where:
CPOHC " concentration of POHC as analyzed by Method 8270.
2) Sum the amount of POHC found In all samples associated with a single
train.
Total (ug) = XAQ-Z (ug) + condensate (ug) + rinses (ug) + 1mp1nger (ug) (10)
3) Divide the total ug found by the volume of stack gas sampled (m3).
(Total ug)/(tra1n sample volume) • concentration of POHC (ug/m3) (11)
11.0 QUALITY CONTROL
11.1 Sampling; See EPA Manual 600/4-77-027b for Method 5 quality
control.
H-2 Analysis; The quality assurance program required for this study
Includes theanalysis of field and method blanks, procedure validations,
Incorporation of stable labeled surrogate compounds, quantltatlon versus
stable labeled internal standards, capillary column performance checks, and
external performance tests. The surrogate spiking compounds selected for a
particular analysis are used as primary Indicators of the quality of the
analytical data for a wide range of compounds and a variety of sample
matrices. The assessment of combustion data, positive Identification, and
quantltatlon of the selected compounds are dependent on the Integrity of the-
samples received and the precision and accuracy of the analytical methods
employed. The quality assurance procedures for this method are designed to
monitor the performance of the analytical method and to provide the required
Information to take corrective action 1f problems are observed In laboratory
operations or In field sampling activities.
11.2.1 Field Blanks: Field blanks oust be submitted with the
samples collected at each sampling site. The field blanks Include the
sample bottles containing allquots of sample recovery solvents, unused
filters, and resin cartridges. At a mini BUB, one complete sampling train
will be assembled In the field staging area, taken to the sampling area,
and leak-checked at the beginning and end of the testing (or for the same
total number of tines as the actual test train). The filter housing and
probe of the blank train will be heated during the sample test. The
train will be recovered as If It were an actual test sample. No gaseous
sample will be passed through the sampling train.
11.2.2 Method blanks: A method blank must be prepared for each set
of analytical operations, to evaluate contamination and artifacts that
can be derived froa glassware, reagents, and sample handling In the
laboratory.
11.2.3 Refer to Method 8270 for additional quality control
considerations.
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12.0 METHOD PERFORMANCE
12.1 Method performance evaluation; Evaluation of analytical procedures
for a selectedseriesofcompounds must Include the sample-preparation
procedures and each associated analytical determination. The analytical
procedures should be challsnged by the test compounds spiked at appropriate
levels and carried through the procedures.
12.2 -Method detection limit; The overall method detection limits (lower
and upper)mustBedetermined on a compound-by-compound basis because
different compounds may exhibit different collection, retention, and
extraction efficiencies as well as Instrumental minimum detection limit (MDL).
The method detection limit must be quoted relative to a given sample volume.
The upper limits for the method must be determined relative to compound
retention volumes (breakthrough).
12.3 Me thod prec1s1 on and bias; The overall method precision and bias
must be determinedonIcompound-by-compound basis at a given concentration
level. The method precision value would Include a combined variability due to
sampling, sample preparation, and Instrumental analysis. The method bias
would be dependent upon the collection, retention, and extraction efficiency
of the train components. From evaluation studies to date using a dynamic
spiking system, method biases of -13X and -16X have been determined for
toluene and 1,1,2,2-tetrachloroethane, respectively. A precision of 19.91 was
calculated from a field test data set. representing seven degrees of freedom
which resulted from a series of paired, unsplked Semi volatile Organic Sampling
trains (Seml-voST) sampling emissions froa a hazardous waste incinerator*
13.0 REFERENCES
1. Addendum to Specifications for Incinerator Testing at Federal Facilities,
PHS, NCAPC, December 6, 1967.
2. Bursey, J., Homolya, J.f McAllister, R., and McGangley, J., Laboratory
and Field Evaluation of the Seml-VOST Method, Vols. 1 and 2, U.S.
Environmental Protection Agency, EPA/600/4-851/075A, 075B (1985).
3. Martin, R.M., Construction Details of tsoklnetlc Source-Sampling
Equipment, Research Triangle Park, NC, U.S. Environmental Protection Agency,
April 1971, PB-203 060/BE, APTD-0581, 35 pp.
4. Rom,, J.J., Maintenance, Calibration, and Operation of Isoklnetlc Source-
Samp Hng Equipment, Research Triangle Park, NC, U.S. Environmental Protection
Agency, March 1972, PB-209 OZ2/BE, APTD-0576, 39 pp.
5. Schllckenrleder, L.M., Mans, J.W., and Tnrun, K.E., Modified Method 5
Train and Source Assessment Sampling Systen: Operator's Manual, U.S.
Environmental Protection Agency, EPA/600/8-85/003, (1985).
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Date September 1986
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6. Shlgehara, R.T., Adjustments 1n the EPA Nonography for Different Pltot
Tube Coefficients and Dry Molecular Weights, Stack Sampling News, 2:4-11
(October 1974).
7, U.S. Environmental Protection Agency, CFR 40 Part 60, Appendix A, Methods
1-5.
8. Vollaro, R.F., A Survey of Comnerclally Available Instrumentation for the
Measurement of Low-Range Gas Velocities, Research Triangle Park, NC, U.S.
Environmental Protection Agency, Emissions Measurement Branch, November 1976
(unpublished paper).
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METHOD 0010, APPENDIX A
PREPARATION OF XAO-2 SORBENT RESIN
1.0 SCOPE AND APPLICATION
1.1 XAD-2 resin as supplied by the manufacturer is Impregnated with a
bicarbonate so-lutton to Inhibit mlcroblal growth during storage. Both thi
salt solution and any residual extractable monomer and polymer species must be
removed before use. The resin Is prepared by a series of water and organic
extractions, followed by careful drying.
2.0 EXTRACTION
2.1 Method 1; The procedure may be carried out 1n a giant Soxhlet
extractor.ArTaTT-glass thimble containing an extra-coarse frit 1s used for
extraction of XAO-2. The frit Is recessed 10-15 RIB above a crenellated ring
at the bottom of the thimble to facilitate drainage. The resin must be
carefully retained in the extractor cup with a glass-wool plug and stainless
steel screen because ft floats on methylene chloride. This process Involves
sequential extraction In the following order.
Solvent
Water
Water
Methyl alcohol
Methylene chloride
Methylene chloride (fresh)
2.2 Method 2;
Procedure
Initial rinse: Place resin 1n a beaker,
rinse once with Type II water, and
discard. Fill with water a second time,
let stand overnight, and discard.
Extract with H20 for 8 hr.
Extract for 22 hr.
Extract for 22 hr.
Extract for 22 hr.
2.2.1 As an alternative to Soxhlet extraction, a continuous
extractor has been fabricated for the extraction sequence. This extractor has
been found to be acceptable. The particular canister used for the apparatus
shown In Figure A-1 contains about 500 g of finished XAD-2. Any size may be
constructed; the choice 1s dependent on the needs of the sampling programs.
The XAD-2 1s held under light spring tension between a pair of coarse and fine
screens. Spacers under the bottom screen allow for even distribution of clean
solvent. The three-necked flask should be of sufficient size (3-Hter 1n this
case) to hold solvent
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DirdlUa Tafc*
i 032 cm Unfen
Cavu hit*
Pins
"^ma
mmm
w,:::w.;*.:
Huilnt Mantft
Figure A-l. XAD-2 cleanup extraction apparatus.
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equal to twice the dead volume of the XAD-2 canister. Solvent Is refluxed
through the Snyder column, and the distillate Is continuously cycled up
through the XAO-2 for extraction and returned to the flask. The flow 1s
maintained upward through the XAD-2 to allow maximum solvent contact and
prevent channeling. A valve at the bottom of the canister allows removal of
solvent from the canister between changes.
2.2.2 Experience has shown that 1t 1s very difficult to cycle
sufficient water In this mode. Therefore the aqueous rinse 1s accomplished by
simply flushing the canister with about 20 liters of distilled water. A small
pump may be useful for pumping the water through the canister. The water
extraction should be carried out at the rate of about 20-40 mL/n1n.
2.2.3 After draining the water, subsequent methyl alcohol and
methylene chloride extractions are carried out using the refluxIng apparatus.
An overnight or 10- to 20-hr period 1s normally sufficient for each
extraction.
2.2.4 All materials of construction are glass, Teflon, or stainless
steel. Pumps, if used, should not contain extractable materials. Pumps are
not used with nethanol and methylene chloride.
3.0 DRYING
3.1 After evaluation of several methods of removing residual solvent, a
flu1d1zed-bed technique has proved to be the fastest and most reliable drying
method. " ~
3.2 A simple column with suitable retainers, as shown In Figure A-2,
will serve as a satisfactory column. A 10.2-cm (4-1n.) Pyrex pipe 0.6 m (2
ft) long will hold all of the XAO-2 from the extractor shown In Figure A-l or
the Soxhlet extractor, with sufficient space for fluldlzlng the bed while
generating a minimum resin load at the exit of the column.
3.3 Method 1: The gas used to remove the solvent Is the key to
preserving the cleanliness of the XAO-2. Liquid nitrogen from a standard
commercial liquid nitrogen cylinder has routinely proved to be a reliable
source of large volumes of gas free from organic contaminants. The liquid
nitrogen cylinder 1s connected to the column by a length of precleaned 0.95-cm
(3/8-ln.) copper tubing, colled to pass through a heat source. As nitrogen Is
bled from the cylinder, It Is vaporized 1n the heat source and passes through
the column. A convenient heat source 1s a water bath heated from a steam
line. The final nitrogen temperature should only be warn to the touch and not
over 40*C. Experience has shown that about 500 g of XAO-2 may be dried
overnight by consuming a full 160-liter cylinder of liquid nitrogen.
3.4 Method 2: As a second choice, h1gh-pur1ty tank nitrogen may be used
to dry the XAD-2. The high-purity nitrogen must first be passed through a bed
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UquM Nltvf in
Cffindif
Figure A-2. Xfln-2 fluldtiedl-bsd drying apparatus,
0010 - A - 4
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of activated charcoal approximately 150 ml 1n volume, with either type of
drying method, the rate of flow should gently agitate the bed. Excessive
f1uld1ration may cause the particles to break up.
4.0 QUALITY CONTROL PROCEDURES
4.1 For_both Methods 1 and 2, the quality control results must be
reported for the batch. The batch must be reextracted 1f the residual
extractable organIcs are >20 ug/mL by TCO analysis or the gravimetric residue
1s >0.5 mg/20 g XAD-2 extracted. (See also section 5.1, Method 0010.)
4.2 Four control procedures are used with the ftnal XAD-2 to check for
(1) residual methylene chloride, (2) extractable organfcs (TCO), (3) specific
compounds of Interest as determined by GC/HS, as described 1n Section 4.5
below, and (4) residue (GRAV).
4.3 Procedure for residual methylene chloride;
4.3.1 Description: A 1+0.1-g sample of dried resin 1s weighed Into
a small vial, 3 ml of toluene are added, and the vial Is capped and well
shaken. Five uL of toluene (now containing extracted methylene chloride) are
Injected Into a gas chromatograph, and the resulting Integrated area 1s
compared with a reference standard. The reference solution consists of 2.5 uL
of methylene chloride In 100 nL of toluene, simulating 100 ug of residual
methylene chloride on the resin. The acceptable maximum content Is 1,000 ug/g
resin. .
4.3.2 Experimental: The gas chromatograph conditions are as
follows:
6-ft x l/8-1n. stainless steel column containing 10% OV-101 on
100/120 Supelcoport;
He Hun carrier at 30 mL/n1n;
FID operated on 4 x 10-" A/nV;
Injection port temperature: 250'C;
Detector temperature: 305*C;
Program: 30'C(4 rain) 40*C/m1n 250*C (hold); and
Program terminated at 1,000 sec.
4.4 Procedure for residual extractable orqanlcs:
4.4.1 Description: A 20+0.1-g sample of cleaned, dried resin 1s
weighed Into a precleaned alundum or cellulose thimble which Is plugged with
cleaned glass wool. (Note that 20 g of resin will fill a thimble, and the
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resin will float out unless well plugged.) The thimble containing the resin
Is extracted for 24 hr with 200-ml of pesticide- grade methylene chloride
(Burdlck and Jackson pesticide-grade or equivalent purity). The 200-ml
extract Is reduced 1n volume to 10-ml using a Kuderna-Danlsh concentrator
and/or a nitrogen evaporation stream. Five uL of that solution are analyzed
by gas chromatography using the TCO analysis procedure. The concentrated
solution should not contain >20 ug/mL of TCO extracted from the XAO-2. This
1s equivalent to 10 ug/g of TCO 1n the XAD-2 and would correspond to 1.3 mg of
TCO in the-extract of the 130-g XAD-2 module. Care should be taken to correct
the TCO data for a solvent blank prepared (200 nL reduced to 10 ml) in a
similar manner.
4.4.2 Experimental: Use the TCO analysis conditions described In
the revised Level 1 manual (EPA 600/7-78-201).
4-5 GC/HS Screen; The extract, as prepared 1n paragraph 4.4.1, 1s
subjected to GC/MS analysts for each of the Individual compounds of interest.
The GC/M5 procedure Is described In Chapter Four, Method 8270. The extract 1s
screened at the MDL of each compound. The presence of any compound at a
concentration >25 ug/tnL 1n the concentrated extract will require the XAD-2 to
be recleaned by repeating the methylene chloride step.
4.6 Methodology for residual gravimetric determination: After the TCO
value and GC/NS data are obtained for the resin batch by the above procedures,
dry the remainder of the extract In a tared vessel. There oust be <0.5 mg
residue registered or the batch of resin will have to be extracted with fresh
methylene chloride again until 1t meets this criterion. This level
corresponds to 25 ug/g In the XAO-2, or about 3.25 mg In a resin chaT-ge of
130 g.
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METHOD 0010, APPENDIX 8
TOTAL CHROHATOGRAPHABLE ORGANIC MATERIAL ANALYSIS
1.0 SCOPE AND APPLICATION
1.1 In this procedure, gas chromatography 1s used to determine the
quantity of lower boiling hydrocarbons (boiling points between 90* and 300*C)
in the concentrates of all organic solvent rinses, XAO-2 resin and LC
fractions - when Method 1 Is used (see References, Method 0010) - encountered
In Level 1 environmental sample analyses. Data obtained using this procedure
serve a twofold purpose. First, the total quantity of the lower boiling
hydrocarbons 1n the sample 1s determined. Then whenever the hydrocarbon
concentrations in the original concentrates exceed 75 ug/m3, the
chromatography results are reexamlned to determine the amounts of Individual
species.
The extent of compound Identification Is limited to representing all
materials as normal al(canes based upon comparison of boiling points. Thus the
method 1s not qualitative. In a similar manner, the analysis Is
semiquantitative; calibrations are prepared using only one hydrocarbon. They
are replicated but samples routinely are not.
li2 Application; This procedure applies solely to the Level 1 C7-C16
gas chromatographfc analysis of concentrates of organic extracts, neat
liquids, and of LC fractions. Throughout tht procedure, 1t 1s assumed the
analyst has been given a properly prepared sample.
1.3 Sensitivity; The sensitivity of this procedure, defined as the
slope of aplotof response versus concentration, Is dependent on the
instrument and must be verified regularly. TRW experience Indicates the
nominal range 1s of the order of 77 uV*V*sec*uL/ng of n-Nptane and 79
uV-sec-ul/ng of n-hexadecane. The Instrument Is capable ;f perhaps one
hundredfold greater sensitivity. The level specified here 1s sufficient for
Level 1 analysis.
1.4 Detection limit; The detection Unit of this procedure as written
1s 1.3 ng/uL for a I «C Injection of n-decane. This Unit 1s arbitrarily
based on defining the •Inlnni detectable response as 100 uvsec. This is an
easier operational definition than defining the •Inlmua detection limit to be
that amount of material which yields a signal twice the noise level.
1.5 Range; The range of the procedure will be concentrations of 1.3
ng/uL and greater.
1.6 Limitations
1.6.1 Reporting limitations: It should be noted that a typical
environmental sample will contain compounds which: (a) will not elute m
the specified boiling ranges and thus will not be reported, and/or (b)
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will not elutt from the column at all and thus win not be reported.
Consequently, the organic content of tht saiple as reported Is a lower
bound and should be regarded as such.
1.6.2 Calibration limitations: Quantnation 1s based on
calibration with n-decane. Data should therefore be reported as, e.g.,
mg C8/m3 as n-decane. Since response varies linearly with carbon number
(over a wide range the assumption may Involve a 201 error), 1t Is clear
that heptane (C7) detected in a sample and quantltated as decane will be
overestimated. Likewise, hexadecane (C16) quantttated as decane will be
underestimated, from previous data, H 1s estimated the error Involved
Is on the order of 6-71.
1.6.3 Detection limitations: The sensitivity of the name
lonlzatlon detector varies from conpound to compound. However, n-alkanes
have a greater response than other classes. Consequently, using an ri-
al kane as a call brant and assuming equal responses of all other compounds
tends to give low reported values.
2.0 SUMMARY OF METHOD
2.1 A art. aliquot of all 10-«L concentrates Is disbursed for GC-TCO
analysis. With boiling point-retention tine and response-amount calibration
curves, the data (peak retention tlaes and peak areas) are Interpreted by
first sunning peak areas in the ranges obtained froa the boiling point-
retention tine calibration. Then, with tht response-amount calibration curve,
the area sums are converted to amounts of material 1n the reported boiling
point ranges.
2.2 After the Instrument Is stt up, the boiling point-retention time
calibration 1s effected by Injecting a mixture of n-C7 through n-C16
hydrocarbons and operating the standard temptrature program. Response-
quantity calibrations art accomplished by Injecting n-decane In n-pentane
standards and performing the standard temperature program.
2.3 Definitions
2.3.1fiC: Gas chromatography or gas chromatograph.
2.3.2 C7-C16 n-alkanes: Heptane through htxadecane.
2.3.3 GCA temperature program: 4 m1n Isothermal at 60'C, lO*C/m1n
froti 60* to 220'C.
2.3.4 TW temperature program: 5 n1n Isothermal at room
temperature, then program from 30*C to 250*C at !5*C/m1n.
3.0 INTERFERENCES
Not applicable.
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4.0 APPARATUS AND MATERIALS
4.1 Gas chroroatpgraph; This procedure 1s Intended for use on a VaMan
1860 gas chromatograph, equipped with dual flame 1on1zat1on detectors and a
linear temperature programmer. Any equivalent Instrument can be used provided
that electrometer settings, etc., be changed appropriately.
4.2 Gases;
4.2.1 Helium: Minimum quality Is reactor grade. A 4A or 13X
molecular sieve drying tube 1s required. A filter must be placed between
the trap and the Instrument. The trap should be recharged after every
third tank of helium.
4.2.Z Air: Zero grade Is satisfactory.
4.2.3 Hydrogen: Zero grade.
4-3 Syringe; Syringes are Hamilton 701N, 10 uL, or equivalent.
4.4 Septa; Septa will be of such quality as to produce very low bleed
during the temperature program. An appropriate septum Is Supelco Wcrosep
138, which Is Teflon-backed. If septum bleed cannot be reduced to a
negligible level, It will be necessary to Install septum swingers on the
Instrument.
4.5 Recorder: The recorder of this procedure must be capable of not
less than I mV full-scale display, a 1-sec time constant and 0.5 in. per mln
chart rate.
4.6 Integrator; An Integrator Is required. Peak area measurement by
hand Is satisfactory but too time-consuming. If manual Integration Is
required, the method of "height tines width at half height" Is used.
4.7 Columns;
4.7.1 Preferred column: 6 ft x 1/8 In. 0.0. stainless steel column
of 10X OV-101 on 100/120 mesh Supelcoport.
4.7.2 Alternate column: A ft x 1/8 In. 0.0. stainless steel column
of 10X OV-1 (or other silicon phase) on 100/120 mesh Supelcoport.
4.8 Syringe cleaner; Hamilton syringe cleaner or equivalent connected
to a suitable vacuum source.
5.0 REAGENTS
5.1 Pentane; "01 stilled-In-Glass" (reg. trademark) or -Nanograde' (reg.
trademark) for standards and for syringe cleaning.
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5.2 Kethylene chloride; "Distilled-1n-Glass" (reg. trademark) or
"Nanograde"(reg. trademark) for syringe cleaning.
6.0 SAMPLING HANDLING AND PRESERVATION
6.1 The extracts are concentrated In a Kuderna-Qanlsh evaporator to a
volume less than 10 mL. The concentrate 1s then quantitatively transferred to
a 10-mL volumetric flask and diluted to volume. A 1-mL aliquot Is taken for
both this analysis and possible subsequent GC/NS analysis and set aside In the
sample bank. For each GC-TCO analysis, obtain the sample sufficiently In
advance to allow It to warm to room temperature. For example, after one
analysis Is started, return that sample to the sample bank and take the next
sample.
7.0 PROCEDURES
7.1 Setup and checkout:
following:
Each day, the operator will verify the
7.1.1 That supplies of carrier gis, air and hydrogen are
sufficient, I.e., that each tank contains > 100 pslg.
7,1.2 That, after replacement of any gas cylinder, all connections
leading to the chromatograph have been leak-checked.
7.1.3 That the carrier gis flow rite 1i 30 * 2 nL/raln, the hydrogen
flow rate Is 30 + 2 rat/mln, and tht air flow rate~1s 300 + 20 ittL/raln.
7.1.4 That the electrometer Is functioning properly.
7.1.5 That the recorder and Integrator are functioning properly.
7.1.6 That the septa have been leak-checked (leak-checking Is
effected by placing the soap bubble flow meter Inlet tube over the
Injection port adaptors), and that no septum will be used for more than
20 Injections.
7.1.7 That the list of sanples to be run Is ready.
7,2 Retention tlae calibration;
7.2.1 To obtain the temperature ranges for reporting the results of
the analyses, the chromatograph Is given a normal boiling point-retention
time calibration. The n-alkanes, their boiling points, and data
reporting ranges are given In the table below:
0010 - I - 4
Revision 0
Date September 1986
-------
NBP.'C Reporting Range,*C ReportAs
n-heptane 98 90-110 C7
n-octane 126 110-140 C8
n-nonane 151 140-160 C9
n-decane 174 160-180 CIO
n-undecane 194 180-200 Cll
n-dodecane - 214 200-220 C12
n-trldecane 234 220-240 C13
n-tetradecane 252 240-260 C14
n-pentadecane 270 260-280 CIS
n-hexadecane 288 280-300 C16
7.2.2 Preparation of standards: Preparing a mixture of the C7-C16
alkanes Is required. There are two approaches: (1) use of a standards
kit (e.g., Polysclence Kit) containing bottles of mixtures of selected ri-
al kanes which may be combined to produce a C7-C16 standard; or (2) use of
bottles of the Individual C7-C16 alkanes fro* which accurately known
volumes may be taken and combined to give a C7-C16 mixture.
7.2.3 Procedure for retention time calibrations This calibration
Is performed at the start of an analytical program; the mixture Is
chromatographed at the start of each day. To attain the required
retention time precision, both the carrier gas flow rate and the
temperature program specifications must be observed. Details of the
procedure depend on the Instrument being used. The general procedure 1s.
as follows:
7.2.3.1 Set the programmer upper limit at 250*C. If this
setting does not produce a column temperature of 250'C, find the
correct setting.
7.2.3.2 Set the programmer lower limit at 30*C.
7.2.3.3 Verify that the Instrument and samples are at room
temperature.
7.2.3.4 Inject 1 uL of the n-alkane mixture.
7.2.3.5 Start the Integrator and recorder.
7.2.3.6 Allow the Instrument to run Isothermally at room
temperature for five mln.
7.2.3.7 Shut the oven door.
7.2.3.8 Change the mode to Automatic and start the temperature
program.
7.2.3.9 Repeat Steps 1-9 a sufficient number of times so that
the relative standard deviation of the retention times for each peak
is <5I.
0010 - B - 5
Revision 0
Date September 1986
-------
7.3 Response calibration:
7.3.1 For the purposes of a Level 1 analysis, response-quantity
calibration with n-decane Is adequate. A 10-uL volume of n-decane is
Injected Into a tared 10 ml volumetric flask. The weight Injected 1s
obtained and the flask Is diluted to the mark with n-pentane. This
standard contains about 730 ng n-decane per uL n-pentane. The exact
concentration depends on temperature, so that a weight 1s required. Two
serial tenfold dilutions are made from this standard, giving standards at
about 730, 73, and 7.3 ng n-decane per uL n-pentane, respectively.
7.3.2 Procedure for response calibration: This calibration is
performed at the start of an analytical program and monthly thereafter.
The most concentrated standard 1s Injected once each day. Any change In
calibration necessitates a full calibration with new standards.
Standards are stored 1n the refrigerator locker and are made up monthly.
7. 3. Z.I Verify that the Instrument is set up properly.
7.3.2.2 Set electrometer at 1 x 1CT10 A/mV.
7.3.2.3 Inject 1 uL of the highest concentration standard.
7.3.2.4 Run standard temperature program as specified above,
7.3.2.5 Clean syringe.
7.3.2.6 Make repeated Injections of all three standards until
the relative standard deviations of the areas of each standard are
7.4 Sample analysis procedure;
7.4.1 The following apparatus 1s required:
7.4.1.1 Gas chroaatograph set up and working.
7.4.1.2 Recorder. Integrator working.
7.4.1.3 Syringe and syringe cleaning apparatus.
7.4.1.4 Parameters: Electrometer setting ts 1 x 1Q-1° A/mV;
recorder is set at 0.5 1n./«1n and 1 mV full -scale.
7.4.2 Steps In the procedure are:
7.4.2.1 Label chromatogram with the data, sample number, etc.
0010 - S - 6
Revision
Date September 1986
-------
7.4.2.2 Inject sample.
7.4.2.3 Start Integrator and recorder.
7.4.2.4 After Isothermal operation for 5 mln, begin
temperature program.
7.4.2.5 Clean syringe. lf
7.4.2.6 Return sample; obtain new sample.
7.4.2.7 When analysis Is finished, allow Instrument to cool.
Turn chromatogram and Integrator output and data sheet over to data
analyst.
7.5 Syringe cleaning procedure;
7.5.1 Remove plunger from syringe.
7.5.2 Insert syringe Into cleaner; turn on aspirator.
7.5.3 Fill plpet with pentane; run pentane through syringe.
7.5.4 Repeat with methylene chloride from a separate plpet.
7.5.5 Flush plunger with pentane followed by methylene chloride.
7.5.6 Repeat with nethylene chloride.
7.6 Sample analysis decision criterion*. The data from the TCO analyses
of organic extract andrinseconcentrates are first used to calculate the
total concentration of C7-C16 hydrocarbon-equivalents (Paragraph 7.7.3) 1n the
sample with respect to the volume of air actually sampled, I.e., ug/m3. On
this basis, a decision Is made both on whether to calculate the quantity of
each n-alkane equivalent present and on which analytical procedural pathway
will be followed. If the total organic content 1s great enough to warrant
continuing the analysis -- >500 ug/a3 -- a TCO of less than 75 ug/m3 will
require only LC fractlonatfon and gravimetric determinations and IR spectra to
be obtained on each fractton. If the TCO 1s greater than 75 ug/ra3, then the
first seven LC fractions of each sample will be reanalyzed using this same gas
chromatographlc technique.
7.7 Calculations;
7.7.1 Boiling Point - Retention Time Calibration: The required
data for this calibration are on the chromatogram and on the data sheet.
The data reduction is performed as follows:
7.7.1.1 Average the retention times and calculate relative
standard deviations for each n-hydrocarbon.
0010 - B - 7
Revision
Date September 1986
-------
7.7.1.2 Plot average retention times as abscissae versus
normal boiling points as ordlnates.
7.7.1.3 Draw 1n calibration curve.
7.7.1.4 Locate and record retention times corresondlng to
boiling ranges 90-100, 110-140, 140-160, 160-180, 180-200, 200-220,
220-240, 240-Z60, 260-280, 280-300'C.
7.7.2 Response-aaount calibration: The required data for this
calibration are on the chromatogram and on the datasheet. The data
reduction Is performed as follows:
7.7.2.1 Average the area responses of each standard and
calculate relative standard deviations.
7.7.2.2 Plot response (uvsec) as ordlnate versus ng/uL as
abscissa.
7.7.2.3 Draw in the curve. Perform least squares regression
and obtain slope (uV-sec-uL/ng).
7.7.3 Total C7-C16 hydrocarbons analysis: The required data for
this calculation are on the chromatogran and on the data sheet. The data
reduction Is performed as follows:
7.7.3.1 Sun the areas of all peaks within the retention"time
range of Interest.
7.7.3.2 Convert this area (uV-sec) to ng/uL by dividing by the
weight response for n-decane (uV-sec.uL/ng).
7.7.3.3 Multiply this weight by the total concentrate volume
(10 ml) to get the weight of the C7-C16 hydrocarbons In the sample.
7.7.3.4 Using the volume of gas sampled or the total weight of
sample acquired, convert the result of Step 7.7.3.3 above to ug/tn3.
7.7.3.5 If the value of total C7-C16 hydrocarbons from Step
7.7.3.4 above exceeds 75 ug/m3, calculate Individual hydrocarbon
concentrations In accordance with the Instructions In Paragraph
7.7.5.5 below.
7.7.4 Individual C7-C16 n-AUane Equivalent Analysis: The required
data from the analyses are on the chromatogram and on the data sheet.
The data reduction Is performed as follows:
7.7.4.1 Sun the areas of peaks In the proper retention time
ranges.
0010 - B - 8
Revision
Oate September 1986
-------
7.7.4.2 Convert areas (uV-sec) to ng/uL by dividing by the
proper weight response (uV-sec-uL/ng).
7.7,4.3 Multiply each weight by total concentrate volume (10
ml) to get weight of species In each range of the sample.
7.7.4.4 Using the volume of gas sampled on the total weight of
sample acquired, convert the result of Step 7.7.4.3 above to ug/m3.
8.0 QUALITY CONTROL
8.1 Appropriate QC 1s found in the pertinent procedures throughout the
method.
9.0 METHOD PERFORMANCE
9.1 Even relatively comprehensive error propagation analysis 1s beyond
the scope of this procedure. With reasonable care, peak area reprodudbtHty
of a standard should be of the order of IS RSD. The relative standard
deviation of the sun of all peaks in a fairly complex waste might be of the
order of 5-101. Accuracy Is more difficult to assess. With good analytical
technique, accuracy and precision should be of the order of 10-20*.
10.0 REFERENCES
1. Emissions Assessment of Conventional Stationary Combustion Systems:
Methods and Procedure Manual for Sampling and Analysis, Interagency
Energy/Environmental RU) Program, Industrial Environmental Research
Laboratory, Research Triangle Park, NC 27711, EPA-600/7-79-029a, January 1979.
0010 - B - 9
Revision
Date September 1986
-------
APPENDIX J,5
CEM AND GC
-------
PI. M, App. A,
II
Sampling Equipment environmental Pro
lection Agency. Reaearrlt Tflanalr Park,
N C APTD OAW. March, toil
t Smith. W a.. R T. Bhlgrhara. and W
P Todd A Method ol Interpreting Start
Sampling Data. Paper Prevented at lhe llrd
Annual Meeting of the Air Pollution Con
Iral AmocutUon. St. lAuia. Mo. June It ID.
in*.
• amlth, W. 8.. et al. Black «** Sampling
Improved and BlmpUfM with Mr* Kquitt-
ment APCA Paper Mo. tl-ill, IM7.
• EtoedllcaUon* lor IneineraUv Toting at
Federal PacUnvnv PHB. HCAPC. IVtl.
1. Bhlgehar*, K T.. Adjualmenla In UM
•PA Nomograph lor DUIerrnl Pilot Tube
Coel'tctmt* ami Dry Molecular Weight*
rAac*. •—f"-f "«*» I* It. October. I*M.
I. Vollaro. R. r.. A Barmy of Commercial
ly AraUafakt liMn^nlilhai fat the HMO-
mimLiil of Urn Range Oaa VetodUea US
mrtr nrva»mtil ProtacUon Agency.
Rcacmrch
IVM 41
L of AST* Standard! Part
I Daft*: AlavflB-
i BarMy for Teat
PhUadctpru*. Pa. |g1«
PP tll-wSI.
I*. VoUaro,
dun for i
II InclMa In
Protect*)*! Agency,
jch Triangle Park.
N.C.
MHIIM* It— MauuaoiKVT or Qtunot O»-
g*WlC CXMErOOW* BMlBBIOM IT OM
CmOwmraBmofWl
fftfmtfBeMoa
• IwBi Mill nil ahnuld not tie attempted by
!•!••» imlamlllpr with UM pwlormanet
cbanettHaUoi of «•* clWMMM«rapli». nor
br UMM peram vho m unfumte
rilB|. Pulicutaf emre
UM ucs ol vfclv
40 Cra Ch. i (» I M CdMlon)
I lir ma|or organh- rrmfMuirnlJi nt a iu
mliiurr are: fte|**r*ir. but an cape-
rlenccd OC operator Mlh a reliable Imtru-
mem can readily achieve t peroenl KBD
Par trite method, the folloirlng comMned
OC/optnlai raluea an required
lal Prertalon. DuplloUc analyaea art
within • prrotnl of Ihdr mean value.
(bl Accuracy Analywa rawulu of prepared
i am wlUiln It percenl of prep
Thte awthod appllea to
•• ovroenl of
from an
II i
lo IdcnUIr
bulkttr« air and
Ttote MBUWd. Mil MM drlemtne tarn
ir-fft^f thai i I ' arc mlynMrlc (lilili nolecii-
lar *H«htl, 111 cam polymerise be lore anal* •
•ta. or III ham very to* «apo< preamrei at
•tack or InatruncM condlilanB.
I 1 Principle
taUrlfrracf* inai «=»)• occur
dtadnaMd by apfiroprlate OC
and detector cftok* or by •nilllnf
the retention Una Ihrouch ctianfa In Ihf
flow ral« and ine uae ol tempera-
ture prog rmmmlnt
The analyUcal »mm to detnonUraied u>
toe raaenllally free fnm conlamlnanu by P*
rtodfcally wtalyiinM blwdu thai cimit*! "'
hydrocarbon Ire* air or nltraaen.
Hamplr crow conUrolrmllon thai orcim
•hen high l*»rl and lo* level uumtlri <>'
uaiuterdt are analyied •lurri.iriy n >"••'
drall «llh by lharou«h puriln* of lhe CIC
•wnple loop belveen lunptom
To anure ronibitrnt drteeUw rmponie,
olibrktlun iun are cnnUtlnml In dry air.
To id |u»l (urou* oriuik- mncmlratloiu
•hen Baler «apor U prevent In the munplt.
••l«r oafior cnnrrnlrallona are determined
lot thoa«> uunpln. and a correction factor It
applied
t Prrimrurt aad Pfcmniry Samtplimg
frrlarm a praurvey lor rmch «ource lo be
lestm. Refer la PlftiK !• I. Batnt at the In
lartnallon can be collected from literature
survey* and wxirce penonnel. Collect ea*
aunplfa thai can be analymcd la confirm the
Idrnlltla and appioilmale conccntrallom
ol ine omanJc rtntaiam
ft. I Apparalu*. Thla apparatiia Hti atoo
•ppllei to Sectlona • and 1.
B.I.I Teflon Tublna. IMenUon of trade
nanea or weciflc producu doca not curtail
ml* mdo»«en>enl by the U.B, •milronnien-
lal Protection Aiency > Diameter and
length determined by connection require
mtnlM of cylinder rcfulaton and the OC.
AddltlonaJ Itifefni ii neceaaary to connect
UM OC aamole loop ID the cample.
Ill Qaa ChnHnatof rapti. OC Mlh aulla-
He detector, column*, tcnapetmlure-can-
Ifolled aample loop and valve uaembly. mmt
teBperature proiramabhr oven. If nrrraiiir
The OC inall achieve aenalUvlly require
menu for lhe compound! under itudy.
« l.i Pump CajMble of oumplna 10* ml/
Mn, r\w M«tthtn« aamnie loop
• If Wowrn*l*n To meaaure flow rates
ft IB Regulaum. Uaed on IM cyllndera
lor (K: and for cylinder Mandar*.
» I • Hecnrder. Mttnrder Mth linear atrip
chart la minimum acceptable Intearaiof
(optional I b) recananendod.
».l 1 flyrliwea *B ml. I a- and 10 micro
Uler *t*e». calibrated. maiUmon amiracy
(|or preparation ol iu Mandajdi.
^ ^ Ift • Sample ftmMk* t4ir iircvurvey tain-
»l'i, U|fM have IM I If in wala
% I I* Adnrptlnn f>ib<-« II nerraary.
wlin iitrrstaty adaurbpnl
ff. *0. App. A, MMk. It
, Trn«i. RAD J. tlf I lot praur
IT f oamplra
S 1.1*1 Prnonncl SarnMlrai Pump. Call-
braled, lor mUrctlna adiurbent tube preaur-
S.I II Dilution Syilem, Calibrated, the
dilution tyilern U U> be enngtructed follow
ing the apedffrBilorui of an acceptable
method
S.I.It Sample Probei Pyrei or ililnUm
iteel. ol *ulllrleiil length to reach ccntroU
ol itach. m a point no clnaer to lhe walla
lhan I m.
ft I W Baromrier To meaiure barometric
premure.
S.I Keagenu.
A I.I Octontenf Ouilflet! Witer
S.l.a Methylene IMchlotlde.
i.l J Calibration Oaan. A »crte» ol Hand
ard! prrpuet] lor every compound of Inlcr-
ett.
S.lt Organic Compound Boiullona. Pure
(Ml percent), or aa pure a* can reaaonably
be aMalned. liquid vamplea ol all the organ-
ic compound* needed to prepare calibration
itandardi.
B.l.ft Eitrartlon Solvent*. Por eatractlon
ol adHtrbenl tube aamplec In preparallon
for analyala.
l.ll Puel. Af rrcornmemlnl by lhe man-
ufacturer lor operation of the OC.
ft.1.1 Canler da*. Hydrocarbon free, ai
recommended by lhe manufacturer for op-
eration of the dHector and oompaianlllty
•llh th« column.
B.I.I Zero Oaa. Hydrocarbon tree air or
nitrogen, to be turd for dilution*, bluu
preparation, and *landard prrparUton
61 Sampling
t.l.l Concction ol fUmpWa with Olam
fiampllng Pteik*. Preaurvep rnrnnki can be
collected In precleaned IM-ml doutrfc ended
flao sampling flaifc*. Teflon atopmrt*.
vilhoMt greace. are preferred. Pla*k* should
be cleaned u folio**: Remove lhe aloptnrta
from both end! of the Hack*, and »ipe the
paru U> remote any greaee. Clean the Hop-
cock*, barrel*, and receiver! with methylem
diehlorMe, Clean all ilam port* with a aoap
•olullan. then rlnac with tap and drummed
dMHIed waler. Place lhe flavfe In a cool
flam annealkng furnace and apply heal up
lo Mo' C. Maintain at Ihte lemperalurT lor
I hour Alter thia time period, artut off and
open the lurnace la allow lhe flaafe to cool.
(ireue lhe Moecocta MUi tlin**~* greaae
and return them la the flaat receiver*.
Purge I he BBWrnbly with high purity nliro
grit fur I to ft minute*. Ctaae off the ilop
rorlu after purging U> raalnlaln a illght
poalllvc nitrogen prraaure. Secure lhe Mop
rnru "Ufi tape
Prriurvry *amule> can be obtained r liner
by rtravlng Ihr ca*e* into lhe prevloualr
e**d'u*le«l llaok tti Uy dravlrtg the §••<*• Into
008
669
-------
and purging Ihr flam* «Uh t rubbrr siirllnn
bulb
>J I.I Evacuated MA*B. Procedure Use a
high vacuum pump In r»arual* the flask lo
Ihr rapacity ol Ihr IHimp, Ihrn close oil Ihc
•laprjark leading lo the pump Atlaeh • 8
mm ouUMr diameter (OUI glass Irr In Ihr
flask Inkpl with * (hart piece of Tcllon
tubing. Select • ••mm OD boroatlicale ssm
pllni prate, enlarged si onr end lo • 13 mm
OD and of sufficient length to reach Ihe
crntrotd ol the duel to br sampled Insert a
glasa wool plug In the enlarged end ol HIT
probe lo lanove paniculate matter Attach
in* other end of the probe to the le* with •
short ptrcr ol Tenon tubing. Conner! a
rubbrr auction bulb to the third In ol Ihr
lr* Place the flllei end o> the probe at the
ccnlroM of Ihe duct, or at • point no closer
lo the walls than I m. and puree Ihr probe
with the rubber iurUon bulb. Alter the
probe ta complrtrlr purged and (Hied with
duct IBM*, open ihc stopcock to ihr grab
flask until Ihr pressure In the flask reaches
duct piisaurr. Cloar off the iloproca. and
remote the probe from ihr duel- Remove
Ih* Ice Irorn the flwft and tape the stop-
cock* to piewenl teaks during shipment.
Measure and record U*e duct lerrtDerslurr
and pressure.
83.1.1 Purged Pla*t Procedure. Attach
one end of the sampling flank to • rubbrr
suction bulb. Attach the other rnd lo • fl
mm OD flam probe H described In Section
S.J.I.I. Place Ihr Illler rnd ol Ihr probe at
the centroM ol thr durl. or at a polnl no
clover lo the wills than I m. and apply luc-
lion vllh thr bulb to completely purge the
probe and (lad Alter thr flask has been
purged, close oil the stopcock near the sue-
lion bulb, antf then close Ihr stopcock near
the probe. Remove the probe from thr duct,
and disconnect both Hie probe and auction
bulb. Tape the Hancocks lo prevent leakage
durlni ahlpntent, Measure and record the
durl temperature and prevail!*,
6.1.3 PtealMe Bat Procedure. Trdlar or
alumlntaed Mylar baca ran also be used lo
obtain the preaurvcy samule. U*e new bags,
and Ink Chech them before lield use. In ad
dttlon. check the bag before use for con
lamination by filling II with nitrogen or air.
and analysing the gas bf OC at high sensi-
tivity. Esperience Indicates that II Is desira-
ble lo allow the Inert gas to remain In the
bag about M hour* or longer to check for
desorptlon ol organic* from thr bag, Polio*
the lea*. Chech and ample collection proce-
dure* given In Section 7.1.
BJJ Determination ul Moisture Content.
Por combustion or water controlled proeeas-
em, nMabi the mofcUurr content from plant
peraotinel or bf mrasurrmrnl during the
presurvev. II Ihr immrr Is brlna SO" C,
measure thr wrl bulb and dry bulb tempera-
turei. and calculate HIP moisture ronlr.nl
uilng a piychromrtrir rlmrt. At lilniirr tern-
|H-rtliiri'S, ll.w Mclhtwl * in rtrlrrmliir Ihr
rmilsturr ronlrnl.
&* Drlrrmliiallmi ul .Slalir f*rr»i
llhialn Ihr ilailr prruturf ftnm llir plan!
lirrsonnrl or mrajiiirrrnrnl. II a I JDT 8 ptlix
liibr and an Inrllrird manomrler arr uird,
lakr rare lo align ihr iillnl lube SO from
thr dlrrrllon of llir flow. Dlsronrn-cl one pi
Ihr I uba lo the tnanomHrr. ind read ihr
llallc premnure: note whether till! irradlug If
po&llivr or n«gatl*e.
9.S Coll«-llon of Prrsurvry fUmpIri «Hh
Attvorpllnn Tubr Polio* Rrrllon 1 I for pri-
inr>ry aampllng.
g. I arlectlon of Of; Parameter*.
0, 1 . 1 Column Chok*. Baicd on I he Initial
contact with plant prraonnel mncrrnlng thr
plant procem* and the anllrlpalrd rmbatom.
choaae a column that pro»klri good reaolu
lion and rapid analvils time. Thr choice ol
an appropriate column ran be aided by a III
rralurr ararrh. eonlacl with manufarlurrrs
ol 11C column*, and dbjcumton with permn
nel al the embwion source,
Matt column mmnufactureri keep rmfft-
knl recorda of their pmdueU. Their lerhnl
ral service defawlmenlg mar be. able lo rec-
ommend appropriate columns and detector
Ivor for irparallng the anllclpated com
pound*, and they may be able lo provide In
formation on Intrrlerrarei, optlmtim ocw-r
ailng condition!, and column limitations
Plan) I with analytical libnralortra may
also be able to provide Information on ap
proprlale analrlk-al procedurri.
813 Preliminary UC Adliulmrnl Uilrn
the standard! and column obtained In Sec-
tion nil. perform Initial imls ID determine
appropriate OC conditions that provide
good resolution and minimum analysts Urn*
for the eompoundB ol Internl.
g.l.l Preparation of Preiurvey I3amp4«»
If the samples were collected on art adsorb-
ent, eitracl the sample as reeomrnrmled by
the manufacturer for removal of the com
pounds with a anltml sulLablr to Hie Ijff
of OC analvmta Prepare other •ampin In an
appropriate manner,
t.1,1 Premunrry Sample Analyioi. Before
analysli. heal the preaurvcy sample u> the
duel temperature Ui *a|>orlzr any condrnaed
mslrrlsl An si Kit the aamplea by the OC
procedure, and compare the retrnlion I Intel
against thow of ihr calibration aamplrs
that contain the curnponenla tsprrled lo br
In thr stream. If any compounds n.nrmi br
IdrnlllM with certainly by tills procedure,
Identify them by other mraiu sucli as tit"/
hi ana ipeclraacop* IQC/MS) »r UC/lnfrired
techniques, A OCYMS lyilein is recom-
mended.
Use Ihr OC conditions iti'lrrmlni'fl by llir
l>rocrdiiri*s of Si-rUon HI, 'I for ilu Mrsl in-
jection, Vary ihr (1C uaramrti-r!* durlnl
lubseqiirnl Injeclluiis to di'lcrmlm- llir n|Hl
m,im u-Mliigx Once Ihr orilimiim
|ia*r l«e«i ,lrl. rml.i. rl iirliorm repeal I«|IT
llnn.1 of llir samplr In rtrlrrmltw llir rrlrn
I Inn Umr- cil rarh ronipniind Tn ln|«-l a
samuir. rtra« itamplr Ilirough the loop al a
mrulant ralr i IOO ml/mill lor JO aeeond»»-
Hr rrsrrftil nol to prrsa«irli« Hie ia» In mr
loop. Turn off the pump and allow the gas
In ihr, sample loop to come lo ambtertl pres^
,,irr Arilvslr tlie sample *alve. and record
inlecllon Umr. loop temperature, eolumrt
Irmprrsl.irr carrier flow rale, eliarl apeed,
and attenuator »eUlng, Calculate the reten
lion lime of racli peak using the distance
from Inrn I to the peak maslmiim dlvW
rd b» the , hart speed- ReWnUon Ume»
ihould be repeatabte within 0.1 aecotidi.
II the concenlratlona are loo high lor ap
proprlatr detector reaponse, a smaller
sample loop or dllullom may be use* lor gas
sample*, and. lor IHuW aamples. dilution
with solvent la appropriate, Ua« the •tand-
ard curves (Section • 1» t» obtain an e*ll
mate of the coneentratlom.
Identify all peaks by cornparlrsi the
iirmwn retention Umea ol compounds ea
prricd lo be In the relenllon time* ol peaks
In the sample- Identify any remaining un-
identified peaks which have areas larai-f
than ft percent ol the loial uilng » OC/M8,
or estimation ol possible compounds by
I heir retention times compared lo known
'•i—ipsiiiids, with i:onllrmaltui» by lurtlirr
uc analysis.
• 1 Calibration Standards. Prepare or
obtain enough calibration .ilamlards «o thai
there are three dlllrrenl concrniralion.i ol
each organic comiiourid rMpertad lo be
measured In the nouri-e sample For each or-
ganic compound, nrlecl thowr concenlration-i
that bracket the concentrations eipecled In
the source aamples. A calibration standard
may contain more than one organic corn-
pound. If available, commercial cylinder
gaars ma* be used II th€lr concentrations
have been certified by direct analysta.
If samples are collecled In adanrbcnl lubes
(charcoal. XAFt 1 Tensis. ttf.t. prepare or
obtain standard* In the tame aorvent issrd
lor the sample eilracUon procedure. Refer
lo (lection 7.4-i.
Verify the stability of all standards for
the time periods they are used II gas itand
ards are prepared In the laboratory, use one
or more nl ihr following procedures.
9.3 I Preparation ol Standard* from
High Concent ration Cylinder Standards
(HitsJii enoufh high ntncentrallon cylinder
Mandsub. lo rrprr.wnl all Ihr oiganlc com-
DUUiid.1 nnrt:led In thr source sampler.
t)s»- Ilii-sc high KHHi'iilf »l Imi standard* In
lirrparr li>*cr riiiiii'iil'Blinn alsiutards by
rflliillim as Nltnwn ny Hguri-s III 5 and It «
Tn prr|»ar'- Ihe diluted i-tlllirslimi Min
iilrs rallhraled urtsmclrrsl srr normally
,«rd lo mclrr hiMli Hir High concentration
rallbralliin n«-s ainl I In- dllurnl «•-' Ollwr
iypc» ol flowsnrlrrii and rofiimerrlally avail-
able dllullnii lyslcmw can all* br used.
Callbralr racli fluwmelrr brloTC use by
placing II hJ'twi'Mi tlw dlltienl gas supply
and inllsbly .irwd bubblr mpl«, sttlnirneter,
or wrl Imt mrlrr Rrrord *U dala shown on
FHurr 18 4. While. It Is driliaWr to calibrate
Ihe cylinder gM llowmcter wllh e»Mnde«
gas the avallahlr iinaiitll]' anrt cost maf
Iirerindr it Tlir rrn»r Intradurrd by "»'"•
Ihr dlHienl «a> lor rallbrallon Is InakjiHIl-
rani lor gas miilurrs of up to LOW *o 1.MV
pum ol each or«»ni<" coinpotieiit
Once the fluwmrlrrx are calibrated, con-
nect the Itowmel.-rB U. ihr ratibratlnn and
diluent gas imjsjilie*- "aslril * rnm Telton
tubing Connei-i IHr w
-------
T
. 40, App. A. MUlfc. II
Where:
10* ^ Conversion lo Kim.
X - Hole or volume fraction ol the orfaluc
In Ihc calibration fu la be diluted
q.. - Flow rate of Uie calibration IB* to OB di-
luted In aU«* I,
d, - How rale of the calibration iu <•> be 61-
luUd In «*•• I.
Ov - no* rate of diluent |U In itaae I.
q* - Flo* nle of diluent iai in tUtf t.
Further detail* of the calibration method*
lor notnaetaf* mad the Remove the •rrlme.
w * j When the haf la filled, slap the pump, and
cluce the DM I™1*1 valve. Record the final
neier reading, lempenlure. and preuurc
DMnnneci the DM Iron llie Implnaer
ouilel. Mid either act II ulde fm •! lemol I
hour, or —wtl" Ihe ba« to Insure oumpleu
throuih • dry iu mrirr thai hu
been callbriled In • mumer ronilBlrnl *lth
Dlu(e tMtmine af dry *u meter, mm
H«
T»- Ateolule lemperalurc ol dry lai meter.
•K.
IOOO" Convcralon lactor, ml/liter
«11 1 liquid Injecllon THhulauc Uw
the equipment ihov/n In Mjuri- II B i:«ll
brmle the dry |u met" H drwrlbrd In Sec-
lion till •llh • virl Lnl mrlrr ur • id I
Cq. 18-3
romeler. Uae a water manometer lor the
prevwire (aiujo and •>••>, Teflon, brui, or
U«lnm> «lcel for all connection*. Connect a
ral*e lo the Inlet of the M liter Tedlar baj.
To prepare the tianda/da. aiirnitih Ihe
equlpmetU ae thown In Pbiiire !•-•. and
leak check Ihc *yilem. Cumpietcly evacuate
Ihc bag Pill the bac wUh hydrocarbon Irer
air, and evacuate the bag Main Ctoec Ihe
Inu-i valve.
Turn on Ute hot plate, and allo*r Ihc
water lo reach toillnc. Connoct Ihe bai lo
Ihe unpinarr outlel. Record the Inllul
n«i*r rcadlrui. open the oaj Intel valve, and
oprn the cylinder. Adjiut lite raie au thai
Ihr bat xlH be completely tilled In approi)
maiely in mlnuLea, Hn-ord meter prcuurr
and temperature, and loctl barumrlrk- pri-a
•urc
AllDW Ihe liquid urianlf lo rqulllbrilr In
room u-mprralurr, fill tlte 10 01 10 mln.i
IKer nyrlruje Mi Ihe drilrril liuuid toinnir
PI 60, Aftp. A. Math. II
Mcuure the tulvnil liquid denclty «l
ruom trmurrBlure by ncuraulr »elftllna •
hriovn volume ol Iht iMlerUI on an anal|rt-
leal balance In Die nrarul I O mllltflrmm A
•roundaliu aloopcred II mil vnlumetrlc
fluk or • tlaot Btiippercd opecirie |T*«ll>
bottle b auluble (or »el«htn| Calculate the
rauli In term* ul i/ml. Aa in alUmallie,
IllerBlure values ul the demlty of the liquid
ki 2O *C m«v be UMd.
Cclcullle earh oriuilc HanfHrd concen-
iratlon C. In OOm u l
6.24 • 10
l,P
Cq. IB-4
•here:
U~Uquld volume of nnuile Injected pi.
rU Liquid oraank dendtv ai detrrmlned. I/
ml.
M = HolecuUr weujhl olor(anlc.•/•mole,
M.OU- Ideal iu molar volume at »> 'K
and 1M nun Hi. lll*r»/« mole
!«•- Conienion to ppm.
laoo-Oonventon faeur. ^l/ml.
».t PrefMfBtton of CaUnrUlon Curvem.
Bf««Mi«»» peeper OC amdllloni. then Huih
UK ampllni toao for M •eoond* at > rale ol
100 ml/mln Alto* Lhe wmple loop pi inure
u> equlubrue to aUBoaniierle pnaiiii». and
atUvalc UK Injection nl*e. Record Uie
ttmndmrd OBoccnlntlofi, aUcnumtOf factoi.
Injection Uma. chart Bml rctcnUon tine.
peak, area, aunple loop lempermiure, oalumn
temperature, and canter M* now rale.
Repeat Uw (UndaJd Injection unUI two con
•mtlve InjKcUoni «l*e an* count* vlihln 6
percent ol their average. The trcraie value
awlUpted br ihc atunualar lacu> u> Uwn
the emJIbfUkm area value lor the ooncenO»
Uon.
Repeat ihta procedure lor each Umndard,
fntmn > traphicaJ ptot ol cancentrmUan
1C.) teraui the callbraUan are* valuei. Per-
form a n«te**I ihe Independeni analy*!*
672
873
-------
PI, 40. Apov A, AfUrh. II
ronrwntration I* wllhln S peirenl ol the |U
manufacturer • concrnLrallon
1. nnol Sanplliip and jlHafvlll Procnftrr
ConaMrrlng wifely I name hazards! and
ihe awn* ootxttUanm. vetecl an approprlaie
awnpllng and on»Jr*l« procedure ISeclUm
II, 7.1, 7 J, or 1 «i Inaltuallona where a hy
drogen flame la a haxard and no Inlrlnalcal-
ly vale OC la aultabk, uar Ihe fleilMe bog
coUactlon techfugue or an adaorptlon lech
nlque. If ihe aource trmperalure U below
IWC. and live organic onncenlraUona are
oullaMc for the detector lo to uard. uae the
direct Interface method II the aource gaaa
require dilution, UK a dilution Interface and
either the bag aample or ooanrpllon lube*.
The choice btlween theae two technique*
wUl depend on the phrrical layout of the
die, the aource temperature, and the ator-
age MabUJty of the compound* If coJteetcd
In Uw bog. Sample polar compound* br
direct Interfacing or dilution Inuwfactng to
prevent aample loai bj adaorptlon on the
bag.
1,1 Integrated Bag Sampling and Ana/r
•to.
1.1,1 Evacuated Container Sampling Pro-
cedure. In thai procedure, the bat* are filled
by eraeuaUng the rigid aJr light conlalncn
that hold the baga. UK a field umpir dala
•heet aa ahown toi Figure la 10. Collect trip
Iteau; aample (nun each aample location.
1.1.I.I Apparaiin
1.1.1.1.1 Probe. BUJnlea cteeL Pyrei
ilaam. or T«npn tubing probe, according to
the duel temperature, with M-mra OD
Teflon lubtng of niffietenl length to con
nect la the aamptr bag. Uae atatiueai Meel or
Teflon union* la connect probe and aample
line.
1.1-1.1.1 Quick Connect* Male 111 and
female ill of atalnJeav rim coroarucUon
1,1,1,1.1 HevdV Valve. To control gaa
flow,
1.1.1.1.4 Pomp Leakkaa Teflon-coaUd
diaphragm trpe pomp or equivalent. To de-
llrar at leaat l IILer/mbi
11. LIB Charcoal Adaorptlon Tube. Tube
fUlod wtUi activated charcoal, wlln gtaai
-'- I each end. lo adaorb organic
1.1 I.I.• novnteter, 0 to tOO-ml flow
r*me; wtth manufacturer* calibration
curve,
1,1.1.] Sampling Procedure, To obtain a
•MBDle. aovnubhj the ownple train a* thorn
In Figure It-t. Leak cheth both the bmi and
Ihe ODnutner- Conmcl Ihe nacuum line
from the needle ral*e to the Teflon cample
line from the probe Place the end of the
probe at the omtrold o( the MM*, or at a
point no cloaer lo ihr walk than I m. and
Mart the pump with the nndfe ralte adfi^t-
»d lo field a Oo« o( o 3 liter/minute. After
allowlnfl •ufflclem llmr to purtr the Hne
BF*erml tlmn connrri the *uuum line to
the bag. and eiaruatr until Ihr roiamrler
40 CPU Ch. I (7-l-m Edlll«n)
no flow. Thrn pn.il I Inn the ump)r
and vacuum llnrji for uinpllng. ind begin
Ihr actual umpllnf. krrplng Ihr rate prn
parllonal lo Ihr nlarh vrkrllr A* a prnjui.
Won, dlieel Ih* *su rilllnt Ihe roCamewt
• ••v from okmplliig penumnr I. Al the rnd
of the umple prilnd shut oil Ihe pump
dtoconnect the umple line from the bag
and duKOnnecl the vacuum line Iran the
bag container. Record the aource tempera-
ture, barometric preaure, ambient tempera-
ture, aampllng flow rale, and Initial and
final nrnpllng lime on Ihe dala aheel thown
tn Figure If, 10 Piotcct the. Tedlw bag and
IU container from mnllght When pooatMe
peiform the analyita wllhln 1 noun of
•ample collection.
1.1,1 Direct Pump aampllng Procedure
Follow I.I.I, eicepl place the pump and
needle valve between the probe and the bag
UK a pump and needle valve eonMruded of
(tatnlea* ateel or aome other material not al
reded by the rtack lao. Leak check the
•votem, and then purge with Hack gaa
before the connectlnt lo the prevtoualy
evacuated bag.
1.1.1 Eiploaton Rtok Area Bat aampllng
Procedure, Follow I.I.I eaeept replace Uw
pump with another evacuated can late
Figure la-ta> Une thto method whenever
there b) a poatibillly of an ciplcaton due to
pumpa. hratrd probea. or oilier nanx pn>
ouctng eqjulpnent,
1.1.« Other Modified Bag Sampling Pro-
. In the event that cnrtdenamUon la
In the bog while collecting IM
aample and a direct Interface lyWm caftnot
be uaed, heat the bag during collection, and
maintain It at a rallaMy elevaledl tempera
lure during all aubaequenl operatlorw.
(Note: Take care uj leak check the lytien
prmr to the dUutkma oo aa not lo create •
potcntiallr eiplodve aUnoaphere I Aa on ok
lernatrve. ootleet the oample aa*. and itoul
taneoualr duute It tn the Tedlar bag,
In Ihe Itrat procedure, heal the boi con
lalnlng the aampk bag to the avuree ten-
peratura, provided the componenU 9! the
bag and the •urroundlng boa can wllhiUnd
thto icmperatme. Then tranoport ihe ban ai
rapMIr aa powdble to Uw analytical area
while malnUlnlnu the heating, or eorer the
hoi with an Inaulalint blanket- In the ona-
IrUcol area, keep the boa heaved to aource
tempenture until analvata. Be rare that the
method ol healing the boi and Ih* control
for the heating circuit are compatible *tLtl
Ihe aafetr eeftilcllona required In each are*
. To uae ihe aecond procedure, preflll ln«
Tedlar bag with a known quanlltr of Inert
gu Meter the Inrrt gaa Into the bag accord
Ing to the procedure for the preparation of
gu concentration itondarda ol volalltr
liquid material! the aunpllng valve wHh
a piece of Teflon luMng Identified lor that
bag. Follow the apecllKaUon on ntpHcate
analrv* cpectlled for the callbraUon laon.
Record the data Ibted In Figure 11-11. If
certain Item* do not applr. uae the notation
'HA' Alter all »»mptem have been ana
Ivaed, repeal the analywn of the eallbraUon
goa mlilurea, and generale a aecond eallbra-
Uon curve, Uar an average of the two curve*
lo determine the tample gai concentratlorai.
If Ihe two calibration curvn differ br more
than 8 percent from their mean value, then
report the final reaulu b» comparb)on to
both calibration curves.
1,1.1 DetermuiaUon ol Bog WBUH Vapor
Content, ateaoure and record the anbtent
temperature and baromelrle tiifaiuit near
the bag. Prom a water •aturoUort vapor
preawre UWt. deUrmlne and recort the
water vapor content ai a deebnal figure.
< Aavume the relaUve humldltr UP be 101 per
rent unleai a leaaer value b> knownJ If Ihe
bag hai been maintained at on elevated tem-
perature aa drarrlbed In Bectlon 1 1,4, deter-
mine Ihe Mark laa water content b* Method
«.
7.1.1 Qualllr Aawirance. immrdlaUIr
prior to ihe onalrila of Ihc (lack taa a*ai-
PleB, perform aiidll analvxea u deacrlbed In
Sertlon OS The audit analyon must agree
»llh Ilir auilll roncenlralloru) within 10 prr-
"•nt II Ihr reaulla are aereplabir. procrrd
>llh Ihr aiialv.v* ol Ihr HHirce luunplra If
Ihry do mil *aree »llh(n IO permit, thru
fl'-Krm|ii1 |||,< trmjuin {at Ihf dlacrrpuM'y,
•n or purgrd with source gai or
In dlrrrl witrt'r las Into the (JC hulriimenl.
874
875
-------
II
T.I I • Needle Valve. To contrul iu &am
pllng rale Irora the lource.
I.I.I. 1 Pump, Leakleaa Teflon coated dia-
phragm-type pump or equivalent, capable of
at leaat I liter/minute aamplliuj rmlt,
lilt Plowmeter. Of tollable range to
meaaure aampiing rale,
11 I • Charcoal Adaortaer To adsorb or-
ganic vapor cottoned Iraa Ihc lource to
prevent eipneure at penonnel la lourca gaa.
I.I.I 10 QM Cylinder* Carrier gM
(helium or nllrogeol. and oiygen knd hy-
drogen lor • Dame lonlaaUon detector f PTD)
If one U wed,
1,1.1.11 Gaa Chninalograph. Capable ol
brim moved Into the field. »llh detector.
healed gaa aampling valve, column required
lo oocnpiete BttmnkUon ol dtghid eompo-
nenu. and opllon (of temperature program
1.11.II Becatder/lniefraiof. To record
rcaulU
1.1.1 Procedure. To obtain • ifj~rt*. eav
Ihe aamnllng ayiieoi a> ahown In
Hit. Make gure aU oonneciaarui ara
Ullil, Turn on the probe and aampte line
healen 4g UK temperature of the prate
40CflO> 1(7
133 HrlerrnliiBiliin ol -Slaia lias Mi>ls
lure Cuiilrnl liar Mr I hud 4 lo inruuir tftr
slat'k fu muuvlurr ciuilrnl
1.1 4 Quality Assurance. Same a& Section
1.1.7. Introduce the audit gaseg m ihi-
•ample line Immediately tallowing u,r
probe.
11 ft Emlaalon Calculation!. Same u 3rt.
lion 1.1.0.
7,1 Dilution Interface Sampling and
Procedure Source aajnulet lhi(
i a high concentration of orgfenle mm
I majr reaulrc dilution prior lo analyili
lo prevent aalurallng Ihc OC detector The
required for Uita dlrrcl Interlace
tt baaically the came ai that be
arrthrd In the Section 1,1. eiecpt a dilution
•mem M added h«i»een the healed aample
line and the aw aanptlng valve. The top*
raUai li arranged ao thai Hlher • IO:I or
10»l dlhtUoo ol the Hura gu can be dl
reded la Ilia chroeaalagraph A pump «f
mreer capae*y to abo required, and Ihb
pomp mual be healed and placed In the
•yalem b»t»eeo lha •ample line and the di
peraiuR a* trff**lTf On the IhertDacouuie
rokdmu dnk>. oooUul the hcallni lo main
lain a temperature of e la I'C above the
mnprralure While the probe and
r are betm healed, dtmnnect the
and attach the one from the calibration gxat
•liUire Pluah the aample loop with call
bration gaa and analpee a portion of that
•a*. Record the reaulu After Ihe calibra-
tion gBi amnpie haa been flushed Into the
OC taatrumenl, turn Ihe gai aampllng valve
lo fluafa p»JHn« then reconnect the probe
line lo the valve Place the Inlet of
i at the eemrotd of the duct, or at a
to the "mill than I m. and
dnw aoun* gai tauo the probe, hraftad. line.
loop. Alter thorough
; awmpMt iialrul the
lion* aa lot the callhrmllon gai mliluro
the analyate on an nMHhrt"'
, Mcaaurc the peak area* lor Ihe tew
••plr*. and If Ihe* do not agree lo v/tthln 0
percent of their mean value, analyae addl-
i until l»o conancutlre anaJy
Ihto criteria. Record Ihe
Alter conataieni reaulu arc
Hirnone Ihc probe from the aource and ana
lyee a aecond mltrmtHm gai mliture
Record thto calibration data and the other
required data on the data aheel ahavrn In
Plgiur If 11 deleting the dilution gaa tnlor
(Non Take care u> dra« •!! lampln, call-
oration mlilure*. and audlu through the
•ample IUUD »l tnr aimr prrvvurr I
T.I, I Apparatus,. The equipment required
In addition lo thai apedfled for the direct
Inter!tee iveloD to ae foJIoanv
1.1.1.1 aample Pump. Leakleaa Tenon
coaled diaphragm type thai can •llniUnd
being heated lo I»'C gnd deUver 1.6 liter*/
minute,
1.1.11 DUutioo Pumpm, T»o Model A IU
Komhyr Teflon poaitire dleplaecnerit type
delivering ltd ae/mBujte. or equivalent. Ai
an option, calibrated novmeten can be ueed
In oonlunctlon aillh Tenon-coaled dU
phragm pump*.
1.1.11 Valvea. T*o Teflon three »ay
valvca, aullahtr for connecting u> 4.4 nun
OO Teflon Uibing
1.1.1.f Plowmeton. Two. for meaiure-
menl of diluent gaa. eipocted delivery flow
rate lo be I.UO cc/mln.
1.1.1.i Diluent OH »Uh Cylinder* and
Regulator*. Oae caul be oltrogen or clean
dry ab. depending on the nature ol the
1.1.1.0 Healed Boi. Suitable for being
Lo IIB'C. lo contain the Ihret
three way valvee, and aaaoclated
The bn* ahould be equipped
•lib auk* connect flUlnga lo lacllllale con-
oecUon ol: < 11 The heated (ample line from
Ihe probe. 41> Ihe gai aampllng valve. Ill
Ihe calibration gai mliLurea. and 41) diluent
gai llnea A •rhemallc diagram of the com
ponenu anl oonnectloni to ahovn In Figure
|g II.
I HOT* Care mual be taken lo leak check
the lyHem prior to the dilution* ao ai not 1°
create a potentially eiploilve •imoaplierr I
Ttir healed bo* iriuafii In rlgurr IB IH l!>
dcllgrn-d lu recrlvr • hraletl llnr Itwm U>»
Environmental frolodlon
prote. Ait optional uepilin Is lo build • probe
unit Lltai •llurlii-a dlfMlly lo Ihr liektrd
boi In this vay. llir heated boi contclitx
I he ranlfou for the pi or* healen, or. II the
put Is placed agklruL Ihe durl being um-
plrd. It may be puulble lo eliminate Ihe
probe heiieri. In either rase, a heated
Triton line If uied 10 connerl the. healed
boi Lo Ihe gai aampllng valve on the chro
mitogiaph.
1 1,3 Procedure. Aiaemblr the apparent!
by connecting ihe heated tun. Ihown In
Figure II II. between the healed aample
lUtt from Ihe probe and the gai uniplirui
••Jve on the chrornalograiiri. Vent Ihr
lourrc gat from the gai lampllng valve di-
rectly to the charcoal filler, eliminating the
pump and rotameur Heat the cample
probe, aample line, and heated boi. Inert
ihe probe and lource IhennocDupte to the
ocntrold of the duct, or lo a point no cloacr
la the valta than I m. Heature the aource
temperature, and adjiut all healing unlla lo
a lemperalure 0 lo J'C above Uito lernpera-
uire If thli temperature la abort the aafe
operating temperature of the Teflon compo-
nent!. ad|ual the heating to maintain a tem-
perature high enough lo prevent condenaa-
1km ol water and organic compound*
Verily Ihe operation of Ihe dilution lyatem
br Bfialnlni a high concentration gai ol
known compoalllon through cither the 10:1
or IOO I dilution atagc*. u appropriate. (If
neccHary. vary the flow ol the dJIuenl gai
to obtain other dilution railm.) Determine
the canxntntton of the diluted calibration
gai ualng ihe dilution factor and the call
brallon curve* prepared In Ihe laboratory
Record the pertinent data on the date. «heet
ahovn In Figure !• II If the data on the dl
tilled callbraUon gag are not •llhln 10 per-
eenl ol Ihe empecmd value*, detennlne
•taetber Ihe chromatograph or the dUiUlon
intern to bi error, and correct. U. Verify Ihe
OC operation latinf a le* ennoantral ton
Mandard bi diverting the gaa into the
aimple mop. bypaiatng Ihe dilation intern
If these analyeea ara not within atinepiaMf
Umtta. oomri the dUuUon tyatem U provide
Ihe dealred dilution facton Hake IhU cor-
ractlon by diluting a hlgh-onneenuratlan
Mandard ga« mliiure lo adjual the dilution
PI M. App. A. NUrh. !•
IVlrrmliiBllon of Slick Oat Mole
iui-ni -S«rnt- •& .Srt-liun 121
Ai.-.uf»nri- Samr u Section
Once the dilution lyitem and OC opcr-
•UOIM ara aaltoraclory. pronexl «Uh the
analraui ol avurce gai, mabilalnlng the eame
ifilutlan Klllna u uied for Ihe alandard*.
Kepeal ihe analyata until t«o oonaccutlve
»«Jue» do no* vary by more than 8 percent
iiam their mean value are obtained,
Repeal ihe analyata of the calibration gai
mlilure* to verily equipment operation.
An*lyic;irte I BO field audit lamplu uilng
'llhrr Vhe dilution ayileai. or directly can
nrri Ui the ga> ujnpllng valve aa required,
Hn-urd all dala and report Ihe reoului ui Ihr
1,1 U
lurr Co
1.3 t
1.14
7 ],& Emlublun <;*lcui«lluns, Bune u 8ec
lluii l.l.S. •Illi i lit dllullun factor applied.
1.4 AdsorpllcMi Tiibr I'rurrdurc lAllema
live Prucedurri. II L> augmted that Ihe
irjirr refer to ilie NaikHial liulltule of Oc-
cupiilonal Salny »ikd Health «NIO8Hl
method for tlic particular organlca to be
aamplrd The pih» l(i»l Inlerlerent will be
ttalcr vapor If valrr vapor to praaenl at
concenlratlona above 1 percent, alltca gel
•Itotild be uied In fiunl of the charcoal,
Where more Him one compound la preaenl
In Ihe emlailoiu. then develop relative ad
aorpllve capacity Inlormilton
1,4.1 Addillonal Appwatui In addition
to the equipment luted In ihe N1OBH
method for the particular onanlcii) to be
aunpled, ihe folbmmg llemi lor equivalent)
are niggetled.
1.4 I I Probe (Optional). Boroalllcale
glui or aulnlcoi ilecl. appro ilmaicty t mm
ID, «lth a healing lyatem if water eooden-
•atlon U a problem, and a filler (either In
alack or oul-uack healed lo alack tempera-
lurei u> remove paniculate matter In most
Inatancea, • plug of gUia •on I la • aaUalae-
lory filter,
1.4.1.1 Pkilble Tubing. To connect probe
la adaorptlon tubes Uae a material that ei-
hlblti mbnlmal cample adaorptlon.
1,4,1-1 Leak «*»• Hajnpir Pump. Plow onn-
trolled, conatant rate pump. «lUt a art ol
limiting I ionic) o/l f lea lo provide pumping
nia from approiimalely 10 u 100 cc/mln
1.4.1,1 Bubble Tube Plowroeler. Volume
accuracy vllhln i I percent, lo calibrate
pump.
1,4.1.4 BiopMlch. To lime aampllng and
pump rate eallbraUon,
1.4,10 Adaorptlon Tubee, Bunllar lo onea
•perifhed by HIO8H eicept Ihe amount* of
adaorbent per pnauwy/bkckup eecUone are
•DO/m mg for charcoal tube* and 1040/MO
mg for alllca gel Uibea. AM ao altemallve.
the lubea may contain a poroua polymer ad-
aurbenl auch ai Tenaa OC or KAO-1,
1.1.1.1 Bararoeler. Accurate to • mm Hg.
lo meauire aimoapherlc pnavun during
aampllng and pump calibration.
1118 RotaineleT. 0 lo 100 cc/mln. to
detect change* In flo* rale during aampllng
Lit Sampling and Arwlyati. It I* aug-
gealed that the Uaier follow the ammpung
and analyaU portion of the reapeeUve
NIOSH method aecllon entitled -proce-
dure' Calibrate Ihe pump and (bulling ori-
fice nuv rate through iirttiT-r""*' tube* Mth
Hit bubble lube Itflwmeur before eanipllng.
The aampl* lyitem can be operated aa a "re-
clrr-ulatlng loop" lor IhU operation. Record
Hie ambient leoipeialure and baromeLrtc
prrwurc Thru, during umpllnt. uac ittr to
-------
tameter La verily thai ttir pump and cirlllrr
•unpllng ralr remain* constant
U«e • aample prattr, It rrqiilrrd. in obtain
Ittr sample at (he crnttold ol Ihr dun or at
* point no cloaer la the *•!!• than I m Mln
Imtae the length ol fkilble lublni brtwrrn
Ittr probe and adaorpllon lube*. Several ad
•orpfJon tube* cmn be amnedtd In •rrla, I'
the ell** adBWpttve capacity It needed. Pro
'Mr UMB ga* aajnple u> the aample »y*tem •(
• praam* turftctcnl for the limiting orifice
to lynetlon M • mmte orifice. Record the
tout IbM and «an>p*e now rat* tor the
number of pump flnMCi*. the baroraetrte
pyegam*. and ambient temperature. Obtain
• laiAJ BMRpkt volume oomfnenaurate «IUi
the ••peeled enneenlraUaMl) of the volatile
o>gaiitn«) prut lit, and ncoiiiliiended
BBOipM loading laden (•eight mnple per
vetgfit •dBvpCJon oMdltl. laboratory tat*
prior U) actual aampllng may lie in uia«ai|
Mi predetermine Uito volume. When more
Ihwi one organic to preaent In the rmt**ton*.
then devmlou retaUve adaofntlve capacity In-
formation, If amler vapor to prevent In the
MBafMe «i concentration* atoove } to ] per
cent, the adaofntlve capacity map be aevere-
ly reduced. Operate the gaa cnronialag;r*ph
according to the manufacture'i InMructlon*:,
After eatabitohlng apUmiifn condition*.
verify and document theae condition*
during all operation*. AnalfM the *udlt
araploi «KC Seclkm 1,t i.ll. lh«n Uw emb
•Ion ampler Repeat the anaJrcb of each
•Mnplc until the retoUn devtellon of two
oonaecuUfe Inleclioni doe* not eieeed B per
(Mil.
T« j SUndwnli utd Calibration. The
•Landartt* cmn be prepared •ocnrtinf la the
re>vectl*e NIOSH melhad, ttae a inlnHnum
ol three dlllcrenl xUndankv aelect the con
oenttmtlom to bracket the einecUd a*era«e
•mmple eonomUmttoii, Pcrlonn ttte oJIbn
lion before and after each dav'i ainiple
•nalinea. Prepare the calibration curve by
ualna the leajd. •quam melhod.
t.t.4 Quality Amrmm.
1441 OcleraitnaUon of Daorpuon Bfri-
rteney. Ourln* the le*tlnt pnwrain. Orler
mine UM aemni*tuti efficiency In the ei-
pecied tarnpV coneenlratlon ran«e for each
batch of adjBrpUon media to be iiwd Use
on Internal Mandard. A minimum doorp-
llon effleleney of BO pereent sh»ll be ob-
telmd. Repent Uw deaorpUon drtermlna-
tkm until Int relative deviation of two con
•eeuutc detcmtnaUom doe* not rkreed a
pereent. Uae the a*ena* dcnorpllon efri
Hency of liteae two cnraecutlve drtcrmlna-
Uon* for the oomctlon mpoclllcd In Section
1448 If the dnorptton rfllclenry of the
rompouTMld) of Interest U queillonable
under actual tampllni rondlilona. \ar of the
Method of Bland*rd Addllkim may br hrlp
ful to determine Hito value.
1.1.4.1 DetcrmlrHillon ol Samplr Collrc-
lion EffIclencip. Por inr gouree «uni>lm, an*
40 CHI Ch I (7-1-lf EdllUn)
IY/S Ihr primary and barkup pntllnn>i nl ihr
•dMirulliin IUDRI wrraritrl]' It Mir backup
ptirtlnn firrrda IO prrrrnt ol Ilir InlM
•mount 'primary and bmrkupP. repeat irM
sampllni wllh a litirr umpllni portion
14,4.) Analyibi Audit. Immediately
bFfnrr the aample analyara, analyze the Iwto
•utfll* In accordance with Bn-tlofi 7 4.3 Thr
analysli audit ihall aaree with the audit
concentration wllhln 10 percent.
1 t tt Pump beat Checks and Volume
Plow Rale Clieckn. Perform both of lliemr
checln Immediately after Bampllni with *i;
•ampllnf train component* In place. Prr
form all leak chedu according to the manu-
facturer'! InBtrucHona. and record the re-
nilta, Uar Ihe bubble tube ftowroeter u>
tneaiure Uw pump volume now iat« vith
the orlfln i*w?d In the lot aampllna, and
Uw mult. If II ha* chanted by more than I
but ttai Ifun Ml percent, calculate an aver-
age flow rate for the lot. If the flow rale
hut chanced by more than ID percent, reca-
librate UM pump and repeat the aampHtifl.
1448 CaJculalton* Jill calculation* can
be performed aocordln* to the tumecuve
NIORH method. Correct all mnple volume*
to Mandard concUUona If a aample dilution
•f*t*m hai been uned, multiply the mulu
by the approprlale dilution ratio. Correct all
remit* by dividing by the deaprpUon fill
dene? (JeUiiiaJ value). Report reiulta ai
ppm by f otmne. dry baata
78 Rrportln* ol ReiulU At Ihe comple
Uon of the field Dnalymti portion of the
rtudy. ensure that Ihe data ihecu ahoann In
Figure 11-11 have been completed liumma-
rh* thl* data on the dau aheeU iliown In
Plture !•-!•.
I. 0lbHovniB*»
I, American Society for Testing and Mate-
rial*. C, Through C. Hydrocarbon* In the
AUnoiphere by Qai Chrornalotraphy.
A0TM D nao-11. Pnrt IS. Phitadelplhta, r>-
u tM> BM irii
I. Coraaon. V. V, Metrwdology for Collect-
Ing and AnaJyUng Organic Air Pollutant*
U.8. EnTtrnnmefllal Protection Agency.
Publlcatkm No. EPA «»/1 7t 041 Prbru
ary If7t,
1. Dravnldu, A.. B. K. Krotnatyiutl. J.
Whlllleld. A. O Donnell. and T. Burgwald.
Bnvlranntental Sctence and Technotogy.
Kll> 1100 mi ini
«, B«frrt*en. P. T., and'P. M. Netan. Ou
Chramalagraphk: Analyala ol Engine Bi
hauat and AUnDaphcre. Analytical Chernla
try. J*«) 1040 1041 1MB
B. FValrheller, W R. P. J. Mam, D H
Harrbi, and D. L Harrla. Technical Manual
lor Procea* aampllng atrategln (or Organic
Material*. US. Envlronrnpntal ("rolrrtlni"
Agency, Reiearch Trlinglr Park, Nf Publl
cation No. EPA 000/1 tfl 122 April 1018.
It] p.
2301"
fl FM J» FH 9319 9323 l«14.
1 FH J» FH 32851 31IHW
* FH. 41 FK 2J089
iw90 ine
B r*
and D. B, Undaay, BPA/IBRURTP Proce
dum for Level I Sampling and An»ly»toof
Organic Material* O8 EnvtroninefilalPro-
tectlor. Agency, l^""*™?""* *££
HC Publlcalton No. EPA ajyayl-li-OM. I**
rutty lft» lS4p. . _ _
II Harm. W. «. M « Hal»«>d l^>
grammed Temnrralufe Oaa ChrornaWgra
phy. John Wiley * Sons. Inc Mew ¥ori.
IVflA
IS Inlrrsorlrlj Committee. Method* of
Air Sampling and Analfabk AmertMlt
Health Amorlallon Washington. DC. '«*•
10. Jot**. I' W . R » Orammai. P E.
Strap, end T. B. SlMnlortt. tnrirwunrnW
Sch-nce *nd Technology. IffiOi-ilO. IM",
17 McNklr Hail Bunelll. E. J- BMte Has
Chromal«|ra|>liy Consolnlaled Prlnl«r.
fJerkeley IM«-
IB Nelcnn CJ O. Controlled Tral Atmw
phrrm. Prlnrtplrt and Technique.. An"
Arbor Ann Arbor Sclenre Pubitahrm Itll.
141 p.
10 NIOKII M I «'l AnalyHral Melhnd».
V m« I 1. J. 4. S. g. 1 U S llenaHinnil
,.( llrallli »>'«I II » S"-'"^'" National In
Milule lor Ik-riipalmniil «»l'lf ..«! llralll.
Centrr lor IHwaiir runliol 4»7B Columhl.
Parkmy i'lnrlnnall. ««"» 4SJM Ai.rll
irii Augu»i IMI. M«y br a*allabl» from
the Buperliil-ndrnl of IliiruiiirnW. €lovern
menl Printing Olllfi-. *whlngto«. «.
I040J Stor* Numbei /Price: Vuluwr I-OIJ"
0110BM1 J/IIJ. Volume 2 OI1|»« "»W>
•/ill Volume 1-Oil 03ll OOMI «/••«-
Volume « -.n-OM -tin J/it.». *»'««*
6 Oltwll 00)4t I/IIO. Volume i-OlT OM
OO»g»-i/W. and Volume 7 Olt OM-MJ"«-
i/|t. l»Fte*i *ub»r«t t» change f%reHn
ordera add It prn ml-
M achuetile. l>. T J- Friiter. and 8. R
Huddell. Samnline and Aniilym ol Eroto_
alorv Irani «iatlona»» Snunssa: 1 CWor ana
Total Hydro»«rhiKi« Journal ol the Air Pol-
lution Control ABWctaUon. WIliwV-ffM.
'"l. Bnyder, A II. F H llod«Mr. M A^
Krmmer and J H MrKrmlnT. UlHIly ol
BolM B«wbri»ta Inr Sampling Urganh- Emta
.Ion* from Sl-lloiiary Ha-irci-n U.S. I^»«J
ronmenlal H»,*rrtlm, Agenrj Hes^ich TH
amile Pat*. W PubHratlon Ho KPA BOO/I
10 mi July ina 11 p
II. Truiillve Mil hod lor OwiHnuou*
Anilyils •'! Tirtnl llydrorarl«Mii In Hit- Al
moapherv. lnl»'is«'-l"lr Covamlllee. Amrrl.
can l"ubllr llratlli A.v<«'Iallon. Wa«hln»l»n,
I1C l«73 P '*« IW
JJ /.wrrn O . t:Ht; ll«iidbiic* ol ChrnniB.
innraphy, ViriiniM* I wnl II Hhrrma. Ji««-ph
led ». C"H<; Pfi'SS, Cleveland.
818
819
-------
PI. tO. App. A, M*th. I* 40 CFI CH. I (7-1-19 Edition) Iiwliwwwnlal Protection Agency Pi. 60, App. A, MUlfa. I*
I. toaoof I'MHII toto . III. iHvltat Ifta
Flfun U-1. PraltalMry wnwy toti
flto
tact riMM Ml if n
totortol
• to to MMlol toll fMciMts
r_- - UpstrtMi •!•'
fact or v«t to to iotolol Hn of port _
SIM Of KCOU
II.
.^__—___-__«»^ I. Prifortlw of *•
; £ • To^rituri .t
toloclly , Bttt
„ Stotlc pniMrt lictos l^O. tau
tow wtoHal _ MQlitiifV IMIOM f. tou
, tartUHUu cMUflt , Otu
_^ »_
ciclo CO^
Ctoch; fetch ComtloMis Cyclic „ m^
9t katci or cfclo ,
it MM to lost
18-1 (ontlawd). Pr«1l«lMry m«ty tfau
-------
40, App. A. ate*. It
C. fMpltaf cff
t» tit •» 1C
ta to bo
ctol
*t i
iwfltita «*r
Ptwt
tonc«ntr>tion
tr«fffe
cKroMt»fTaphie toll
rat*
Coli
Coli
Xaj^ciion port/»aa»l* loop
D»t»ctor
•• $
-------
ft tO. App. A, M*lh. !•
40 OR Ch I (7 I-S9 Edition)
rroparatloo of SUndardi IA Todlar Bagt
••4 Cal Ibratloo CUPI*
Standard* *roo«r«tl«*
Orfoolc:
••I
MIMuiV
fl
or Ho»llflcatlo«
Dry MI ovtor calibration factor
Hoof Ba
tor roodlng
Initial o»lor roarflof IllUrf)
MUro* •OloBt (Hurt)
••orofo oMtor toBO*ral*r* ("HI
toorofo *otor proMor*. fMgo COB H|)
Avoro00 otOMpMrlC protloro (OB H|l
fo«r*t* ••*•«• frtttvrt . ikuUte IM Nfl
Ifrtaft tMpfibrt 111
ISKllM 4.J-J-II
IIB H|)
l« *f gat •
lM «.I.M1
«i
(SMttW t.l.t.l)
!•• «f tl«l« !•
*.!.}. II
ft/ill
(HI
It)
Ctrrltr »li flw rtU (•!/•!•)
I«H tiifir<
Ultlal I*CI
Ic Nat
Coocoatratlon:
UJoctlo* Itao lt«-br clock}
Ofitooco lo ooaa ICB)
Cborl ioo*4 I «/•!•)
Oiooalf rotonllon tloo (oJol
•ttoowttoo factor
Pooh holfftt If*)
Pooh aroo tmfl
Pook aroo a attMnalloo factor (OB*)
Calcolatotf coocootratloo (opol
(C«Mtf«o It 3 or l*-4|
Plot oook aroa a altoMatloo factor «o«lnit calcitlaUd concon
to obtain calibration cvrvo.
IB-). Stanoar4i proparM I" Todlar 0491
and calibration como.
Prelection Aooncy
or IdfnllMctliOn
Pt. 60, App. A. HUHi. |«
C*HbnUon
FIOMMUr
Flo^tttr typt "1
Calibration da*let [.]. aubbif -tier
•aadlngi at laboratory condition!:
laboratory lenpcriturc
'SpfroMtrF
laboratory baronwtrlc prctlurc lf\4fl
flo> data;
rvadlng
lai Mrttdl
• ' "
- --
----
1 toOD.
(1)
'
{aotolMlcl
Ci
tl««
(•In)
1
ilibratlM dMlct
1
gat voliMt* \t\om rat*11
1
I
1
1
r i
i
. i
I • noli** of fa* wa lured by callbritlon device, corr«cttd to lUMdard
condition! (Ittertt.
b • Calibration dnlce 9*1 voltaM/tlw.
Plot no^i
iUr rtadlof. afalntt HOB rait (itandard ce^llloat). Md Ara* a
nlk CMTM. I' **• flowUr b«lng callbr*u4 It a rotaavur or «U«r
o* «•*!<• tMt ll vltcoilty d«p*ad«nt. II Mr «• ntctiiary ta
aallf* «' calibration c«rvti tkat cwtr ta* op«rall«f Kai»«ra
atw* ra»f*t of tho rioMttar,
ato a
•¥Ht U» follOMliin UchnKkW ikMld bt »trlfl«d btfor* appllcatlo*. U •«/
ko acitlblt to calcylaU Hw rata raadlAgi for rotavUri at *t
flo- r*«0
(I
flow raU
II lion i
Flourt 16-4. FloM*Ur eallbratlo*.
HH4
HHS
-------
vnHRjMOONIML
VAIVB
TtDLUMC
»*t IM. Stafto-tUft ulltovtt* fn tfflitf* tyttm.
6
Q
3
m
ft
f
QMCDftiATIM
msn
HUiNIAII
•EUOffAIR
WKWtStAUCCOf
CAS
ll-». Tw-iUft
-------
HIW
ffliVM
-OHIHOi
-------
•ussvoou
Ftfim It-*. Intent* btf M^
train.
M rtrt pi H9lta|
-------
• *• ^W,§ ^4^^.r fl^ Hifl^^L I m
I"C)
(•ml
If)
1«n«f ratolippr.)
ttart «•
Fltlrt
11.10. n«i«
faf OlItCtl
40 Cft Oi. I (7-1-W MM**)
fete
PI, 44), A»p. A. «*•*. It
MM*
i.
- r««Ur
fcMt
i-ei
•• i*ci
ll
pl« IM» «•!•• toll
IMlUAl' I*C)/I1M
Cantor
rat*
r knli)
fu flow !•«• talAUal
u-n. ru» ••
802
893
-------
s
t
I
.1
i
I
-------
ItatM L1M
Qrlefc
1H
10:1
l.lL/Mi
QirteltaMets
T« ••! fc*U
. Vil**4
!• 1»:1
tattti
— HBcc
I
(ta
Of In)
n* bu of &
mo —
«t IH Or
11-13. ScftMtk «1«fm «f tkt hMta* boi r««u1r«d
of M^tt |U,
I!
J i !l!!f!
1 ..!
il
Hill
,IH
a a a a 0 DQO a a a a a a a aaca a
!l
o a :
aaa
a 3 '
i
r
111 IHii! iifBlMffl
!
I! i
-I! 5
-I!
-------
EPA METHOD 3A
-------
caution Calibration .III tor ml
fected bt variation In (tack *u tempera
tor*. praMun. nmii»i»IMIIlr. and motocu
bu Mlihl. Uar- the procedure in Section
I I.I. Record all Uw laiM'irliuj device pa
ramewn on • line interval frequency iubr«tkm
Caefllclcnl. Y^ lor each cun *J follow!
. t
ten- prrauira
to Method U. Sec
fkeldumtcandl
«I lUroaarter CkUbral* the barometer
U> be laved In Uw fl*id UT* with a nvncury
mm Ms (Infill barometer prior to Uw fkHd teal.
thai do not have •
la Ute nanufac-
CilcubUc Uw
flo« r»tc. Q_ M
Q. - K.Y.Q.
T.
Ahcra:
K. - »
(air.
for mum* tonal
of MmMMi—QM Aluuvau RIB C«MDB Dial-
IM. OITOVB. KICBU Au. UB DB* Mo
. Dd Practice of
,. The FtoiDoro Com-
. •oaboro. MA IWI
P. PundameniAla of
_ . and no* Meature
John Wiley and Boom, Inc.
Ton., art. lam
I- Priactafe urn*.
I.I Prtndpm A tx cample b eiUncied
from a alacfc. by one of the fallow* roeih
oda: Ml dnilepalnl. §rab aamplbuj: 111
•Irujle point, mtoaraicd ounpllna/. or 111
mulU point, bile«TBt«cl HBfillnf. The ia*
I for percent carbon dloi
606
tO. Ap*>. A, M**h. 9
nuk ttlMt mn I>TMI Jr • Kyrlle ' wnlyu-r
miv br uwd for- Ihc iiMlrolii tor imctmt ilr
or emlulan r»lx rarrecllon factor drlcrml
nation, an Orul uialner muu br uard
I I AuttHcablliU. ThU mrthud IK appllr*
Me for drtcrmlnlruj CCi. and O. ronccnlra
Lion*. t*crm a». and drr molecular vrlal»
of a aampte from a cu ilieam of k luull
fuel canbuMlon prooeea. The roclhod may
aaw be wtlemblr io other proixve* wtirrt
U hw bHO drlenalned lhal compound*
other than CO.. O» CO, and nhracen «H,»
an not oreaent In canccnlrallona uifflcknl
la affect Ihc mulU
Other mclhwto. a* veil u rnodllkatlon* to
Ute procedure described herein, arc auo ap-
plicable lor aorbc or all of the above deter-
mlnaltoru Ciunptra ul ipeclflc mrlhoda
and raodlfkAUam bwlude: Ilia mulll polnl
eampllni meUKid uain« an Oramt an«lr*er to
analnc Individual «rab aaiBplea obtained at
etch poUil: O) a method ualrw CO. 01 O.
and «U)*th»3ro*Ulc calculation* to determine
dry molecular vewhl and eaona ate; Ul a*-
a value of 1OO for drr molecular
, In lieu of actual mcaaurcoicnU. lor
bufnlna natural ••*. coal, or oil.
Them* method* and nwdlflcBlJanB tnay be
but arc aubjee* u> Ihc approval of Ihc
r. lift Environmental Prolec
A* >n •lu-n.iinr lu Ihr jamulin*. kppara
lui and xtslrnu druirribrd hrreln. other
*amplliuj ivilr-nu ir • HquM dtaptocrmcnl I
may bt lued provuted lurfi lyimn* are <=•
uable of obulnlii« • rrprt«cnt*ll*e aaoiple
and malnulnlnc a comUnl ammpllni rale.
•nd mft tithrrvbr rmiwoJe of rfeldlna; me-
crpl«bie rriulu Uw: of iuch *ril«m* la *ub-
feci to Ihr apuruv*! o| ihr AdmlnaUnlor.
II Orab Hamplliiv] I n«urr I 1 1
1.1 I Probr The ptobe Utould be ntaoV of
•lalnlm >i*«l or borualllcau ilaai lublnfl
•nd Miould br «|uu»ard "Uh an In Hack or
out •Lark litter Ui remuve partirulaU rotlitr
la uluf of |Iau ajuol U aattefactor* for lhb>
purpoae). Any other material* Inert to O..
CXK CO, and M, utd r**l*unt U> UxnnerB-
lurr at aampllii« condlltoni may br uan) for
the probe; eiuuple* of aueh roalcrtaj are
aluminum, cooprr, quart* ftma and Teflon.
1. 1.1 Pump A unt-ny aquecce bulb, or
equivalent, b utrd lo trtMport the «a*
•ample la the analyur
1.1 InUgratedHamplMujlPUure J li
1.1.1 Probe. A probe *uch a* UUU da-
•crlbed in Section 1. 1 I I* ulLable,
'Mention ol trade name* or ipeclflc prod
urli doe* not corutilute (iidoncnicnl uy lite
EnnlronmenUJ ProlrtlUio Aintcy
607
-------
«0, App, A, fcUlh. 3
40 CM Ch, I (7-1-89 Edition)
WOit
11 Illlll
m ii« iciA&s noon
UOIIIIHll
-2
Environmental Protection Ag«ncy
111 Cnndriurr, An felr-rooird ni wilrr
rix>Ird eoiidi'nsri, or other conderurr that
•III not rrmovr O. CO.. CO, and N. may be
uwd U> remove. ricroii moblure which would
Interfere with the operation of Ihe pump
ind flow meler,
11.1 Vilve A needle valve la mtd lo
adjual aarnplr |ai Ha* rale,
1.1-4 Pump A leak-lree, diaphragm-type
pump, cw equivalent. U uaed lo transport
•ample gu la the lleilMe bag. Irudall •
•mall nurgc lank between the pump and
rale meler lo eliminate the pulnlton effect
ol the diaphragm pump on the rotarneler,
l.l.B Rale Meier. The rotfemeler. or
equivalent rale meler. uaed ihould be emu*
bte of measuring flaw rale lo «llhln 1 1 per
eenl of In* aclecled How rate. A flam role
range of MM to 1000 cm'/mln b niggnMd.
1.1.1 PleMlble Bag Any leak-free plutk
Ce.g.. Tedlir, Mylar, Teflon! or plaatk
mated aluminum (e.g., alumtntad Mr lor >
hat, or equlrmlcnl. hartni • capadll con
•talent with the Ktecud flow rale fend lime
krujth of tne iftl run. may be lived. A c»
In the range ol At to M Illera b uif -
To leak-check the b*|. connect It U» •
•tier muKmwlei fend preanjrtae the DM lo
9 lo 10 cm HX> Motecular Weight Detennliu
lion, An Oraat anaJrur or Fyrlle type corn-
buxLlon gai analfier mar b* uaed.
1.1.1 Bnlailon FUtt Correction Parlor or
Eiceai Air Delermlntllon An Orul anilr*
«r mini be iiaed. rW tow CO. I tea* than 4.0
percent) or high O, Igrealn thai ISO per-
cent! concentrfeUonf , the rneaaurfng buretle
ol the Oral mutt hue al teaat O.I perccnl
aubdlr
,1 Or* Molecular Wetohi DfUrminalton
Any ol the Ihree uunpllng and anilyHral
procedures deacrlbrd brlow nuy be uvd lor
determining the dry molecular writ hi,
1.1 Single Point, drab Sampling anrl An
olytlca] Procedure.
Pi. 40. Apgt. A, «UHi. 3
I I I Thr umpllnR point In Ihe duct
•hell rllhri be al thr cenlroM of Ihe croav
arcthm or at • point no cloaer U» the walla
than 1.00 m III fit. unlea otr«rwwje apecl
llrd by Ihe Admlntattaior.
1.1.1 Set up the equipment at •hown In
Figure II. making rare all eonnectloni
ahead of Ihe analyzer are light and leak
free, M an Great analyzer b uied. It b rec
ommrnded thai the analiavi- be leaked-
checked by following the praoidure In Bee-
ikm 5: ho«e*Kr, the Ink^neck •> optional.
I.I 1 Place Ihe probe In Uw Mack, with
the Up ol lltf probe pnrtthinnl »t the aam
pllng point, purge the aampllm lint. Draw a
•ample Into ihr analywr and tnnwdlalelf
•nalyie It lor percent CO, feral Dtrccnl O»
Determine the percentage ol U«e (a* thai b
N. and CO by cubtracUng In* man ol the
prreenl CO, and percent O, (rwn IM pet
cent. Calculate the dry molecular weight ••
IndlcaUd In Section • 1
114 Repeat Ihe ounpltng. iinalyaav and
calculfetlan praeedurea, until the dry i
alar weight* ol any Lhree grab
dllfer from Ihelr mean by no nnrc than • J
f/gmoV 10.1 lb/lr>mol«l, Aierage Uteae
three molecular welghU, and report the re-
cutui to the neareal O.I g/g mole (Ib/lb-
mote)
1.) ainglr Point, Inlegraletl Sampllnt
and AnalyllcBj Procedure,
111 The ampllng point In the duct
ahall or located aa apeclflrd In llectton 1.1.1.
1,1.1 Uak-chnk loptlonall Ihe fleilblc
bag a* in Section 1.1.1. Bet ui> the equip.
menl ai ihown In Figure II .luat prior lo
campling, leak-check
-------
Determine Ihe percentage of the gu lh*i I*
H. and CO by euMnctlng Ihe »um ol the
percent CO. and percent O. from 100 per-
cent. Calculate. Ihe di* molecular oelgnL u
Indicated In BecUon •-!.
l.l.g Repeal Ihe •nalylai and calculation
praeedurae until the Individual dry molecu-
lar wetghU lor any three anaJyaea dlfler
from indr mom by no more than 01 1/1
raoto (HI uj/ltmota) Average theae three
molecular •dgM*. uid report the reaulu u>
the newea* 0 I g/g oMrtc (0.1 Ib/lb-mole)
1.1 Hull! PotoL, lotetrated aampllng and
Aratlylkml PTooedure
I.*. I Urueaa otlwrKMc apedHed br the
Adenlnartnior. a mmlmum of eight unvtne
lor circular ataefu
ilainO.41 nlH m). a
3-3— SAUHIMG R*if DAT*
x iOD
bao.110%11
having •tutvaJmnt 4t*BM. for pcrcenl CO. or per-
cent
410 Alter the analyato la completed.
levk-chedl tm*mlalrtry> the Great analyser
once again, u described In Section A. Mtr
the resulu of Ihe BnaJiati to be valid. UM
Oramt analnef mini paaw Uila leak tori
before and after the antlyab
HOIK Bmn Uik dngle point, grab aam
and analytkml prooedure In normally
bi conjunction with a tingle-
potnt. grab aamfiUng and analytical prone
dure lor • pollutant, only one UMljali b) or
dliakrUr cABductodL Therefore, gnat care
muat toe token to obtain • vaJtd ammpte and
•nalyal* Although bi moat caaeg only CO.
or O. to raqidnd. It la recommended thai
both CO. and O. be mfmtiifed. and thai Bex-
Uon 4.4 be toed to validate the analytical
4.1 Single-Point. Integrated Sampling
and Analytical Procedure,
' 4.1.1 The aampllng point In the duct
•hall be located a* •pecUled In Section 41 I.
4.1.1 Leak-check (mandatory) the Heil-
ble bag H In Section 1.1J. Bel up the equip
menl a* ahown m Plgure 1-1, Juat prior lo
aampllng. leak-check (mandatixy) UM train
610
bjr plarlna * vu-iium gauge ml Hie < um1«-iu<-i
In let pulling • nruum of a Irui JM> mm II*
(10 In II||, plugging llic uullrl at Utr quick
dix-onnm. and then luritlnf oil Ihr pump
Til* vacuum ihill remain stable fui at IruL
OB mlnuic, Evacuite the fleilblr bag CIHI
nwi Ihe probr and place II In Hie alack,
•IIh Hie t||i of Ihr probe positioned H I lie
•ampllm) point; purge Ihe Ufn[illn| llnr.
Neil, connect the bag and make mrr thai
•II ronnrxlloru »re tight and Irak free
4.3 J Sample M a conatanl rale, or u
•peclftod by the Admlntal»u>r. The iam.
pllnt run mutt be almultaneoua irlLri. and
for the aame loUl length ol Urn* u. ihr pal
lulant rmlailon rale determination. Collect
at lemil M I lien (1,00 111 of (ample |u
Smaller volume* may be collected, iub|eci
to approval ol the Admlntalralar.
4,1,4 Obtain one Integrated Hue iu
•ample during each polluUnl emualon rate
determination. Par emuakm rmie correction
lector drUimlnaUon. analyse the awnple
wllhln • noun after II b laken lor percrni
CO. or percent O. lu outlined In Section.
4.1.6 through 4.1,1), The OnaL analner
muu be leak -checked (aee Section B> before
UM analval* II cicoa air to dealred. proceed
M follow*, in within 4 boon alter lh«
•ample ta taken, analyze It 0
percent or ibl o 1 percent by valume «hrn
o. b greater than at equal la ISO perreni
A*rra* three aoxpUble valuet of per.
cent O. and report the rnulu la the IM-UCII
O.I percent.
«,l.e.» for pcrcenl CO. repeal Lhe ui*
procedure until the reiulLa of any
Him- unaly.vrs ililfn by no more IMu. in
prrri'lll Anraur ll.r Ihrre UTppl.liH
Vlllli-A llf D.'.rrJ.I C|J ,1MJ ,,tHin ttlr re.li)u
Eti ilii^ iifiiriLM it I prrrenl
*'n Alli-r tin- •utiysu i^ runiplrlr>Ji
Irik.lmk iiiiuiidlluryl Ihr Or.ul (iiKlywr
UIM-C •••in. as ih'M-rlbra In Serliua J Ful
Hie IPSUIL-, uf ihr BiialyiUi to be valid, Itir
Or&n ikiialnu-r must pau Lhlj leak Leil
befure an aOer Hie analyahi.
_NOTI. AlUinuifli In maul Instance* only
*,'(>. ur (1, la rniulred, it u recommended
Ilicl bolh CO. antl O. be mtuured. and lh*l
Becllon til br u^etl to nalloale the analvil-
caJ dmia,
« J Mulll Huini, liLlr^i.trd Sampling and
Analytical frucrdure.
t 3 I Hull) ihr minimum number ol tarn
pllng polnLj and the aampllng point local Ion
(hall be as ipmflrd In Section J J I ol tub
method The UH ul lever potnu than ipecl
fled U *UD|ecl to the approval ol Ihe Admin.
4.3.1 Ptollow the procedure* outlined In
aeeUom 4.1.1 through 4 1.1, cicept for the
lolloping Traverse all iampllng poInU and
•ample al each point lor an equal length of
time. Record iampllng daU u ihovn In
Flrurr J 1.
44 Quality Control Procrdures,
l.f.l Data Validation When Both CO.
• ltd O, Are Measured Allhough in moat In
lUnrrs, only CO, ur O, mruurcmenl U re
qulrril, II Is recummended that Dulh CO,
and O, be mruured to provide a check on
Ihe quality of Ihr data. The following qu*l
H y cunlrol (irurrdurr la iu(*-«lril.
NUT* 3lrue the method lor validating Ihe
CO, and O, iiwlyses IB basrd on iiwnbuatlun
ol organic and loull fuel* and dilution ol
the gu ill-ram vlth air. thli meiliod doe*
not apply to aoureei thai 4 1 1 remove CO, or
O. through procewe* other than corabua
Won, Hi add O, (*g. oiygen enrkhmenl)
and M. In proportion* dlflerent from thai ol
air,
-------
PI. M. A... A.
4ocraai.
HI
*co.
Eg II
Ch »r neiuaat' In ambient air
ronpfluM* Iriel ehouM be oonmMrred n
irrmlnlna If • reteu to appropriate. I.e., If
Ihe nireeund em be ton* are much tower or
much frcelcr than the compliance limit.
repetition of Ihe leet would not amlfkanU*
etiange Ihe oflraplkinc* elalai of Uw i
and would be unmem*aru> i
endcuUy.
I L*m*O*t* Fnmmtmn fat Onmt Jaalpevr*
Horbu) an Onal enalran Irrquamlv
mam M to leak. Therefore, an OtaU i
UM (tfeutoUon for P. a. f •*"*! «».UM~.*IH
tola •- Tne procedure for I
«CCMadJI.%CO,i »CO <>•»« analjraw br
•.I fkrbHj Ihe I
«CO Bp ID the i
ftCO- Percent CO b? *oft*B*i «drr I
4.4.1.1 C*eap*»* Ibe odevteli
wttH UM CBpeeMd P. nluam The following
i for UM eipectod P. If Ihe fwri bring k 4 __
i are burned to M^ tn* M^^d hivd hi u^ i^Mii* ttm ^^mm.
__ . _ _ _ ^ ^BM* ^B^ ^^^^^H ^PWV •• ««^^ l^B^F^^W IV^ •••W^
I P. lector* «aa deftonl to Method III ac ~, i >. ^ Cknal^uml**** to mw* U»
^1 to UH Dtomdbwc hi HcUud II 0«c |iu tfurt. iaj jmuaumT-_11- -^
Uoa 1.1.1 Then catenate the P. factor a. . . , ^ ^^^ tg^t to
moat not toll below UM bottom of UM <
torr lobkaj dating Uu* I »duoli *mew»»l.
•.»• p. 1,1.1 The iiKHMaue hi Ibe havetle BMDt
not cheat* br men than • 1 ml durtng Ihto
f. « mbmte kntemL
t • If UM mmly*er fatto UM
Eq 14
i unUI UM i
itw-tM Mtm
!«•• *^™WOm» ip*>a) Wpf VQDHMf I*J
•.M4-Halloof O. to H, to ob. »/•
i the Uat reeuNo.
of
1 and the amlrdng tcch-
tnrvn oanBailraUan. tuch M
•*-. Ow luH teter •hould be rerk»«J mnd
range ol t II pet
lor the P. (KV» ol
•Ui«d lueto vlUi vmrteble furl raUoi Tn«
lerel of Uw untoUnn rate relilln to the
•.•H.MoJwumr oetoht of O.
!•»
• 44*-Uotocular wekjM at CO.
IM
• I Pwpcml Biome Air. CWemMe Ihe per
oenl eiooBi air 4U appltoaak>. br *ub*tltiit-
b«] the appropriate valuta of pervent O.
CO. and Hi (obtained from Section 4 1.1 or
4 141 IntoEoiutlofi II
612
M, App. A. JwVHfc. SA
*0, 0 »» CO
0 M4 %N. <%(V 0.8 %COl
Eq 3 I
Nor* The equation above •atnuiu thai
anMeni Ui to u>ed M the mrev of Ob and
Inml UM fuH doc* not contain •pprcctabk
aroounla of N. (aa do rake o*m or Mart luf
ta). Por thoac caan when apprecto-
Me amount* of N. arc pinaant«
natural *aa do not
aowunu of N.I or when
.OH.,
Uon of the lampir Mream to ixmvrrcd U> an
Inciruntrntal analyien*! lor drt^rmlnailon
of O. and CO, concentrsUanta*. Pcrlorm
am apcclllcMioni and tot oroordura mit
provklrd u> rmurv rrltoblc dai*
1. Itmmft mm* SemiittvUf
Hanc •• Method 4C. SecUom II and 11.
eiDcvt Utml Inr •*•» of Uw •xvutonnt
Matoui chall be artected anch that the atcr-
a«e O> or CO, coneentraUon li not tea* than
M peraenl of the apan.
1. DfflmUiami
1.1 Meawrenmrt BnbM. The loUl
pronl of (he A
• 1 Dry Mokra
i 1 to ralnilato
UM
T_ii__t:^^rjtTr_ «o«lpBi«nl required for UM drlcmlnaUon
•rSSS^JfrC^I^ Z^Z^^STS^JZlZZZ
^rs±r^ssrs sssir.^™^^
* drr "Wfceular Mmihl of uen»».l.l.«,l.l.a»« 1.1.1.
Nova: The
cr aram to air (atanrt »-•
fJPV Vk A
4VT.1V. A
about * I petcMM b bitradand The later
nay opt to tnctade atton to UK analrato
btoct to appronl of Ihe
SecUom 1.1 UirOBih 1J. and !.!•.
1.1 IMerferenet niannM*»i. The
of the a*ea*oranen>l *>alcn to a
to UM auapat BBL oUwr Uian
I. AlUhuller. A. P,
Vapor* to rtoaitr Bat*. '•
nal of Ab and Vater PoOvUon. Alt-ll.
Bame aa Methori tC. HeeUmm 4.1 thrau«li
4,4,
t tinmrmtm* ana1 A'ratniui
for O, or CO. Uiat OHCta the
of Into •wtnDd, A
«C I of McUnil «C. The ai-
Plflh A<
4, MHcnrll. V. J
RvnaMMr •* Ihe
of Ab PoDDUon CMMrol
«M Ma? irta.
i, abJccnara. H. T., R- M. HavHeML aod
«. a andlh, ValldaUti* Onat Anatna* Data
fraca Pcaril P*wl-Pbcd UnMa.
puna Neva. «lrtl-M AaavL ItW.
I.I I aanoto Probe. A kaa.ifn
auirMent knalli to Iravcrae the
atmo* 1A— DbraBtoiHirKM OF Oinavi •••
Ctffom Duaiae CoMWTMnona n
Dilation* Paoai ffriTfo*i«aT OouMn
f*ocv>mi)
I. ^ffHntnillf mn4 PrlmeiHt
I.I Appllcabintv Thto meUnd b appll
cable lo Ihr drtermlnallon of oirecn (Chi
•nd carbon dloiM* (CO.) concrntr*Uoo» In
rmtoatom from •lilkmarr «ourcrm only
•hen apecllted «llhln the rrvuiailom.
1.1 Principle. A lample b ronllnuaiuly
*Blracl«d from Ihr rffluvnl ilrram. • por
A heatoili
to not nuulnnl tor trvtenn lhal i
O, or OOb concentration on a drr
IfMBflorl drr I
1,1.1 9ampl
Vatae AwemMr. Mobtore RoaioraJ 8*«ICB,
Pita Rale Control. Utawle DM Manifold.
aad Dal> Rocorder, Hame aa Method ac,
ftoctlora B.l.l llinMil* • I t. and II II.
eicept lhal Ihr requfrmanili ilo uae aUhi-
In mtrrt. Teflon, and nonraaeltra ibun fil-
ler* do not tpDlr
B.l.« aa* Analr*er, An analyarr to oMer
mine ronllniiouHlr Ine O, or CC", mnenitrB-
Iton In Ihe •ample •*• itrvani. The analran
•lull rwrl the applicable prrlormam apec
lltcKllona of Section 4. A meant of control.
lint thr inalrwr (lov rale and • devln for
drwrmlnlruj proprr umplr Ron t»l*
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 3 - Gas Analysis for the Determination of
Dry Molecular Weight
1. APPLICABILITY AND PRINCIPLE
1.1 Applicability.
1.1.1 This method is applicable for determining carbon dioxide (CCLJ and oxygen
(O?) concentrations and dry molecular weight of a sample from a gas stream of
a fossil-fuel combustion process. The method may also be applicable to other
processes where it has been determined that compounds other than C0,t CL, carbon
monoxide (CO), and nitrogen (N?) are not present in concentrations sufficient
to affect the results.
1.1.2 Other methods, as well as modifications to the procedure described herein,
are also applicable for some or all of the above determinations. Examples of
specific methods and modifications include: (1) a multi-point sampling method
using an Orsat analyzer to analyze individual grab samples obtained at each
point; (2) a method using COn or 02 and stoichiometric calculations to determine
dry molecular weight; and (3j assigning a value of 30.0 for dry molecular weight,
in lieu of actual measurements, for processes burning natural gas. coal, or-oil.x
These methods and modifications may be used, but are subject to the approval of
the Administrator, U.S. Environmental Protection Agency (EPA).
1.1.3 Note. Mention of trade names or specific products does not constitute
endorsement by EPA.
1.2 Principle. A gas sample is extracted from a stack by one of the following
methods: (1) single-point, grab sampling; (2) single-point, integrated sampling;
or (3) multi-point, integrated sampling. The gas sample is analyzed for percent
C02, percent 02, and if necessary, for percent CO. For dry molecular weight
determination, either an Orsat or a Fyrite analyzer may be used for the analysis.
2. APPARATUS
As an alternative to the sampling apparatus and systems described herein, other
sampling systems (e.g., liquid displacement) may be used, provided such systems
are capable of obtaining a representative sample and maintaining a constant
sampling rate, and are, otherwise, capable of yielding acceptable results. -Use
of such systems is subject to the approval of the Administrator.
2.1 Grab Sampling (Figure 3-1).
Prepared by Emission Measurement Branch EMTIC TM-003
Technical Support Division, OAQPS, EPA May 14, 1990
-------
EMTIC TM-003 EMTIC NSPS TEST METHOD Page 2
2.1.1 Probe. Stainless steel or borosilicate glass tubing equipped with an
in-stack or out-stack filter to remove particulate matter (a plug of glass wool
is satisfactory for this purpose). Any other materials, inert to CU, CO,, CO,
and N2 and resistant to temperature at sampling conditions, may be used for the
probe Examples of such materials are aluminum, copper, quartz glass, and
Teflon.
2.1.2 Pump. A one-way squeeze bulb, or equivalent, to transport the gas sample
to the analyzer.
2.2 Integrated Sampling (Figure 3-2).
2.2.1 Probe. Same as in Section 2.1.1.
2.2.2 Condenser. An air-cooled or water-cooled condenser, or other condenser
no greater than 250 ml that'will not remove 0*» CO?' **^' ani^ N2' *° remove sxcess
moisture which would interfere with the operation of the pump and flowmeter.
2.2.3 Valve. A needle valve, to adjust sample gas flow rate.
2.2.4 Pump. A leak-free, diaphragm-type pump, or equivalent, to transport
sample gas to the flexible bag. Install a small surge tank between the pump
and rate meter to eliminate the pulsation effect of the diaphragm pump on the
rotameter.
2.2.5 Rate Meter. A rotameter, or equivalent rate meter, capable of measuring
flow rate to within 2 percent of the selected flow rate. A flow rate range of
500 to 1000 cc/min is suggested,
2.2.6 Flexible Bag. Any leak-free plastic (e.g., Tedlar, Mylar, Teflon) or
plastic-coated aluminum (e.g., alumni zed Mylar) bag, or equivalent, having a
capacity consistent with the selected flow rate and time length of the test run.
A capacity in the range of 55 to 90 liters is suggested. To leak check the bag,
connect it to a water manometer, and pressurize the bag to 5 to 10 cm H^O (2 to
4 in. HoO). Allow to stand for 10 minutes. Any displacement in the water
manometer indicates a leak. An alternative leak-check method is to pressurize
the bag to 5 to 10 cm (2 to 4 in.) HLO and allow to stand overnight. A deflated
bag indicates a leak.
2,2.7 Pressure Gauge. A water-filled U-tube manometer,, or equivalent, of about
30 cm (12 in.), .for the flexible bag leak check.
2.2.6 Vacuum Gauge. A mercury manometer, or equivalent, of at least 760 mm
(30 In.) Hg, for the sampling train leak check.
2.3 Analysis. An Qrsat or Fyrite type combustion gas analyzer. For Orsat and
Fyrite analyzer maintenance and operation procedures, follow the instructions
recommended by the manufacturer, unless otherwise specified herein.
-------
EMTIC TM-003 EKTIC KSPS TEST HETHOD Page 3
3. SINGLE-POINT, GRAB SAMPLING AND ANALYTICAL PROCEDURE
3.1 The sampling point in the duct shall either be at the centroid of the cross
section or at a point no closer to the walls than 1.00 m (3.3 ft), unless
otherwise specified by the Administrator.
3.2 Set up the equipment as shown in Figure 3-1, making sure all connections
ahead of the analyzer are tight. If an Orsat analyzer is used, it is recommended
that the analyzer be leak checked by following the procedure in Section 6;
however, the leak check is optional.
3.3 Place the probe in the stack, with the tip of the probe positioned at the
sampling point; purge the sampling line long enough to allow at least five
exchanges. Draw a sample into the analyzer, and immediately analyze it for
percent CQ2 and percent 02- Determine the percentage of the gas that is N^ and
CO by subtracting the sum of the percent CO* and percent 0, from 100 percent.
Calculate the dry molecular weight as indicated in Section 7.2.
3.4 Repeat the sampling, analysis, and calculation procedures until the dry
molecular weights of any three grab samples differ from their mean by no more
than 0.3 g/g-mole (0.3 Ib/lb-mole). Average these three molecular weights, and
report the results to the nearest 0,1 g/g-mole (0.1 Ib/lb-mole).
4. SINGLE-POINT, INTEGRATED SAMPLING AND ANALYTICAL PROCEDURE
4.1 The sampling point in the duct shall be located as specified in Section 3.1.
4.2 Leak check (optional) the flexible bag as in Section 2.2.6. Set up the
equipment as shown in Figure 3-2. Just before sampling, leak check (optional)
the train by placing a vacuum gauge at the condenser inlet, pulling a vacuum of
at least 250 mm Hg (10 in. Hg), plugging the outlet at the quick disconnect, and
then turning off the pump. The vacuum should remain stable for at least
0.5 minute. Evacuate the flexible bag. Connect the probe, and place it in the
stack, with the tip of the probe positioned at the sampling point; purge the
sampling line. Next, connect the bag, and make sure that all connections are
tight.
4.3 Sample at a constant rate. The sampling run should be simultaneous with,
and for the same total length of time as, the pollutant emission rate
determination. Collection of at least 30 liters (1.00 ft ) of sample gas is
recommended; however, smaller volumes may be collected, if desired.
4.4 Obtain one integrated flue gas sample during each pollutant emission rate
determination. Within 8 hours after the sample is taken, analyze it for percent
C02 and percent 02 using either an Orsat analyzer or a Fyrite type combustion
gas analyzer. If an Orsat analyzer is used, it is recommended that Orsat leak
check described in Section 6, be performed before this determination; however,
the check is optional. Determine the percentage of the gas that is N« and CO
by subtracting the sum of the percent C02 and percent 02 from 100 percent.
Calculate the dry molecular weight as indicated in Section 7.2.
-------
EMTIC TM-003 EMTIC MSPS TEST METHOD Page 4
4.5 Repeat the analysis and calculation procedures until the individual dry
molecular weights for any three analyses differ from their mean by no more than
0.3 g/g-mole (0.3 Ib/lb-mole). Average these three molecular weights, and report
the results to the nearest 0,1 g/g-mole (0.1 Ib/lb-mole).
5. HULTI-POINT, INTEGRATED SAMPLING AND ANALYTICAL PROCEDURE
5.1 Unless otherwise specified by the Administrator, a minimum of eight traverse
points shall be used for circular stacks having diameters less than 0.61 m
(24 in.), a minimum of nine shall be used for rectangular stacks having
equivalent diameters less than 0.61 m (24 in.), and a minimum of 12 traverse
points shall be used for all other cases. The traverse points shall be located
according to Method 1. The use of fewer points is subject to approval of the
Administrator.
5.2 Follow the procedures outlined in Sections 4.2 through 4.5, except for the
following: Traverse all sampling points, and sample at each point for an equal
length of time. Record sampling data as shown in Figure 3-3.
6. LEAK-CHECK PROCEDURE FOR ORSAT ANALYZER
Moving an Orsat analyzer frequently causes it to leak. Therefore, an Orsat
analyzer should be thoroughly leak checked on site before the flue gas sample
is introduced into it. The procedure for leak checking an Orsat analyzer is as
follows:
6.1 Bring the liquid level in each pipette up to the reference mark on the
capillary tubing, and then close the pipette stopcock.
6.2 Raise the leveling bulb sufficiently to bring the confining liquid meniscus
onto the graduated portion of the burette, and then close the manifold stopcock.
6.3 Record the meniscus position.
6.4 Observe the meniscus in the burette and the liquid level in the pipette
for movement over the next 4 minutes.
6.5 For the Orsat analyzer to pass the leak check, two conditions must be met:
6.5.1 The liquid level In each pipette must not fall below the bottom of the
capillary tubing during this 4-minute interval.
6.5.2 The meniscus in the burette must not change by more than 0.2 ml during
this 4-minute interval.
6.6 If the analyzer falls the leak-check procedure, check all rubber connections
and stopcocks to determine whether they might be the cause of the leak.
Disassemble, clean, and regrease leaking stopcocks. Replace leaking rubber
connections. After the analyzer is reassembled, repeat the leak-check procedure.
-------
EMTIC TM-003 EHTIC HSPS TEST METHOD Page 5
7. CALCULATIONS
7.1 Nomenclature.
MJ • Dry molecular weight, g/g-mole (Ib/lb-mole).
%C02 3 Percent COj by volume, dry basis.
^2 a Percent 02 by volume, dry basis,
%CO » Percent CO by volume, dry basis.
%N2 - Percent Nj by volume, dry basis.
0.280 » Molecular weight of N2 or CO, divided by 100,
0.320 * Molecular weight of Og divided by 100.
0.440 » Molecular weight of CO- divided by 100.
7.2 Dry Molecular Weight. Use Equation 3-1 to calculate the dry molecular
weight of the stack gas.
Md - 0.440(%C02) + 0.320(%02). + 0.280(%N2 + %CO) Eq. 3-1
Note; The above equation does not consider argon in air (about 0.9 percent,
molecular weight of 39.9). A negative error of about 0.4 percent is introduced.
The tester may choose to include argon in the analysis using procedures subject
to approval of the Administrator.
8. BIBLIOGRAPHY
1. Altshuller, A.P. Storage of Gases and Vapors in Plastic Sags. Internationa)
Journal of Air and Water Pollution. 6:75-81. 1963.
2. Conner, William D. and J.S. Nader. Air Sampling with Plastic Bags. Journal
of the American Industrial Hygiene Association. £5:291-297. 1964.
3. Burrell Manual for Gas Analysts, Seventh edition. Burrell Corporation,
2223 Fifth Avenue, Pittsburgh, PA. 15219. 1951.
4. Mitchell, W.J. and M.R. Midgett. Field Reliability of the Orsat Analyzer.
Journal of Air Pollution Control Association. 26:491-495. May 1976.
5. Shigehara, R.T., R.M. Neulicht, and W.S. Smith. Validating Orsat Analysis
Data from Fossil Fuel-Fired Units. Stack Sampling News. 4{2):21-26.
August 1976,
-------
Time
Traverse
pt.
Average
Q,
1 iter/min
% dev.a
a % dev. - (Q - Qavg)/Qavg x 100 (Must be <|10%|)
Figure 3-3. Sampling rate data.
-------
EPA METHOD 10
-------
I
4
I
•m
« 3 Performance RvnluiUtin Teat* Thr
ownrr nf • IMar syBlem flhcll »no|ert aiirli *
Ildtr MyBlem to the performance irerlflrmilon
ImUi descrlbe-d In flection 1, prior to llrnl tine
nl thin method The annul! calibration *hall
be performed I of three Beparmle. complete
mm uxl In* reiillta ol each ihould be re
carded. The rmuirmwnu of Section 111
mint he fulfilled lor each of the three rum.
Oner thr condition* of Ihr annual calibre-
Unit are luJflllrd the lldar (hall be aubfected
to the routine verification lor three aepa-
rale complete rum. The reqiibwnenui of
Section 1.1.1 mtal be fulfilled lor each of
the three nina and the reaulla should be TV
corded. The Admtntatrator may requaA that
the rnulll of the performance evaluation
be submitted lor rctlev.
6. HrftiruefM
8.1 The UK of Ud*r lor
Source OlMcHr Determination, U.8. En»1
ronraenlal ProirrUon Acrncy. N«tlon*l En
forecmenl lnve«U«KUon* Center. Denver.
CO. EPA MO/I ItXIOJ R. Arthur W Dyb-
dmhl. current edition INTtS No, PBtl-
B J FVM evmliMltaii of Mobile Udv for
Lhf Mpuuremml of 8mokr Plume Opadly,
US Entlronmerital ProtecUon Afenef, N«
Uon* I enforcement InivftlgmUons Center,
Denver. CO. EPA/MIHC T8 IM. FVonnrF
ma.
ft,} Remote Hemmrement of Smoke
Plume TmramUuMicc U/dm Ud&r, C, 8.
Coot. O W, Beihlc, W. D. Conner (EPA/
RTF I Applied Optk» II. p« 1141. Augucl
1012.
i.4 Udar Sludk* of SUck Plume* In
Rural and Urban Bnttroninefila. BPA-iSO/
and Sr«lHrtl»
II Rente 0 to l.ooOppm
1.1 SetwlUitlr Minimum detectable con-
omtratlon ta 10 ppoi for a 0 to 1.000 pom
I, tmtrrfrmfft
An? cutetance hartn* • rtfon* ataorpUon
of Infrared ti'iti'lf vtll tnterfere U> anne
for eiampte, dtacrfmbiailon ralloa
lot wal« (H.O> and cmrbon dtoilde ICO.I
arc I.S perccnl ttJO per "I ppra CO and I*
percent CO. per 10 ppra CO, reapectlnlr.
tot devfeMB nitaxirl 1^1 In Uw I.6OO to l.OM
ppm ran«e Par deih«« nuaiurlril hi Uw 0
to 100 ppm range. Interference ratioi can be
M hlfh a> I.S percent H.O per a ppm CO
and 10 percent CO, per M ppm CO. The uae
of illtca «el and aac*rlu> trap! anil allevlale
the major Interference problem!. The meu-
ured tai relume muit be corrected If Iheae
trapa are uartl.
< PrwrtUcm and 4rc«ra<-w ' •
41 Prectolon. The precMon ol mail NDIR
tnalywra It iptiroilmately ' 2 percent of
ap*n.
f .1 Accuracy. The accuracy of mart NDIR '
anaJrcen It approilmKlely *5 percent of
apan after calibration.
S, Apvanttvt
•.I ConUnuoui Sample
rrfnore partlculBt* matter.
1.11 Air Cooled Condenaet at Eqalralrnl
To remove any eicne moWar*.
B.1.1 Valve. Hevdle valve, or equivalent, to
to adhi*t no* rate
B.1.4 Pump. L«ak free dlaphracm type, or
equivalent, to limnavorl t*».
B J J Rale Meter. Rotametcr. or equiva-
lent, to nmmre a now range from O to i.o
liter per mtoi (0.01& cfm)
' Mention of trade namea or apedfk prod-
ucui don not conntltute endorarmeni by tne
l^ivlrnnmpntal ProlrrUon Airncy
763
-------
6.1 a Pleilbl* But, Tedlar, or equivalent,
•lilt a cajwcur or an LO BO men n to i n M.
Leak lot Uw !•• In the laboratory before
using by evacuating bag with • pump lol
loved by a dry gai meler. When evacualton
U oampJete, there should be no (torn
through the outer.
1.1.1 ntoi Tube. Type 8. or equivalent, at
lacked La tin prate so thai Uw sampling
rue can be reiiuaJed proportional to the
•lack gat leloCUr when velocity ti varying
with UM Umc Jf a sample irm*erae hi con-
ducted,
1.1 Amlnw. OVure 10-1).
•.I.I Carton IkfanoiUe Analner, Nondav
peraln Infrared apeelrocneter. or equlvaJeaL.
Thai IntniBOil atuuld be (temonalraled.
preferably by Uw manufacturer, to meet or
•loeed BajHifidurcr'i apeelJtcmUoni and
InoBt ihaiTliiil In into method
•,l.l DrytiHr Tube To contain approil
cutely W0«of irtlkWfel.
I.I.l ChUbrajlim Oat Refer 10 •ection « I.
§-M Fitter. M recommended by KDIR
manufacturer.
6. 3. a R»Ur Mctrr Rolametrr or equivalent
Lo mrraiure |U How rale of 0 lo 1.0 liter per
mln (O.0]6efm> through NUIR.
6.3.9 Recorder (oolionol). To provide per
manc-nt record of NDIH readlnfi.
a. I Callbrailon Uaoei, Known concvntrv
lion of CO In nitrogen IN,) for Instrument
•pan, prepurUled ande of N. for aero, and
two additional fonrenmtlorui cormpondlni
approxlmalelr to 8O percent and 30 percent
apan. The be
•lUilei ±1 percent of the •peclfled eonoen-
trmuVon.
rir
1.1.1 CO, Hem oval Tube. To contain ap-
proximately BOO i ol ucmrtte.
• IB la Wab?r Bath, for ucartte and
•Ulca eel tubea.
6.1.1 Valve. Needle valve, or equivalent, lo
adjual flow rauc
•-] Silica O«l. Indleallnc type. • to It
memh. dried al US' C (111' P» for 9 noun.
• 1 AMmrlle. ConuncrcUlly available.
1. Procrd«re
1.1 BampUnr
1.1.1 ConUnuoui Bamptkni. Be*, up the
equtpmefil aa «hown in Figure IO-I nuullnc
•ure ail eannecUoni are leak free. Place UM
probe In Uw «Uea at a aunpltna point and
purge UM aampUng line. Connect the ana
and begin drawing aunpte Into the an
Allow • Ddnula for the intern 10
aUbUtw. then record UM ftnalywr rcMttnt
aj required by UK leat procedure. (See aec
UoDl.1 Mid •). CO. oonLent el Uie IBB m»y
be dctlennlned by udnt the Heihod > Inle-
fraied g§t^^ procedure, or by welching the
aatartle CO. removal tube and cwnpuUnf
CO. concenLnUon from the fu votunie
aunpied and the weight gain of Uw tube.
1.1,1 lnle«TBled Sampllna Evacutlr the
neilbM bag. Bet up the equipment a* ahown
In Figure 10-1 with the baa dboannected,
>PUoe the probe kn the Mock and purie IM
aampllng line. Connect the bag. making aurc
that all connection* are leak free. Sample al
a rale proportional u> the lUck yelocttr
CO. content ol Ihc ga* may be determined
by ualna the Method 3 Inlearaled (ample
proBerfura, or by weighing the aaculte CO.
removal lube and computing CO. concentn
164
linn (rum the gas volume sampled *"rt ll11"
vrlllii vain ol llir lulx-,
1.Z CO Analysis A-urmble the «pp«r»lus
aft shown In FTfui* 10-1, rallbrale Ihr In
slrumrnl and prriurm other rrqulrrd oprr-
alloni u described In Brcllon 8, Purge ana
lyzer vllh N, prior to Introduction of each
•ample, Direct the wimple stream through
the Inalrumenl for the Led period, record
Ini the remdlnga. Check Ihe lero and wan
•t^ln alter the lest Lt> auure thai any drill
or malfunction U delected. Record the
umple dala on Table IO-I.
8. Co'iftmfion
Aowcmble Ihe apnaralm accordlni lo
Figure 10-1. Generally an Inalrumenl re
gulreo a warm-up period before stability IB
obtained, follow me manufacturer'* In
ilrucllona for ipeclflc procedure. Allow a
minimum lime or I hour for warm-up,
During thti Ume check Ihe cample condi-
tioning apparatus, I.e., filter, condenser,
drying lube, and CO, removal lube, la
erunire lhal each componeni la In good oprr
allng eondlllon. Zero and calibrate Ihe In
mniment according to the manufacturer's
procrdum using, ropecllvely. nitrogen and
the callbrallon ga
10-1— FIELD O*T*
Ctal I
a. CoJi ulo/ion
ConcentraUon ol carbon monomlde. Catcu
late Ihe concenlraUon of carbon monoilde
In the Black using Equation 10 I .
en. 10 i
Wher*:
C, ,, ,10.1 Conrenirallon of CO In slack, Dpm
by vulume (dry basb).
(.*,„ unit Coin, nlrsltoo at CO mcufurKl by
NIMH aiialy/j'r, ppm by volume (dry
' i *",„, Volume Inu-lluii of CO, In ssmplr I c ,
pvrrenl CO, Iruiri < >ri.»l analysis dlvldrd
by IOO
IV drirr nui fvr t r used M an si
lernillvr In (lip slllrs gel and aacarlie Irapa
II. BIMioorupAt
II I Mi-Elroy. Prsnk. The Inlertech NDIR
CO Anaiyzrr, PresenLed al Iliri Melh-
ods Confrrrnrr on Air Pollution, Univer-
sity of California, Berkeley, CA. April t.
tano.
11.2 Jacobs. M B, el al.. Continuous De
Irrmlnallon ol Carbon Monoilde and
Hydrurif bolts III Air by a Modified In-
frarrd Anilyxrr. J. Air Pollution Control
Auorlallun, Mil: 110 1*4, Augiul I»B»
II.] MSA LIRA Infrared Qai and Liquid
Analyur In&trucllan Book. Mine Salely
Appliances Cu . Technical Producla Divi-
sion, PllUburirh. PA.
11,4 Modrb 21SA, 3I*A, and 1IBA Inrrmred
Analyicn, Beck man InjtrumenLs. Inc.,
Beckman liislrucllona Ifllb-B, Puller
ion. CA. OcLubrr 1M1.
lt.5 Conllnuous CO Monitoring Byaleoi,
Model AMI I. I tiler Lech Corp.. Prince
ion. HJ
116 UNOR Infrared Oaa Analyaera,
Bend 1 1 Corp., Honceveiic, WV
A. PERFORMANCE S«ciFic*riOMS FOR NTXR
CARBOM MOHOIHX
> PMCMH linvo
O-IOOOfl
O-IOnv
I0« M • hnn
ccx-ieoo B i. Hj3~»aa
B. DfUnilioni of
tionf.
Kant* The minimum and mailmum
meuuTetnenl llmlu,
Output -Elrclrlcsl signal which \* proper
Uonal lo Ihe measurement; Intended for
connrclliHi lo rraduul or data proceulng
-------
Pl.M,
A.NUth. 10A
Jcmroew—The degree of acreement be-
tween a measured value MM! Uw lru« value:
lOJuallr eipnawad at * percent of full icale,
flM0 to 9t pefcmf rvquww—The lime In-
terval from • atop change hi the tnpul con
eenUmtkm ml the tartrumctil Inlet to • rad-
ii* ol 90 percent of lit* ultimate recorded
(M fwnwnJ)— The Intern) be-
reepooae time and tana to 00
atter aatep Inert an In the
fait n«M (M p*ft*ttf>-The Intern! be-
mittol Mepone* UBM and tine to M
i after a *tep deereue In UM
If- 1-«9 edition)
cracklnf unit cmtalint retenerklon
CFR
I.I Principle. An uitesrMad p» tunplc i,
eitncted from the itack. paaaed tnumjJt to
ftlkallne permanonau ipluUon to remove
•ulfur and nltrocen oihfaa, and collected bj
ft TedUr baf, The CO ooncenLraUon In th«
•junpte la metiured •pectraphotometjleaji.
indnf the reaction of CO with p-*uirunino.
betagokadd.
I.I. RoHetamttSntitioUw.
M.ll Rome* Appraibnataly I to IBM ppn,
CO. Hunptei haTtnt ooaomtimUont belo*
400 ppm are analyMd at 415 inn, and
pie* hartnt oonaentrmtiOM above «M
Zero Drift—The change In
output over a •toted time period, uwallv at
noun, of unadjuatod continuous operation
when the Input concenUaUon b i
ly expreaved a* pereent full acale
Spaa Drift—The change hi
output over a eUled time period, uwally H
of unadjuaiad eontinuaua operation
the Input concentration to • dated
nnenale value; uraally eipraeeed 01 percent
full ecaje.
Practotom—The degree of afreentent be-
tween repeated meamunoment* of the aame
ooncenLraUcn. mpfieand M the avenge de-
vtatlon of the atngle remit* from the mean,
NMat—Sponlaneoui dewlaUona fraa a
i output not eaund by Input oanoentra-
shantee.
Llneartrr—The "•«•'•«•""» deviation be-
I an actual tmtrument reading and the
predicted by a atrabjhi line drawn
> upper and lower calibration potnu.
tnoir ojr CAMBOB
>« m Cnmrrna
lf(MRDUpa Bws-
1. JppHeaMIUv and frlKtob
/,J JppHcaMJU|L Thb) method mppUa to
the meuurement. of carbon monoxide (CO)
at petroleum nrftoertaa. Thb method icrTea
u the reference i»^«i»«»^ In the relative ac-
eurBef teat for Bondltperai*e Infrared
(NDIR) (JOoanttououi embalon monlUirtnc
•TStoma (CBaVV) thai are required to be In-
stalled In petroteum reflneria on Huld cmu-
j.lt SautUvU* The detecUoa limit h I
ppm bated on three Umee the ctaDdard dovt-
atloo of the mean n>a«ent buuui vkluea.
I.I fHCfrJkmian. Sulfur aihtaa. nltrfe
oxide, and other aekl VMM mUrfere viut
the OBkrunetite iuaii*l«»i They are remond
br paawjv the MMpled !•• throufh an alka.
lutlon. Carbon dtorinwt dcee not Inter-
fere. bat, h*re,i»e H h lemmeJ by the ecrub.
bum aolution, IU eonMnlratian roust be
mcMurnd Independently and an appropriate
Minimi eorreetlon »»««A« to the nmplnl gam,
J,S Pneitiou. Accmraet. amd StotHHtv.
I SI Fraetffam The ertlmated tniralaborm-
tory •taodBtd devtaUon of the method bj I
percent of the mean for |mi mmplee ana-
Ijced In duplicate In the concentration
rmnce of U to 411 ppm. The InterLaboratorr
preeMon he* not been ecUbltohed.
I.&.I Aeemmef. The method eontalia no
atfitiflcant faiaeee when cnmpar«d to an
NDIR enalner allhrated with National
Bureau of SUodardi CNB8) rtaudarda.
I.5.J StoMlU*. The Indlvlduml oomponenU
of the eotortmetrie ne«ent are •UUe for at
leaat I month. The eoJortmelrfc: re*c«nt
mint be uaed wtthm 1 dan After prepara-
Uon to avoid emoeavlve blank oorracUon. The
•tmplea In the Tedlar • bat ahould be etable
for at toaM 1 month U U>« ban are leak
1.1 Sampling. The •ampUnt train b ihown
In Flfure IOA-1. and component parui are
dlacumed bekrw:
1 afenUoD of trade names or commercial
product* tn thb) pubUcallon doea not conatl-
lute the endoraemenl or raoommendaUon
for use by the QivtronmenLal Protection
Aaency.
RAM HIIIM,
i—- JU«T V«|VI
figure IOA-1. Sampling train.
M.J
Probe. atalnlCM Bteel,
ika, or equivalent, equipped with •
wool plui to remove partlculaU
Sample Cmdttianina Sfitem. Three
unplncera connected In
with leak-free connection*
2.I.J Pump. Leak-free pump with BUlnleei
•Uel and TeHon part* to traniport lamph
at a Row rate of 300 ml/mln U> the Heilbh
bag.
t.l.t Suroe Tarn*. Uutalled between Uw
pump and the rate meter to eliminate lh<
pulsation effect of the pump on the rau
meter.
-------
EPA METHOD 6C
-------
T
ft. M, Apat. A. Matfh. M
Tit* lajTipllna train I* uvmblrd as slin»n
In Plfure 4A I, eicepl ihr uoproijamil bub
bfer U MM included. Thr piabe miul br
he&lcd la a temperMure aufflctciii lu ore
ten! water condenaatlon and nuM Include •
(liter tenter In aUek. out«f Mark, or bollil
lo prevent parlknOaU rntrammeni In I he
peroxide Unp»n«rr» TIM electric tupply fur
the probe heM rttould be nmllnuoui and
veparate from the lined opeiailun «l the
adjual Ihe IHorr iwlteh 10 nprrale In llH
"on" paalthMi (rum 1 u 4 mlnulem on • I-
hour repeating cycle or other rycte apeclflad
In In* apnllcaDat n*uIaUan. Other liner m-
aurnce* ntir be wed •llh the realrteUon
Dial the total •"•ft* wolume coltascud la be
twcea l» and M IU*«» '<* **** MBOuala of
.-—pj^ reatenu preacrmed In ibJi
method
^Af mid Braver to the lank until Ihe In-
plngcn •ad byHHefa Me covered ai leaat
ta-o-ihtnkj ol Incty lerujlli. The
lecied lrot_ —
Ugh* II Imnlni eomtUloM cttM, the mi
pfcrkje* tlrti'""" and Lite «aUr bath utual be
protect**.
Morm: Bamtrtl'1 mar be conducted eon-
Unuoualy If • to* Itow rat* MOWtc puna i»
U> 4* ml/rain lor U«e rraaenl volume* de
•cilocd M into BMhodi to ui«l Thru Ihe
Ikner twitch u MM netetaaiy In addition. II
UK *r—f** oump kt deavjned lot cooilant
rat* •atnpUna. »** me meter may be defcl
ed The U*aJ Ml volume coHeeied ahouM be
between U and M men (or the aeaounu of
•aojDttna- reagent*, nrrerrtbed In into
Milled.
411 L«ak Chech Procedure The leak-
enact procedure la I he ame u deaertbed In
Method •. Section « 1.1
111 SUB*** CMIrciton nrrord the UO
UM »» faa oMMf readme To tacaln Mm
pUng povUlon the Up ot
meicl|> l »
IttM/odn u IndlcateO b? »« rotajiwler
Aiaurr Ihal Ihr ttaaer It oprralln* ki Inlrnd
ed. Ic.. In the "on" puulion lur Ihv demlred
period and the cycle rrpraU an ri '^ttlrH
Durinf I he 14 ho.il taropline period,
rrcord Ihe dry IU meur Irrnprraiure one
Ibae b*i»«-n CM am tnd MM am and
the berofotUlr prrwurr
Al Ihe concliuhMi ol Ihr run lurn all Ihe
iimtr and Ihe aamplr pump, rerouve ittt
iwobc from Ihr Ukrk. and rrrurd the Unit
|U iM-Irr >oiumr rradinf 4'uixliu-i a Irak
rhcc* M dru-rlbrd In Srrlloii « I I II a Irak
U lound »okJ Ihr tut nm ui "w pturrilurn
arrrul«olr lo Uir Adnibililillor lu ad|uki
Ilir uniplr vulumr fur Irilair H»|N •( Itit
40 CM Ch I (7-l-OT Edition)
ilrps III HllS wrl 1(111 14 I 1> Itir liu I I .'JIKr
nini
I a Samplr Kenwrry Thr puprfiliirrs fur
samplr r«l>*rry iriuUKluf oirasufrnu'llt.
urrinlfle coluiioit. ami ('<>• anuwbrTJ arr
tlir &amr ai In Mrlliod«A, Hrfilim « 1
4 J Samplr Analyali Analysis of ilir prr
oildr Irnplnaer solulhHU l> the &une ai In
Melnod B, Srctlun 4.1.
44 Quality Auurance «JA> Audit Sam
plea. Only wlien thla method I* uw;d lor
compliance deirrminailon*. obtain aii audll
fa-tirf*" aet a* directed In Section l.l.l ol
' •. Analyie the audit *ampln ai
„ for every M day* of umple cat-
and report the reaulta aa directed In
Section 4.4 of MeUiod 4. The analyal per
lonjiUMj Ibe *—*f*" aaalyie* ahall perform
DUE 1.^*i aoajvaea. II marc than one analy*!
perforocd lb* .BBBapto aoalyta during the
M-day mfr"*^ paraud, each analyal ihall
perform UM audll analraea and Ml audit re
aulU ahall be reported Acceptance criteria
for the audit raautla are the aamc a* In
Method •
ol Metering amtent.
B I I Initial Calibration, The Initial cill
oration lor the volume meter In* ayMem U
Ihr tame ai f or Method e. Beet km ft I I
B I.I Ptrtodic Callbralton Check Alter
10 dayk of opermUiM ol the teal train, con-
duct ft calibraUon check w In Srctton all
•hove, eacept lot the lollowUia variation*
i 11 The leak check U not to tor conducted,
Hi Hirer or mare revolution ol the dry .u
mct« mud be used, and ill only Ivo Inde
pnulent run* need be made II the "libra
lion lactar doea not deviate by more than &
percent Iron the Initial calibration factor
determined In tfccuan 611, then lite dry
eu meter •alime* obtained durliuj Hw tot
Mrtn are •ccepuhlc and uae ol thr train
can continue. II the c»Mbr«lloo factor de.l
alem by more than 4 percent, rrrallbralr Ihe
metering MUem aa tn Srctlun ft I I: and l«
the calculallona lor lite precrdlm JO day* uf
data u«e Ihe caJIbrMtun larlur (Initial ur rr
ralloralunl that yield* the loner «u
(oliune [uf each Irai run. U«e Ihr l»Lrs) call
bratlun factor for aucrmlini trU*
51 -niemnnnelfri Calibrate M*""'
mercury In «laa> Ihrroionwui" Initially and
al M day iiilerMui
S J Hotaraetrr, Tlw roiaoirlrf nr*d nu«
ur raltbratnl, but inouM be rlraiml a»d
nialnlalited arcordlii* U> the maiiii(aflur«'»
liulrurllon*.
»4 Uarumrlrr Calibrate aaaliul • "" '
i in ir baronrlrr liuliilly and al M U*y nili-i
vals
ib llarlum rrrrhlwralr thiliilimi iila"
clulir llw Iwiliim prn'hluialr M»l«lli'i»
aaaiiui Ji i»l "' Hi'Mlaitl MI||IIII>' «• I•" I"
•ratoctten Aoan«y
vhlch 10" ml ol |OO percml ujupropanol liax
Dren added.
The nonwiKliliirr and calculation prorr
dura are I IK umr ai In Unhud HA villi
the followlni eirrptUNu:
K_ Initial haruaielrlr plruurr for Ihr lest
period, mm HI,
T. -Abeolute meter temperature lor the
levl period. 'K
1 fnufioa Hale Proftdurf
The rmuaktn rate procedure U the same
ai dracrlbed In Method «A. BCCIUHI 1. ricept
that the timer la needed and U operated la
ikacrlbed In thta method, Only when thta
method ta uaed for compliance detennlna-
ttona. perform the QA audit anMyan aa de-
anlbed In flection 4.4.
Ft 60, App. A. AUth. 6C
nii'iil vyslrin fur a nrll ilrilfnrd ayclem,
I li< mliumiiin d< In l»bli Miiijt should be Iru
than 3 per<~«nl ti' tlir apan
3. fV/ini'luni
3 I Mrastirrinriil Sy\lnn The Uilal
ninlpmrlil rt-cjulicJ l conuriuouj
Ir eitneted Iran a clack, and a portion of
the iMBBte l« conveyed to an Inalruooenlal
inalyan for delermtnaUon of 8O. iaa con
atnlrmUon umlng an ultrmrtolel (IIVl, Dondbi-
perdre taf rated tHDIRI, or nuoreaccnx an
alyaer. Performance apecUICMloni and leal
pracedurCB are provided to enaure reliable
data
1 tame* aad Smttiuil*
I.l Analytical Hanae. Tne analytical
rftiyjr la determined by Ihe Inatrunkental
amaii PIM thla mrihod. a potilon of the an
•lylleaJ ranar U aclcaed by chooaln* Ihe
•pan of the monllorbuj •y*iem. The apan ol
Ihe monltortnl ayitem ahall be (elected
•uch that Ihe pullutanl iu onncenlrallon
rquliralenl lo Ihe embalon Mandard U not
Ini than M percent ol the apan If al anr
lime during a run the meaaured fa* conceit
linlun tmcinlm UM auan, Ihr run iliall br
< niulOjred Invalid
1 2 'BeruUllvHy III* inliilinuni drlc-rublr
Hinlt depend* on II" aiulfUcal rangr, i|iau,
XHl signal LuiitiUir IBlIu ol ilic niraitiir
I I.I Samiilr lutrrlare. Thai poriion ol t
Byiirm uard lur intf ui more al lite fullav
ln«: uniple argjUlilon, aatnpat tranapon,
lample corulniiMilna. of protection ol the
analyxen Iruni Ilir effecu of the aUck ef
fluent.
1.1 1 Uaa Antlner. That ponton of Ihe
lyilem that aeiura Ihe lu lo be measured
and lenerale* an output Drnportlonai to IU
concentration
I.I.I DaU Hecurder A ilrlp chart record-
rr, analoi computer, or dbjilal recorder for
rrcordlruj meauirernent data from Ihe ana
I pier output.
11 Span The upper limit ol the «u con
cenlrallon meaHireme»l rtrtge dlaplared1 on
Hie data recorder.
J.I Calibration Oa» A liiovn concentra-
tion of a iiu In an appropriate diluent «aj
14 Analyter CMIbrallon Knot The dll
ference beLvrrrn Ihe |ai eoncenlrallon el
hlblled by Ilir fu analyier and Ihe kmwo
concentration of Ihe calibration fa* »hen
Ihe calibration iai U Introduced directly lo
the analyver
1 ft Baraulliti ByMem Bla*. The differ-
ence between ihe eaa conceit traUoni eihlb
llrd by Ihe mrafeuremenl (viumi vhen a
known concentration tag li InUoducnJ al
Ihe outlet of the umpllnt probe and when
Ihe *aaw iaa U Introduced directly lo Ihe
analyier.
J« Zero Drift. The dlfieierae In Ihe
meaattrcmcnl lyilem output rcadlns Iraot
the Initial calibration rrowocue al Ine aero
concentration level after a ataJed period of
operation durliuj which no unatlteduled
maintenance, repair, or adjuauaeol loot
place.
1.1 Calibration Drill The dJflermce In
Ihr meaiuremenl lyiteoi output reading
from the Initial calibration reMponae at a
mid ruujc calibration value after a dated
prrlud ol operation durlm aihlch no un
arheduled maintenance, repair, or adjual-
rarnl took place.
l.a ttnpuruir Tim* The amount «f «m*
rmulred for Ihe meaiureoxnl lyatem to dta
play M percent uf a itep chanae In |u con
rrntralUiii on Ihr data recorder,
10 Inlrilcrnu-e t!heck A method lur de
Irclttu/ aii*lrlli-al liilrrrcreiuei aiMl eicrt
iltr Ulftr* I liriiuili dlrrrt foflinaruun ol |U
i ixu rnliill.nu proklilrd by Ihr mraiuir
Illriit ar>lrm UiU by • mrtdlflrd Mrlhud B
luiH-rdurr fur llll> rhn'k. ll« modllrrU
702
-------
Mrlhorf • aainplrt «rr aro,ulrrd ml ilir
urnplr bf paai diirliargr ""I-
] 10 Calibration «:••«* * grapli «" «H«rr
•rilemallr melhod ol "labllshlng «'«" rela
Unruhlp between Ihr analvwr rrs|«niiar and
lhe actual gal concrntrallon Inlrodiirrd lo
the analyser
4 Mn*mrfm**l $Mlr/orme««rr Sprri
Hffltomt
4 I Analyatr Calibration Error Lett than
11 percent of the *l»an for *"« **ro, "«M
range, and high range callbralhm turn
« 1 flantpllng System Btaa l«aj than • 5
percent of Iho BPOJI for Ibe «*ro. UM! mid or
high -range calibration gaga.
* 1 Zero Drift. l*m than ' * percent of
the anan over the period ol each run
t 4 Calibration Drift. UM than ' ' Per-
cent of IN* a»an over the period ol each
run.
«• Interference Check, l on • Ml baato; lor Iheae analyxera. 111
heal the aample llnr and all Interlace ram-
panenla up la the Inlrl ol Ihr analrvr lull!
rtenlljr lo prevent rnfKJrramikjn and (It dr
Irrmtnt Ihe nxiljlurr mntrnl and rtxrrrl
the meaaured iu roncrnlralloni Ui a dry
hwrta ualni approprlaU melhoda. nubjrcl lo
Ilir «|i|ii'iv«r of Ihr Administrator The rtr
icintlriB'I'Hi *»l s»m|«lr m»l*!*irr riMitrnt IK
iiitl tirrr.vtaiy lor tNilliilaitf snalrfet* ItiM
inraaurr rnnrrnlnlhiru iin a "H bail* whrn
III a »r. The filter shall be
boroaltlrstr or quaru glajs wool, or glaat
liber mat. Additional fillers al Ihe mlrt or
outlet "I the motatunr rrmoval ayiaevn and
Inlet ol the analyser may be uard) lo prevent
amonulaUpn ol partlculate material In the
meaaurevaenl lyMem and eitend the uaelul
life of the eomporwnU All Illtetm ahall be
labrlcaled of mnlerlah thai are nonieacUvt
lo Ihe gai being aampled-
B.I.T Sample Pump. A teaMrac pump, to
pull Ihe sample gaa through the ayatei* at a
How rate lufftcktnt to ndnlmbc the re-
sponae lime of the measurement system.
The pomp may be constructed of any male
rial that b nonreacttve to ih« gas being asm-
pled
Big Sample Flow Rale Control, A
•ample flow rate control valve and rotame-
Irr. or equivalent, lo maintain a constant
campling rate within 10 percent.
(Htm. The tetter may elect to tnslajl g
bark premrr regulator to maintain the
•ample gaa manifold al a constant prtavjirr
In order to protect the analvaeHit from
overpreaiurttBtlon, and U> mlnlmtae Ihr
need lor flow rate ad|u»4mrnU I
S.I .g Sample das Manifold. A sample gag
manifold, lo divert a portion of the aamplr
gaa stream to the analyser, and the remain-
der to the by-paai dbcharge vent.. The
•ample gas manlloM should abn bidudr
nrmblong for mtiwducmg rallbraUon gaan
directly la the eralvver. The nuuilfoM may
br conrlructed ol any material that b non
leacUve lo Ihe gai being aa/nptrd
SI 10 OSJP Anslrser A UV or NDIR ab-
aorptlon or fluorescence analyan. to deter-
mine continuously the SO. oonccntraUon In
the sample gai llrram. The analyser ahall
meet the ap»>lteab!r performanoe aprdflca
lions of Section 4. A means ol controlling
the analyser flow rate and a device for de-
termining proper sample flow rate «e.g., ore-
ctaton rotameU>r, pressure gauge down
•tream of all flow controb. rlc.I shall be
provided at Ihe analyser.
• I Nora- Housing the aralywrlil In a rlesn.
thermally MaMe, vibration tree environ-
ment will minimize drift In the analysrr
rernrdrr rrtnlullnn tie. readaMllly' shall
be OS perrrnl ol iipan Alter nail. fly. • dl(l
Ul ur analiif mrtrr having a rranlullon ol
».» peneiM ol »l>»n map br iiard lo »lit«Jn
the analyirr rnpomea and the rradlngi
may br remrded manually II Ihb all*rn»
live la uaed, the reading* shall be obtained
al equally ipaced Interval o»er the dura
Itan ol Ih* nunpllng run For aampUng run
W to M prrcenl of the apan
- 1.1 1 Zero Oaa. CancevvU»Uo« of Mai
than •.» percent of the apan. Purified am-
Went air map be aged for the aera pw Irr
paavJng air through a clmiooal IHUr. or
through one or mote bai»tia|iia containing a
aorulton of I percent
• . MrasmrrmfXt SftttlH f¥r|bnvMnc* Trlt
51 II flau llecordrr. A *lrlp chart re
rordrr, analog computer, or digital recordr''
lor recording meuuremenl data. The data
Perlorm the tallowing- prondura before
inemaurrnxnl al emlatlona (HecUon Ik
1,1 trallbratlon Cla« Concenl rattan Verlfl-
rallon There air two alUrnallvrm for eata*-
Halting the eonrentrallorwi of rallbralltai
gueit Allernallvr Number I !• preferred,
• II AJirrnallve Number I Die ol rail-
brillon (asm Dial arr analyzrd Inlkiwln*
the En*liu (NMaln a rertlHralloii
from Ihr ga« manufacturer I Hat l*rol«rol
Number I van lolluwrfl
• 12 AKrinatlvr Nitmtirf 1 <)w ol rail
hralliin gwx n»l |»ri*f«l BrriwiHng lo Pto
tornl Numbrr I II Ihli allematlve I* rhaaen.
obtain «a» mlilurni with a manufarlurer'•
lolrranrr rail to eirred 11 nerwnl ol the
lag value within * months before the rtnto
•ton leal. analy«r each ol Ihe calibration
gaar* In triplicate uMn« Method • Citation
1 In the nbUographi' dncrtbca procedwrea
and Udintojuea that may be uaed for thai
analyala Record the i-eauHi on a data aheel
leiamcie to ahoam In FlgTrrr tC-ll. >ach of
Ihe mdmdual SO, malyllcal Manila for
each calibration gu ihall be wNMn • per
on* (or • npm, whtolievet la greater> of the
triplicate ael average: otHervlgc. dtacard the
entire aet, and repeal the litnlteatc analy
aeg. If the average of the irtpllraU- analfaca
la •Mhte S percent «f the caMbmtan tag
manufariurrri cyllmtor tag- value, oae UM
lag value: othervlw, conduct at leaat three
alyaea until the eeauHa ol ati
rurv agree with S percent lor •
ppm. whlchevvr la gn>alcr* of thrlr average.
Then uae Ihtm average for the eyi '
value
•.1 Mtaauiement
Haarnililf the meaaw rment lyvtem by fol-
loving the manufacturer • vrlUen matruc
Uona lor preparing at id prramdHlanlng UK
gaa analvcer and. aa awlleable. Ihe other
•yatcm comonneiNa. Introduce Ihe calibra-
tion gaaea to any aeaoenee, and malt all
in 11 a»ry ad)uaunenli lo calibrate Ihe ana
lymr» and the data ncorder. Adluat ayatcoi
componenla to achieve vM'iett aampling
rale*.
• 3 Analyarr fTallbrallon Error Conduct
Ihe analyarr rallbrat Ion error check by tn
U educing calibration gaata to the aneaatrre-
men! •yatem at any inolnl upatrewn of Ihe
gag analrarr aa loltowi
• 1.1 After the. mcaaurement ayatem haa
been prrparr-J for uie. Introduce Ihe atro.
MM-range. and high lange gaata to the ana
lyatr. During ihb rlwck, make no arihaa1
menu lo Ihe ifmirtn i?icept thoae neoeaamry
lo achieve the correct calibration gaa flow
rale el Ihe analyaer. llecord the analywr re
auoiawa to each calllvatlon gaa on a form
almllar lo Figure «C 4.
Norm A calibration rurve ettabltehed prior
lo the analycer rallbratlon error check may
be uavil lo convert the analvaer rmxirue to
Ihe equivalent gu concentration Introduced
to the analyirr- Howrvrr, the aame rorrec
Uon prorediirr shall I* uard lor all effruenl
and calibration mrawirrrnrnU obtained
during Ihe Int.
• 11 The analynv calibration error
rherk ihall br rmtsMcred Invalid II lh« gaa
roncentrallon diaplayinl by Ihr analymer ei
rrrda i 1 prrrrnt of ttie apan for any of the
rallbratmn gasn If ail Invalid calibration b
nhlbilrd. takr cnrirrLl»r action, and repeal
704
705
-------
N. M. App A. MfhV 6C
IIM aiulyur rillbralloii nun rlirrh unlil
•cceplabh- perfor manrr L. t<-|i»->i> * fonn auallar to
ftgtar 1C & Then introduce l Ihr IIIM in. L\
•nil iM-gln ftfeniiiNim Bl I lit* .t*
«.«! The lunptti* n*Han Mat check
•Itoll br cwukWred Im&Ud If Ihc diflercm
bvtBcen Ihe cu amccnlralhini Oliplftirnl br
Ihf araaurenml •mica fw Ihc uulner
ndltvulaa rrrar check mat lot Ihe un>plin«
Milfio bfac check g«mdi I ft pticenl ol Ihe
H*o far either Ute ten* or »p«rmir ccllbre.-
Uao MB II an Invalid calibration b eihlMl
at. lake comcUvr aeUon. and refteu Ihe
pcrlwiaaan to achieved II Mlhuuotni ID
Ihc ao*irm l« raqdlred, lint repeal the an
alpiet caHarBUao erroi check. Iten repeal
Ihe canwllni lydeia blai enrtfc .
1. gmttMo* Tat Pmettmi*
1.1 aetecttan erf aaoplini BMc and 8am
I th* awne criteria that
ar. apfjlrahfcy to HeUwd I
1.1 Imerterenc* Check Preparation tte
each individual analyarr. conduct an Inler-
fereoce check lor at lea** three run* i
. on •
Retain the rraulU, and report
then •Mi each teal performed on that
•ouree category
II an Interference check to being per
funned, aarmbte the modified Method 0
Irani (fh»r coblrol valve, I wo midget Ink
ptngen containing I percent H.O, and dry
iu eoeterl an ahown In figure tC 1 Install
the ammpllru) Italn la obtain a lamptr al Ihc
measurement iyal*m aamplr by paid dto
charge vrnl Heroid Ihr IniMal itry iaa
mcLer i
ll Inn I In
ici-nnlit
ii' rali* AN
Maintain constant rair *ain luui Ur. ' IU
perrrnil during Ilir rnllii- run 'I'lir *ain
pliiig lime pel run iliall br Hit- &amr a,-, fur
Mr!hud S ului lailcr Ihr *y*li-rn rrspuiur
lime. Mir earn run. utr only thuie mruurr
menu oMalnnl after I wire rctpanac lime of
the mrainrfmrrl lyiicm haa elapaed. lo de-
termine the average effluent concenlnllon.
II an Inlcrlciencr check to being pel formed.
open the (lo* conltol valve on Ihe modified
HeUtod • tratft foncui-renl «llh ihr Infit-
atlon of the lampJIng period, and ad|tui the
Do* lo I Uler per minute i i 10 percent i.
< Nam |l a pump to not uaed In Ihe mudl
fled Method • Ualn. caution ahould be earr
la adlueUng the flow rale alnce
of Ihe bnplngrn nuy
ler Italn. result-
ing in poaWwIr
l.« Zeio and OkllbrmUon Drill Teau Ifn
coetUateiy prarrmnar and follaailna each run.
or II art|nBla-*rn Ihc mraauremeni lyatem until
after Ihe drill checkj ate campleled.l
Record and analner'i reepnnara on • form
abullar to Figure *C i
1.4.1 If rllhe* the aero or linaratr callbrm
lion value excecdl the ammpltna »ytt*m bUi
apeclftcatlon. then Ute run to eonaldered In
valid nepemt both the •nalnef callbratkm
error cheek procedure larctlon «.lt and the
aarapUng ipatcna ntoja check procedure I See
Ikan •.<»before repealing Ihe run.
711 If both the Beroand upacaJe callbra
IKm value* are •ItlUn ihe campling ayitem
Ifkcatlon. lorn uee UM kveraar of
I fuutl blag check value* to cal
cuutc the gal caoccntraUon lor the run. II
the ana or upscale caUbrmUon drtli value
eicecdk Ihc dflfl UntU. hgatrt on the differ-
ence between Ihe aaapllng tntaa bUa
check I'm-*—-t BtunetttaUIr before and
arur Ihe run, repeal both the analyun call.
brallon erroi check procedure iBeellon • ll
and Ihe aampllng mien bUa check pioce-
dure l&ccUon t.tt before condLining addl
Uonal run*.
l.ft Inlcrferenot- OMCB lit prrlurrnedl
After completing the run, nmrd ihe final
orr aai meter reading, mclci Lenperatiire,
awl buametrlc pravjun Recorer and ana
lyic Ihe conunu of Ihe mldcei Implngen,
and determine Ihe HO, faa cuirrnlrallun
ualiig Ihe prucidurei of Melhud a ill u ni>l
no ratal y Iu Biialyie EI*A perliirmanrr
audit •ampin lor Hrihud 6 > IteUfrmliir llir
avrragr van ruiicrnliailun *ililbllril by Ilir
aiialyur fur Itir run II itir gai> ruiuriilra
llona
by ihr analyzer mkO itii-
rllMid 0 ililin by mure Him,, ^
prrtenl of Ilir mmltlicd Hrlriud 6 ri-kitll,
Ihe run U Invallilalr.d
a Cmiiilun Calculation
The kveraf' fa* rfflurnl riinrenlrMlim Ii
delrrmlnrd Irum Ihe avrrafr iai cuiu fnlr»
llun dUpuyed by Ihe |U aiuilrwr. and L.
ad|iuled lot the if to and tiuacalr imjnplliuj
•yaiem buu check*, u deUrmined In aceord
ance ullh Becllun T.4. The «»erMe ia> Con
cenlrailun dtopuyed by Ihr. •nalyur m*y be
deunnlned by tnuirallon of the area under
Ihe curve for chart tccurders, or by iverac-
Iruj all of Ihe el fluent meuuremenu, Alter-
lUllvely, Ihe averaie ra«y be catrulmied
from meBiurenwnU recorded aL equftlly
Ipaced intervaU over the entire duration of
Ihe run, for lunpllruj run duraihwu of leu
Irian I hour, owuurenunui al l-muiulx In
lervab or • minimum ol 10 meaturemenu,
whichever to leu reslrlcliic. •hall be uicd.
Por tarapllruj run duration! ireaur than I
hour, mramurenenu •! 2 mlnule InLrrraU
or • minimum of M meuiiremenU, which
ever to leea restrictive, «h*ll be lued. C«ku
late the effluent |at conctnlrnlon luiiuj
EquaUonM.* I.
Whrrri
^•^ Kflliii'iil MAA I'liiit-riiiiailon, dry baala.
ppm.
C Avmni- MIU ••iinrrnuBiloii liulicaled by
cat Bjitlyu-r, Jry baili. Dpm.
C. . Avert*.' ul Inllikl and final lyitem call-
brailuii dial, itlieck reipmuea for Ihe icru
•a*, pptii
L*_ . Afrrayr „( lull 1*1 and Iliutl lyilem
CBlUu-Bltun lilu clirck rcHKHMes for the
UpICBlr CBllbrBlloniu, ppm
<:_ - Actual 1'uiifrntritkin of Ihe upscale
callbrBlkin |B> ppm.
9.
I, 1'rBreaUllly Prolocol lor Eiubltohlruj
True Conrenirilluiu of Gun Hard for Call
braiiocu and AudlU of Conllnuoiu Source
Cmlulun Bfonilnri fruiucol Number I US
eUwlruittneiiltl Hrulrrllun Agency. Quality
Auu/Biure DIvMun. Hewarch Truumle
Paik. N«: Junr |BTi
1. Weillln. I'rtrr H and J. W Hroatn.
Mfllioib fur <'otlnrliii« and Aiulyzlna Qai
Cylliidrr Sample] eiource EvalualkHi Sock
ly Nevilcttei. Jll> 1 It acplcinbrr IM8
706
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S •
•AMBBIIMm Bli* »•» O"IT D*fa
Sourer Idcntiricallon:
Trrt p
Date:
Run number:
Span: _ ...
Dale
Analytic meUrad yard -
Fl«
Oaa
ftnikali
f*to-
Hyslrm
BlM
A*«qp nui to IBM 9mn 0 n p«cam al wan
HUB b» SO to 80 pvo
Piouaj 6C 4 - AJ»L*am c*Li*a«Tioii
Drill
nml an**™ Cal.
Cal Rmixmir AjulfirrCil
Rrmporur „ )00
Span
Initial SfUvni Cal.
Span
Bourn- UnrtJIIeallan:
TcM pvtvmnel:
AiuJrcrr cmllbimtlan dmU for •unpllnt
rum;
Hiram l~Dmmw*no« ov
OMIMI BBIUIOM fuam 8v*Ti(M<
I Pnxrtpir a*4 >tppl*r«frUU»
I I Prtnctplr A into ttmplr b
In an rvKualnl llaak cooUlnln* « dHate
•ulfurtr wld hydro^rn prroiMc •lIMN'Wnt
•olutlon, and Ihr nltraccn omtOtm. cicc«A id-
tr«M nildc. «rr mruurml rolorliwrtrle«M»
unliit Ihr iilirnoldbullnntr arid (PIWi P«o
17 A(>iiltr Lihlllly This mrlhrxl In
bl' In Ilir rrn-MUM-rornl of nllro«pn oiMri
rmlllrtl from sl»Uon«ry >uur Thr ranir
til Ihr inrtlmd IIB.I l»'< n tfrlrrmlnrU In br 1
lu IOU milllifBiKi NO. iu NO. I uri diy
•lantern mMc H»UT. vlUraut Iwdm la
dilute the a/note
I. Avjfrmlmi
1,1 Sunplint im !PI|Utc 1 11. CMItrr ti*b
»7«trmj or rqatpmrnl. canaille ol
liil (•mptr »ilum» to wllhln i 10
and rvlknln* a mrrictmt **mo»r
lo «lto« aiuli'llnl rrprmlurlMHIp to
•llhln i i percent. •!!! br roraMrml m-
rrptablr •llrrtniltn. i.ibjrrl lo atn»ro»Bl ol
thr Artrnlubslrilat. I) 8 Di*ir«mmental Pro
Irctlnn Atriwy Tlir lollovlnf mulpnwnt t»
winl in x*ni|>l!n|'.
1,1 I llobr, flormiliril* flaa luWm. iuf
Ilrlrnllf hr«lrd lo mrvrnl water rot^Vrea
thin and pquIpiHfl with an In Hart m out
• Lmrk flltrr l« rrmo't1 pmrlh-uUlf m«tu-r la
708
709
-------
EPA METHOD 7E
-------
n. to.
40 CH Ch 1(7-1-19!
tftvttM
cttawAi
abould be linear VIUi ihe linear tune, uat
la determine IIM callbra
tahMi renuc cancefMrallan In pi NO. /ml acquired data Round oil llturem allrr final
Do not Ion* the curve Ihroucd trro l(ra» a ralrulallan ,
MMMh cum uinwcn in* i»lnu The cune , , H^mpi, volume. Dry Baal. Corrected
lo Standard Condition Banw a* In Method
1C. Section C I.
• 1 Total M NO. Per Sample
Bq ID-1
Cur* out CBlnitallon*, reuinlnc al lean
a> titn decMMJ flaw* beyond lhal o4 UM
• - 18-Bl *. 160 x
i of MO. a* HO., in Mj&pie. »*
. al MM«ili. ,4 MO. /•!.
of MM*, pfl NO, /•!.
M- Vohoa* of praparad
4a\CI- Moteoalar • iljlil 04 NO.
tlf I - MCMMMf ••KM. of MO.
af KMnO.
H •nruUon.
III
ua.
Protection turner. Re
Pbra. NC. PutaneaUon No
A-tJaVl-Tf-*!™. «l«MI liTI
«, Mutmtmm. J H. « •!. An
HQ.
Ifl
r, Tnh •jctbad H
of
llonary
tne
I J nan Ml n A
ly eiUactcd IrOM a alack, and a porUon of
Io
C.CaaenilraUan of HO. M MO.. dr»
•.4
I • MB HO* I Ml •• HO/H'M BTP
I • BVM HO, - 1*11 iw NO./WM 8TP
1. QaaMlj Omlnt
and «.* •• awiaxtiloaa
romponrnl In the lunpk- fu. ctlltrr than
Ih' la* componcni bclni mruurrd
*. McuBnaWMf lillr* fttfaran.net Sprti
a. Method «C, Scctlom 4 I lltrouili
1.1
Anr mnnin
for NO. IhM najiti Uic avcclfl-
of Uito awUtod A »rt»BMillc of in
Flaw CC I of Mithod tC. TIM
Pi. M, Ap.). A. Merfav t
II 1 Meaiuremrnl Ftytltm Freparatlon An
alrvr Calibration Error and Sample
Hrilna Dial <.lMCfc Pbllo. SectloiM II
ihioua-h • « ol Method ar
1.4 MOt to NO Con.cnian
Unteav data are prcamlcd u>
thai Ihc NO. omnntraUon vfUibi Ihc
•wnple atremm Im not creator than • percent
of Ihc NO. coocmUmUon, >— ~fc— * an NO,
la NO cantrnloa efficiency Lo* to aaonvd-
ara irllh BeMlon • • ol Mellial ».
1. a-Bibnoi Tell
Rate Control. _
Manifold, and Data Recorder
M«Uiod «C. Section* III Uiroawn II*. and
11.11.
I.I.I HO. 10 NX! Convener Thai portion
of UM 11011111 Uial COOMTU UM nKranm dl
oiafa 4 HO.) In the avapHi CM to rwUocm
oiM> (HOI. An NO. lo HO converter to not
i' 'itojaf? If dale art pnamted Io drawn
avmte UuU Ihc HO. ponlon of UM cihaual
CM • ICM than » peromt of UM total NO.
u> de-
t.l.l .
the prtnrlptai of il -
tembM oonUnuoHBtr UM HO. canomirMlon
to Ih* mmolm CM aUcsn. The WMlrwr
•IMJI BMcl UM aptinraM. performaan avec-
irnmikni of BecUon «. A iiimiii of contra*
KIM the analnn Oom ntf and a device for
drtenalntn* prapcr aanaplr no* rate «*• .
1.1 actectlon of
pllnc PMnu. Select a i
iMriiiia t*ina; UM i
Me Io
Metnodl
T.I Barople ColtorUon. fnatllial UM mm-
pllnc probe M the drat i
and begin aampltna- at Ihc i
dunni UM tialun calHmiion drUl icat.
Matnlato amtfanl rate aunnltaj lie . 1 10
during UM entire run Tbc BWB-
Umr per ran chaJI to UM
loUl Umr required la oertora a
Method T. plia ivtae the ty*tra>
UBM. n» each run, oe only Uuac
tOfOtM obtained «fl*r Ivlee UM
time of the
rliparn. u> delcmlnc the a*erm|e einuenl
ranccntrallon.
T > Zero and Callbraibwi Drill Teml
Polio* Section 1 « of Method CC
• Imutiom CalcOmltom
fe»om Section • ol Method CC.
§-• HO. _
Horn BHMI for Uw HO. aaalraer chaU te NO
*" " "^ '"—"— mm ii ajf rtOiI In
i B.I.I. I.I.I, andl.l.l.
1.1.1 NO. lo MO Oanwete*
i (hXV b> UM
Ac- II
BM. Zero
lo The Record. Drill. CaUaraUoB Drtfl. and I
M. IM NH. Interference m Bacoe aa Metnod CC. BtcUoM 1.1
Mrlho*i 1C and TO It
I QoalNy Aianiimmi, Handbook for Aar »» Interference fUavonce. The outpul
Pollulton Miaamiiaiiil ByaUoM Volume reaponat of the airaaummitl iy*ten> ui •
Same a* bjoHaaTaDni of Method «C
rrawai •-IMtawiBirioo OF OOLnmic
Acta Mm *n Souva DIOIIM EHII
MOB* PBOM 8i«rio«uaT flooa
. Conduct an ta
analyacr
prior to Ma IrdUal MM bi UM farld Tncrcaf
tor,, lechara the neaaurmment erMm II
chance* an OMB* In UM tnatnanenlailon
lhal eoutd alter the toterferenee rooMMt
h«( MjHifiimce; rejponat In acrMdanrr
•tin aectkm • 1 of Method »
tilnelod
•nkuwUeally from UM auck. The eulfurie
add rant imclHdlnc aulfur trtoiUe) and UM
irur dtoiMc an arparated. and batn Irac
atparately by UM
ttirfiiai Ihnrtn IMrallnn awlhcirt
II ApnlleaMuty. Ttifel BMlnod at appUca
ale for the determination of auWurta add
MM tlnrludlnc aulfiir Utoilde. and In UM
atoaance of other partlculaM nMllnir and
•dhH dtoiMe inliiliiiM frCM Mallonary
koura CollaiwraUvc toM* haw atwwn trial
ihe mhirnnMD dcteclaote bmlte at UM
mcinod are OM ntllUcranM/eubtc OMter
10M> tc ' poundk/cublc fool I for aullui irt
oilde and I I rnc/B* ICT4 1C ' Ib/fl*) for
•ulfur dloilde No upper IknOi hare been t*
Lanllahed tlaiij on theoretical calculation.
'or MO mlllH*r» ol 1 peraenl nydiocen per
uildr aoluilun, (he uppei concentration
limit lor tulfur dloiMr In a I 0 m'OD.I fl'l
730
731
-------
EPA METHOD 25A
-------
PI, tO. AfMx A. Me*. 1M
40 CHI Oi I (7-1-it
M*h brvri ojlbnllon ft* »l Ihc c&JIbrillon nllmiton iu The •»n«e •Hall or drier
™h» «MtBMr, AdJiBl Uw Winer output rained br the InUvrmllon of in* output r*.
to Uw •evraprfele mch. II mt'iunmrj. Cal ooftBn* o»w in* period iptciried In Uw u>
IbB pndMed naponoe for Ute to* plkaMe rcfutellon
"^*d°n^'!!I!r I'«—IU«« required In tetm. of PCW.M
UM im «Bd Mah cmrtwn. Mt»l mcHurrd conccnlraUam
Eg 2f A 1
C.-KC_
irrtrir Pi i nut lln in
fw Jo« l»»rl and mid Incl
. Mid drtcntilne Uw dlffw _ . , ..
i the iBMuitmml *JT**~ re- i.-urmue oanociHiBiion *• cartun.
*»mn>c cancenMUait H
IBM lllM) § IWffVMDt Of
H m^ « -Cfcrtwn «Qutratent oenwuon taeh*.
K-llafKhmne
MUuKflwnl* to UH>
A-4W/1-
im.».
r nalaml lor ttuMMMm
al OHM UM! fw out-
of
to tfct hUb h»U
Ubanhorr
irn.
Report No. Tt-OA0-«.
U ttw MMt «f Uw U* prrtod.
chart prrtod* of
•Acr bcMi UK mv *od cmllbn
I/ Urn drtft ralon cucvd tto
Uw
fol
io
*jurau«cir KMiflnu tiw tot
•• In JM-
fled period of law.
i to UM MDM M lor Method I O^olAou >od I
•J
OfBI ___^ _
II Boo DrtfL LM UMO ±1 pmo* 01
U CkHbmUM DrUl MM UMD *l Mr- roid« a
(MtofUwwaanla*. to.i
M CuUlinilam ttiar. L^ UMft ±1 per- from • btdk Dtari or i
MMofllMi - - - - "^
•adUManMwsMMiim- 1.1 bHtal *
I. OrVBBtc Ctovcmifralloa CoJrBlarioiu
•*«••* wiui
i of PIKBI u pracuM of alhcr
•ulU «n reported u roluaw concent ralloo
equlvrtcnta of Uw cmllbnlloo «u or **
U ApptMUlUf. Tbto awinad ta MipUc» afutatanf latfraMM.
* lor Uw deaenatattUon of npor U*htma* DM up to «W —• HjO
dcUwrr tank wnlch to H.IMHjO ——
ipor arilBCUan cqulpnwiil. It
Prtnclpla. PIIOHITT *nd >Hniua> ore IcM
•ItenMlclr l
-------
ft. Ml At*. A. Mirth.
40 CM Ck. I <7-|-*« f
ft. M, A.^. A.
ISA
n. u»»
ITaa>rT~ Oipnnmrioa Uaiew a
I. Japririfcritl* mm* J»rtacia4r
I.I ApphcafaUUi TUl. acthod applle* to
tne BMaaMffWaoikt of total gaoMMia organic
of **prn nmia*Mliig prteaaftly
and/or aranae laroeeallc
Tbe ormrnmrethm ki u-
toj Uma of faoMm (or <
rgaofce oaUkmiiaaai ggo» or ea I
1.1 rrtodpte A am
UOTHRk • heated
, U •iruniry. gjul gloai fttwr tUUr to •
liwr fFIAI. llaauMi an
•peciricd lor affected aource caugorlea In
U» applicable pan of the regulatloni Tbc
•pan valuo U ealabllehed In the applicable
refutation and la uaually 15 Ui l.ft lima (hi
applicable embakMi limit II no t,mi, valur h
provided, me • apart value equivalent la I a
la 1» tinea the canceled concentration. Put
convenience, the apart reJue ahould corn
•pood u lot percent of the recorder Kate
11 Calibration Ou A known cxmenlri
Uoaaf • KM in an inpmiiMilg dUueru cu
Lf Z«n» Drlfi. Tne OHIerana In the
» rMpnnM' lo • ten
M* bcrore and after a
of opcnlloa during »hlch na
repair, or adjut
ilimiion
Prate, filauiteue alecl, or
___ Uuachole rake Ifpe BampM
Imlrr ahall ba 4 BUI In *4mf*'«r or amallet
and lotkUd at Ml, H, and U1 percent of
dimeter AUematlvc-
i.a
li. _ _ .
thai a gmm aiaiirHr to ffoltrctcd Iraca the oen-
inlly located It percent area, of the Black
1,1 aaiBpta Line HUlnteu tfecl <•
Taflon* iiiUiii lo irmnaport Inn tampie iu
10 Uw analrarr The MJMple Iliw ahould be
If oaoaaaiv. to prevail eondannv
1.4 CaUbnlkw VaJva AawMhlr. A utrae
•ay tal«a aaaeMolir la dlnct lha acra and
nUntmUoo jaana la Uw an^raon !•
MMM
fU'lMli"^ gaa lo in*
M*.
>• tvUaiMMlm mift. An Imiac* 01 an
oxM-of-etacb glaai fiber (liter to mt\*imtnA
^m || eabouat gaa1 parUculale: leading to atot*
•Uhanl. An out-af*lacs fuut ahould be
healed lo prcveol any eondeneaUoo.
l,g Haoardef. A etrlp-chan recorder,
analog ogeapuler. or digital reourder for re-
data The — *"'——it
r r*qulrenet]( to one neaaune-
i par aunule. Note: Thto gKUiod
often aoolled In highly ciploelve areaa.
In
11 Puel A 40 percent hVgo pcreenl He
or 40 percent H./4O percent H. gae emliluia
IB reeommendcd la avoid an oifaen •rner
llam effect thai reportedly occura vheo
oiraen conceiiLrallon wuie* ilgnif Irani IT
from a mean value.
4.1 Zero Oa« High purity air BflLh leu
(nan o I paru per million by fofuoia (ppoirl
of organic materiel (propane or carbon
equivalent! or leu lhan O.I peroBnl of UM
enan value, whlclwoei !• grealaY ,
4.1 Loo level Callbralhin Oaa. An organic
callnratlon (a* vilh a oanccnlrallan ecjulvm
lent la la lo JS uerceM of UM figt'^M-
apan value.
1.4 Hid level Calibration Oat Anorganic
calibration gai with a coneenlratlon equlva-
lenl la It to » pereeni of Uw apptk»M«-
apan value.
IB Hlgh-lcvrl LrallaraUon Qu An organ-
ic <*alll>ralH>n «w •IUi a eaneciurailan
Equivalent to U la go percent of UM appli-
cable apan value
B, Hcaianrawal SnUm Pirjormemt* Sffft-
ft.l Zero Drill Leu than tJ percent of
the (pan value.
6 J Callbmion Drill, Leu than it per
cent ol epan value.
ftl Calibration Error. Lea* lhan 18 per-
cent of the eallbraUon ga* value.
uaad for eallnratiooa, luel, and com-
Ur (U required) are contained In
gaa qrllnden. Preparation of
aaa ahall be dune aooordUw U
In PttHooo* No. I, Italed In
• I AddUlonallr. UK •anufac-
iwnr of UM cfllndM- •nould pnwuat a rec-
naiaiiiiliililahail life lor aach lalfftnulnn m*»
cyiladat t- rtajuiaUon or purpoae
ol the leal; I.e.. cihauat cuck. Inlet line, etc.
The maple port ahall be tooted at leaai i.a
BeUn or 1 equivalent dlancter* upaurcan
of the gai dKcharge lo ine timnaphrn.
• 1 Location of SwiDfile Probe. InalaU UM
aampte probe ao thai the prate la eatinlly
located In the alack, pipe, or dud and la
ecaled Ughlly al ihe alack pan connection
gl Meaaurmrnl BiraUeB rnparallan.
Prior to Ihe cnlulaa uet. tmtmblr UM
meuumaenl eyitcm fallowing UM caaau
fadurer'e «rut«n liMtmoUoaa to preparing
UK (ample Interlace and UM organic aoaiy*-
er. Make the •rum operable
HA equliMaeiu can ba niltinuii for
almomt any laiige of total orgaolcB coneen-
traUona- fat high eoncefltratlniia of organ
fca <>!.« percent by MMUBM aa propane)
modlfkatloni u meat aeeuaonly available
analyaera arc neceuaiy. One anmnii«d
melhod ol eouJiMDem BMMBflcaUan U to de
crcaM Ihe tlMt al ihe laatple te the analyaer
through Ihe UK of a eaielle
»«.— l»i- cainllary, CHrect and
meaeurcflMnl ul urgank connenimlnn la a
neceeaary consider ailon «hen detcraUnuig
an* modification dtalgn.
• « Caubralloii aVrar Teei. leuBCdlaUly
urlot la Ihe Lcii ierlea.
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