Asphalt Emission Test Report: Mathy Construction Company New Richmond, Wisconsin


United States        Office of Air Quality
Environmental Protection   Banning and Standards
Agency          Research Triangle Park, NC 27711
Air
ASPHALT
Emission  Test Report

Mathy Construction Company
New Richmond, Wisconsin
EMi Report 91-ASP-11
September 1881

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  AP42 Section:       11.1


  Reference Number:  25


  Title:                Emission Test Report, Mathy Construction Company Plant #26,

                       New Richmond, Wisconsin,
                       EMB-No. 91-ASP-10, Emission Assessment Branch,


                       Office Of Air Quality Planning And Standards,
                       U. S. Environmental Protection Agency, Research Triangle Park,

  NC,


                       ApriM992.

Note: This is a reference cited in AP 42,  Compilation of Air Pollutant Emission Factors, Volume I Stationary
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 checked.

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        EMISSION TESTING FOR
    ASPHALT CONCRETE INDUSTRY
        EMISSION TEST REPORT
       Mathy Construction Company
                Plant 26
         EMB File No. 91-ASP-10
          Work Assignment 1.44
         Contract No. 68-D-90054
              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
              April 8,  1992

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                            TABLE OF CONTENTS
Section                                                                   Page

1.  INTRODUCTION	 .    1-1
      1.1    Background	    1-1
      1,2    Overview of Testing Program	    1-1
      1,3    Brief Process and Site Description	  1-3

2.  SUMMARY OF TEST RESULTS  	    2-1
      2.1    Summary of Results	, .    2-1
      2.2    Emissions Test Log	  2-2
      2.3    Metals And Polynuclear Aromatic Hydrocarbon Results	    2-5
      2.4    Paniculate Matter	   2-14
      2,5    PM10/CPM Results	   2-19
      2.6    Aldehyde Results  	   2-23
      2.7    Continuous Emissions Monitoring Results 	   2-33
      2.8    ASTM Methods	2-35

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   	f	    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 25A 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
JBS342                                  U

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                     TABLE OF CONTENTS, continued
Section                                                              Page

6.  QUALITY ASSURANCE AND QUALITY CONTROL		   6-1
      6,1   Summary  	   6-1
      6.2   Quality Assurance/Quality Control Definitions and
           Objectives	  6-2
      6.3   Manual Flue Gas Sampling Quality Assurance	   6-3
      6.4   Analytical Quality Assurance	   6-7
      6,5   Continuous Emission Monitoring Quality Assurances	  6-14
      6,6   Gas Chromatography Quality Assurance 	  6-29
APPENDICES

A     EMISSIONS TESTING FIELD DATA SHEETS
      A.1   PM/Metals
      A.2   PM10/CPM
      A.3   Aldehydes
      A.4   PAH

B     PROCESS DATA SHEETS

C     SAMPLE PARAMETER CALCULATION SHEETS
      C.l   PM/Metals
      C.2   PM]0/CPM
      C.3   Aldehydes
      C.4   PAH

D     CEM DATA
      D.I   Multipoint Linearity/Drift Summary Tables
      D.2   CEMDAS Printouts
      D.3   Stripchart

E     GC DATA

F     ANALYTICAL DATA
      F,l   PM/Metals
      F.2   PM10/CPM
      F,3   Aldehydes
      F,4   PAH
      F,5   Sample Log
JBS342                               m

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                   TABLE OF CONTENTS, continued


G    CALIBRATION DATA SHEETS

H    SAMPLE EQUATIONS

I    PROJECT PARTICIPANTS

J    SAMPLING AND ANALYTICAL PROTOCOLS
     J.I   PM/Metals
     J.2   PM10CPM
     J,3   Aldehydes
     J,4   PAH
     J.5   CEM and GC
JBS342                            1V

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                                   FIGURES




                                                                           Page




1-1   General Process Flow Diagram for Drum Mix Asphalt Plants	  1-5



2-1   PM10 Paniculate Emissions (Ib/hr)	2-24




2-2   PM10 Paniculate Concentration (grains/dscf) 	2-25




2-3   PM10 Participate Catch (in grams)	2-26




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   Pmlo/CPM 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
JBS342

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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	  2-7

2-3   Metals Gas Concentration Emission Rates	  2-8

2-4   PAH Gas Concentration Emission Rates	2-11

2-5   Ratio of Metals to Paniculate Matter	2-12

2-6   Metal Amounts in Flue Gas Samples by Sample Fraction	2-13

2-7   Metals/PM Emissions Sampling and Flue Gas Parameters	2-15

2-8   PAH Amounts in Flue Gas Samples - Blank Corrected  	2-16

2-9   PAH Emissions Sampling and Flue Gas Parameters	2-17

2-10  Paniculate Matter Concentrations and 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
                                               A
2-13  Summary of Aldehyde Emission Factors and Process Operating Data	2-27

2-14  Aldehydes Concentration and Emission Rates  	2-29

2-15  Aldehydes Amounts in Flue Samples - Blank Corrected	2-31

2-16  Aldehydes Emissions  Sampling and Flue Gas Parameters	2-32

2-17  Continuous Emissions Monitoring Daily Test Averages	2-34

2-18  Hydrocarbon Emission Rates and Concentrations	2-36

2-19  Summary of Waste Oil Analysis	2-38
JBS342

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                               TABLES, continued

                                                                           Page

3-1    Summary of Process Operating Data Collected During Emission
      Testing - September 23, 1991 .................................... 3-3

3-2    Summary of Process Operating Data Collected During Emission
      Testing - September 24, 1991 .................................... 3-4

3-3    Summary of Process Operating Data Collected During Emission
      Testing - September 25, 1991 ..............  ........ . ............. 3-5

3-4    Summary of Metals/PM and PAH Emission Factors and Process
      Operating   Conditions   ....................................... 3-6

3-5    Summary of Aldehyde Emission Factors and Process Operating
      Conditions  .............. , .......... , .......... , .............. 3-7

3-6    Summary of PM10/CPM Emission Factors and Process Operating
      Conditions  .... ..................... . ........................ 3-9

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 ........................ 6-8

6-5    Metals Field Blank Results Compared to Test Run Results  ............. 6-10
JBS342

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                              TABLES, continued
6-6   Metals Flue Gas Method Blank Result	6-11




6-7   Metals Method Spike Results ,	,	6-12




6-8   PM10/CPM Field Blank Results Compared  to Test Run Results	6-13




6-9   Aldehyde Field Blank Results Compared to Test Run Results  	6-15




6-10  Aldehyde Flue Gas Method Blank Results		6-16




6-11  Aldehyde 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 6C Sulfur Dioxide Analyzer and Drift, Summary	6-25




6-19  Method IE Nitrogen Oxides  Analyzer and Drift Summary  	6-26




6-20  Method 10 Carbon Monoxide 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
JBS342

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                               1.  INTRODUCTION

1.1   BACKGROUND
      The Emission Inventory Branch (EIB) of the Environmental Protection Agency's
(EPA's) Office of Air Quality Planning and Standards (OAQPS) is responsible for
developing and maintaining air pollution emission factors for a variety of industrial
processes.  The EPA publishes these data in Compilation of Air Pollutant Emission
Factors, commonly known as AP-42.
      In October of 1986, the part of AP-42 that deals with asphaltic concrete plants
was revised by dividing the plants into two major types based on the procedure used to
mix the asphaltic concrete:  continuous-mix plants and batch-mix plants. Following these
revisions, and on the recommendation of the National Asphalt Paving Association
(NAPA), EPA instructed Radian Corporation to direct emission testing efforts at these
two types of plants.
      Mathy Construction Company owns and operates asphaltic concrete plants that
have been cited by NAPA as being representative of both continuous-mix  and batch-mix
plants currently operating in the United States.  Radian has already conducted emissions
tests at Mathy Construction's Plant No. 6, a batch-mix plant.
      This report discusses the results of the testing program conducted by Radian,
under contract to the EPA's Emission Management Branch (EMB), at Mathy
Construction's Plant No. 26, a continuous dram-mix plant located near New Richmond,
Wisconsin,  and one of two asphaltic concrete plants studied for the revision of AP-42.
The testing program quantified emissions of criteria and other air pollutants from the
facility.  The test results will be used by EIB to  update the asphaltic concrete plant
section of AP-42.
1.2   OVERVIEW OF TESTING PROGRAM
      The specific pollutants  of interest in the testing program were particulate matter
(PM); PM less than 10 /*m (PM10); condensible  PM (CPM); sulfur dioxide (SO2);
nitrogen oxides (NOJ; carbon monoxide (CO); total hydrocarbons (THC); polynuclear
JBS342

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aromatic hydrocarbons (PAH), excluding aldehydes and ketones; and trace metals,
excluding mercury (Hg).
      Testing was performed from September 23 through 25, 1991.  The principal
objectives of the testing were to:
      •     Determine levels of CO, SO2, NO,,, 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  Hg was not
             expected to be present in the process  stream.
      •     Determine the filterable PMi0 and CPM fractions emitted from the stack.
      •     Determine the levels of PAHs emitted from the stack.
      •     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.
      In order  to ensure repeatability of results, the above measurements were repeated
in triplicate at near-design operating conditions while the plant was operating on waste
fuel oil.
      Flue gas  concentrations of C02, O2, NO^ SO2, and CO were determined using
continuous emissions  monitoring (CEM) systems designed in accordance with EPA
Methods 3A,  7E, 6C,  and 10. 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  aldehydes and
ketones, respectively.  PM10 and CPM were sampled by means of three  test runs, a
combination of protocols outlined in EPA Methods 201A and 202, respectively.  All ot
JBS342
                                       1-2

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the manual method flue gas samples were analyzed in Radian's Perimeter Park
laboratory facility in Morrisville, North Carolina.
1.3 BRIEF PROCESS AND SITE DESCRIPTION
Continuous mix plants operate in the following manner. The cold feed material
known as aggregate is hauled from storage piles and placed in the appropriate hoppers.
The aggregate is transferred to a set of vibrating screens and classified into as many as
four different grades (sizes). The classified material then enters the drum mix operation.
The drum mix process uses proportioning feed controls in place of the hot
aggregate storage bins, the vibrating screens, and a mixer, which are used in a batch mix
plant. Aggregate is introduced near the burner end of a revolving drum mixer, and the
asphalt is injected midway along the drum. A variable flow asphalt pump is linked
electronically to the aggregate belt scales to control mix specifications. The hot mix is
discharged from the revolving drum mixer into surge bins or storage silos.
Drum mix plants usually use parallel flow design for hot burner gases and
aggregate flow. Parallel flow designs have the advantage of giving the mixture a longer
time to coat the particles with asphalt and to collect dust in the mix, thereby reducing
paniculate emissions. The amount of particulate generated within the dryer in this
process is usually lower than that generated within conventional dryers, but because
asphalt is heated to high temperatures for a long period of time, organic emissions
(gaseous and liquid aerosol) are greater than in conventional plants.
In recent years, old asphalt is removed from the road base and is broken up at a
job site. This material is then transported to the plant, crushed and screened to the
appropriate size for further processing. This recycled paving material is then heated and
mixed with new aggregate, to which the proper amount of new asphaltic cement is added
to produce a grade of hot asphalt paving suitable for laying.
Direct flame heating is typically performed with a drum mixer, wherein all
materials are simultaneously mixed in the revolving drum. Split feed drum mixers were
first used for recycling in 1976 and are now the most popular design. At about the
midpoint of the drum, the recycled bituminous material is introduced by a split feed

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arrangement and is heated by both the hot gases and heat transfer from the superheated
virgin aggregate.
      The unit tested is a mobile 330-ton-per-hour-rated unit that is fired on waste oil.
The rotary kiln dryer/mixer is a co-current design similar to that shown in Figure 1-1.
The oil-fired burner fires into the upper end of the kiln and induces air flow around the
annular area between the kiln and the burner.  This  arrangement provided approximately
30 percent of the air through the burner, with about  70 percent induced through the
annular area.
      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 quality assurance/quality control
(QA/QC) procedures followed in the test program.  Appendices to this report include
detailed methods and procedures, field and laboratory data, and complete calculations
used in deriving the results presented here.
JBS342
                                        1-4

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Coon* Aggr«0al*
$1009. PIU
liCIHP
 	* Emission Points

MM Dueled Emissions

MM Process Fugitive Emissions

fca Open Duel Emissions
                                                                                                                       Exhatol
                                                                                                                       Siocfc
                                                            H«at«d Atphalr Sl
                                                                                                                       Truck Load-out
    Figure 1-1.  General Process Flow Diagram for Drum Mix Asphalt Paving Plants

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                        2.  SUMMARY OF TEST RESULTS


2.1    SUMMARY OF RESULTS

       This section provides  the results of the emission test program conducted at Mathy

Construction Company's Plant 26. Included in this section are results of manual tests

conducted for trace metals (excluding Hg), PM, PM10, CPM,  aldehydes and ketones, and
PAHs. This section also contains the results of the  continuous emissions monitoring

(CEM) for CO2/O2, CO, SO2, NO^ and THC gases, as well as gas chromatography (GC)

results for benzene, toluene,  xylene, and methane.

       The following list summarizes the significant  emissions from Mathy Construction's

Plant No. 26:

       •     Of the 15 metals analyzed, 11 were found in detectable quantities. Their
            average emission rates (Ib/ton of product) were:

                   Arsenic      1.80 x W6;
                   Beryllium    4.81 x 10^;
                   Cadmium    0.66 x 10^;
                   Chromium   11.8 x 10"*;
                   Copper      6.05 x 10"6;
                   Lead        6.02 x 10^;
                   Manganese  11.3 x lO'6;
                   Nickel       15.1 x W6;
                   Phosphorus  54.9 x 10"6;
                   Silver       1.36 x 10"6;
                   Zinc        52.6 x 10^.

       *     Of the 22 PAHs analyzed, 1  was found in detectable levels.  Its average
            emission rate (Ib/ton of product) was;

                   Naphthalene 0.690 x  10".

       •     For PM and PM10  the average emission rates (Ib/ton of product) were:

                   PM                      0.014;
                   PM10                     0.005;
                   PM10 +  condensibles       0.040.
                                       2-1
JBS342                                   *• x

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      •     Of the 18 aldehydes analyzed, 13 were found in detectable quantities.
             Their average emission rates (Ib/ton of product) were:
                   Acetaldehyde                   134 x 1(T5;
                   Acetone                        82.7 x  10"5;
                   Acrolein                        4.83 x  10'5;
                   Benzaldehyde                  11.2 x  10'5;
                   Butyraldehyde/Isobutyraldehyde  16.1 x  10"5;
                   Crotonaldehyde                 8.62 x  10'5;
                   Formaldehyde                  203 x 10"5;
                   Hexanal                        10.9 x  10'5;
                   Isovaleraldehyde                4.10 x  10"5;
                   Methyl ethyl ketone             2.52 x  10"5;
                   Propionaidehyde                13.3 x  10"5;
                   Quinone                        15.6 x  10'5;
                   Valeraldehyde                  6.70 x  10'5,
The following sections present more detailed discussions of the results of this test
program.
2.2   EMISSIONS TEST LOG
      Emissions testing was conducted over a three-day period, from September 23 to
September 25, 1991,  Table 2-1 shows the emissions test log, which includes the test date,
sample location, run number,  test type, run times, and average asphalt production rate
during testing.  Testing was performed using EPA manual test methods for six different
analytes. Testing was conducted  in triplicate for each type of analyte.
      Paniculate 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, and
then was combined with the back half for total metals analysis.
      The PAHs were sampled concurrently with PM and metals by EPA SW 846 Test
Method 0010 using a dual  probe  arrangement, which 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
JBS342
                                       2-2

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                             Table 2-1. Emissions Test Log
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09/23/91
09/23/91
09/24/91
09/24/91
09/25/91
09/25/91
09/23/91
09/23/91
09/24/91
09/25/91
09/23/91
09/23/91
09/24/91
09/23/91
09/23/91
09/24/91
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JBSJ43
                                             2-3

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                                    Table 2-1, continued

09/23/91
09/23/91
09/24/91
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09/23/91
09/23/91
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JB5343
                                               2-4

-------
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.
A combination of CEM and GC instruments was used to sample for 11 other
analytes. To the extent possible, these tests were conducted concurrently with the
manual method tests. 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.
2.3 METALS AND POLYNUCLEAR AROMATIC HYDROCARBON RESULTS
2.3.1 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 emissions
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
(acenaphthylene, ancenaphthene, anthracene, benzo(a)anthracene, benzo(a)pyrene,
benzo(b)fluoranthene, benzo(g,h,i)perlyene, benzo(k)fluoranthene, chrysene,
dibenz(a,h)anthracene, dibenzofuran, 7.12-dimethylbe'nz(a)anthracene, fluoranthene,
florene, indeno(l,2,3-cd)pvrene, 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 of the PM/metals
train was broken during shipment, so only the front half was analyzed for PM and metal
content.
The remainder of this section discusses process operations, average emission rates,
metals-to-PM ratios, and metals amounts in the flue gas-by-sample fractions.
JBS342

-------
2.3.2 Process Operation
Table 2-2 summarizes the metals and PAH emission factor results along 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 217 tons/hr and 287 tons/hr (72 to 96 percent of capacity). Waste oil fuel use
was not determined because no accurate method to evaluate fuel consumption was
available.
The PAH emissions from asphaltic concrete plants may originate from fuel
combustion; the volatile fraction of the asphalt cement, if any; and organic residues that
are commonly found in recycled asphalt (i.e., gasoline, engine oils). Because there is no
fuel use information for this facility, the emission factors presented are expressed in
ib/ton of product rather than Ib/ft3 of fuel oil. During the emission tests, the plant was
operating at near normal capacity, with Run 1 at 96 percent, Run 2 at 90 percent, and
Run 3 at slightly lower than 72 percent capacity. Although Run 3 of the PAHs was at
the low end of normal production capacity, it was still within acceptable limits (within
±20 percent of each other) and was used with Runs 1 and 2 in averaging. The
production rates for Runs 1, 2, and 3 were 287 tons/hr, 270 ton/hr, and 217 tons/hr,
respectively.
Only the metals and PAHs detected are giveruin Table 2-2. The other metals and
PAHs were analyzed, but they were not collected in detectable amounts. Eleven of the
15 analyzed were detected (As, Ba, Cd, Cr, Cu, Pb, Mn, Ni, P, Ag, and Zn). Of the 22
PAHs analyzed, only naphthalene was detected. The metals and PAHs detected were
blank-corrected and reported as shown.
2.3.3 Emissions
Metals
Table 2-3 presents the metals emissions results for the three tests. The date,
metered volume (in dscm), O2 concentration, and flue gas flow rate for each run are also
shown. Flue gas concentrations are given in terms of /ig/dscm and jig/dscm corrected to
7 percent O2. Oxygen concentrations were determined from CEM data (see Section 2.7).
JDS342
2-6

-------
Table 2-2
SUMMARY OF METALS/PM AND PAHS EMISSION FACTORS AND PROCESS OPERATING DATA
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Date
Production Rate (tons/hr)
Virgin Aggregate Rate (tons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cement Rate (tons/hr)
Perce nt of Rated Capacity (%)
Aggregate Moisture (%)
Burner Setting - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exii Temperature (degree F)
Stack Flow Rate (dscfm)
Stack Flow Rate (dscf/ion of product)
Stack Temperature (degree F)
Stack Moisture (% volume)
Slack CO2 (volume % dry)
Stack O2 (volume % dry)
Stack CO (ppmV)
Control Device
Arsenic (Ibs x 10(-6)/ton of product) a
Barium (Ibs x 10(-6)/ton of product) a
Cadmium (Ibs x 10(-6)/ton of product) a
Chromium (Ibs x 10(-6)/ton of product) a
Copper (Ibs x 10(-6)/ton of product) a
Lead (Ibs x 10(-6)/ton of product) a
Manganese (Ibs x 10(-6)/ton of product) a
Nickel (Ibs x lO(-6)/ton of product) a
Phosphorus (Ibs x 10(-6)/ton of product) a
Silver (Ibs x 10(-6)/ton of product) a
Zinc (Ibs x 10(-6)/ton of product) a
Paniculate Matter (Ibs/ton of product)
Naphthalene (Ibs x 10(-4)/ton of product) b

09/23/91
287
193
83
11.4
96
3.8
96
51.1
86
NA c
18000
3765
326
31,1
9.2
10J
42.9
Baghouse
1.49
4.14
0.266
15.6
4.31
4.66
5.64
25.1
43.7
1.04
38.9
0.0169
0.540

09/23/91
270
183
76
10.8
90
3.6
77
60.2
43
NA c
17900
3981
326
31.1
76
10.0
46.9
Baghouse
0.915
0.370
0.588
18.6
4.39
5.28
14.1
19.8
48.4
1.66
49.7
0.00968
0.935

09/24/91
217
147
61
9.4
72
4.2
51
56.0
59
347
17900
4952
328
2S.8
7.2
11.8
129
Baghouse
2.99
9.91
0.965
1.26
9.43
8.13
14.1
0.458
72.8
1.38
69.2
0.0167
0.594


258
174
73
10,5
86
3.9
75
55.8
63
347
17900
4233
327
30.3
8.0
10.7
72.9

1.80
4.81
0.606
11.8
6.05
6.02
11.3
15.1
54.9
1.36
52.6
0.0144
0.690
a = 1 x 10(-6) or (0.000001)
b=lx!0(-4) or (0.0001)
c - Not available due to faulty plant instrumentation.
NOTES:  Run averages were calculated from readings taken periodically throughout the duration of the emission lest run.
        See Table 3-1 and 3-2 for the individual readings-
        Metals and PAH compounds analyzed, but not detected, are not included in this table.
        Metals and PAH concentrations have been blank corrected.
                                                 2-7

-------
Table 2-3
METAL GAS CONCENTRATIONS EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Arsenic
Barium
Cadmium
Chromium
Copper
            (ug/dscm)
            (ug/dscm @ 7% O2)
            (g/hr)

            (ug/dscm)
            (ug/dscm @ 7% O2)
            (g/hr)

            (ug/dscm)
            (ug/dscm @ 7% O2)
            (ug/dscm)
            (ug/dscm @ 7% O2)
            (g/hr)

            (ug/dscm)
            (ug/dscm @ 7% O2)
            (g/hr)
 6.31
 8.30
 0.193

 17.6
 23.1
 0.539

 1.13
 1.49
0.0346

 66.3
 87.3
 2.03

 18.3
 24.1
 0.561
 3.67
 4.69
 0.112

 1.49
 1.90
0.0453

 2.36
 3.01
0.0720

 74.9
 95.6
 2.28

 17.6
 22.5
 0.538
 9.65
 14.7
 0.294

 32.0
 48.7
 0.975

 3.12
 4.75
0,0950

 4.07
 6.20
 0.124

 30.5
 46.4
 0.928
 6.55
 9.23
0.200

 17.0
 24,6
0.520

 2.20
 3.08
0.0672

 48.4
 63.0
 1.48

 22.1
 31.0
0.675
                                      2-8

-------
Table 2-3 (Continued)
METAL GAS CONCENTRATIONS EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Lead
(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)
Manganese   (ug/dscm)
            (ug/dscm @ 7% O2)
            (g/hr)

Nickel       (ug/dscm)
            (ug/dscm @ 1% O2)
            (g/hr)

Phosphorus  (ug/dscm)
            (ug/dscm @ 7% O2)
Silver
Zinc
(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)

(ug/dscm)
(ug/dscm @ 7% O2)
 19.8
 26.1
0.607

 24.0
 31.5
0.734

 107
 140
 3.26

 186
 244
 5.69

 4.42
 5.81
0.135

 165
 218
 5.06
 21.2
 27.1
0.646

 56.5
 72.1
 1.72

 79.6
 102
 2.43

 194
 248
 5.92

 6.68
 8.52
0.203

 200
 255
 6.08
 26.3
 40.0
0,800

 45.4
 69.1
 1.38

 1.48
 2.25
0.0451

 235
 358
 7.16

 4,47
 6.81
0.136

 224
 340
 6.81
22.4
31.0
0.684

42.0
57.6
1.28

62.6
81.3
1.91

205
283
6.26

5.19
7.05
0.158

196
271
5.99
                                     2-9

-------
During the emission tests, P had the highest average mass rate, with 6.26 g/hr,
followed by Zn, with 5.99 g/hr. These emission rates correspond to an average emission
factor of 54.9 x 10"6 Ib/ton of product for P and 52.6 x KT6 Ib/ton of product for Zn.
After blank correction, Sb, Be, Se, and Tl were not collected in detectable amounts for
any of the runs during these emission tests. Metal values ranged from 0.0346 g/hr of CD
in Run 1 to 7.16 g/hr of P in Run 3.
The metals values for the emission tests are not significantly different between
runs except for As, Ba, and Mn. Arsenic varied from 0.112 to 0.294 g/hr, Ba varied from
0.0453 g/hr to 0.975 g/hr, and Mn varied from 0.734 to 1.72 g/hr.
Polynuclear Aromatic Hydrocarbons
Table 2-4 presents the PAH emission results for three test runs. The date,
metered volume, O2 concentration, and fiow rate for each run are also shown. Flue gas
concentrations are given in terms of g/dscm and g/dscm corrected to 7 percent O2.
During the emission tests, only naphthalene was collected in a detectable amount.
The average mass rate was 54.8 g/hr. These emission rates correspond to the average
emission factors of 0.690 x 10^ Ib/ton of product. It should be noted that naphthalene
may be a degradation by-product of the XAD absorbent used in the sample train.
However, these results were blank-corrected and are reported as shown. The
naphthalene values ranged from 39.6 g/hr in Run 3 to 77.6 g/hr in Run 2.
2.3.4 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 0.0157 mg of Cd per gram
of PM during Run 1 to 5.12 mg of Zn per gram of PM during Run 2. Phosphorous had
the highest ratio for Runs 1 and 3, with 2.58 mg metal/gram PM and 4.34 mg
metal/gram of PM, respectively.
2.3.5 Metals in Flue Gas By Sample Fraction and Metals m_Flu_e Gas Sample
Parameters
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
JBSM2 2-10

-------
Table 2-4
PAH GAS CONCENTRATIONS EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Naphthalene  (ug/dscm)
            (ug/dscm @ 7% O2)
            (g/hr)
1540
3170
47.3
2540
4220
77.6
1280
2680
39.6
1790
3360
54.8
NOTE; Concentrations given have been blank correcled. PAH compounds analyzed, bul not delected,
      are not included in this (able.
                                       2-11

-------
Table 2-5
RATIO OF METALS TO PARTICULATE MATTER
MATHY CONTRUCTION COMPANY PLANT 26 (1991)
Arsenic
Barium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorous
Silver
Zinc
0.0878
 0.245
0.0157
 0.923
 0.255
 0.276
 0.333
 1.48
 2.58
0.0615
 2.30
0.0943
0.0382
0.0606
 1.92
0.453
0.544
 1.45
 2.04
 4.99
0.171
 5.12
0.178
0.591
0.0576
0.0752
0.563
0.485
0.838
0.0273
 4.34
0.0826
 4.13
0.120
0.291
0.0446
0.973
0.423
0.435
0.874
 1.18
 3.97
0.105
 3.85
NOTES; Melals analyzed bul not detected are not included in this table.
       Metals have been blank corrected.
                                      2-12

-------
Table 2-6
METAL AMOUNTS IN FLUE GAS SAMPLES BY SAMPLE FRACTION
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)	
          m

Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
ND
7.40
19.3
ND
1.07
76.5
20.4
22.9
26.7
123
203
ND
5.18
ND
180
 ND
 ND
 1.32
 ND
0.254
 1.26
 1.07
0.355
 1.39
 2.22
 14.7
 ND
 ND
 ND
 14.4
ND
7.40
20.6
ND
1.32
77.8
21.5
23.2
28.1
125
218
ND
5.18
ND
194
ND
4.10
ND
ND
1.92
80.5
16.8
20.2
38.7
84.5
194
ND
7.45
ND
199
 ND
 ND
 1.66
 ND
0.716
 3.07
 2.89
 3.50
 24.4
 4.32
 22.9
 ND
 ND
 ND
 24.3
ND
4.10
1.66
ND
2.64
83.6
19.7
23.7
63.1
88.8
217
ND
7.45
ND
223
ND
10.9
34.8
ND
3.52
3.30
34.4
28.7
49.7
ND
248
ND
5,05
ND
247
 ND
 ND
 1.33
 ND
 ND
 1.30
 ND
0.969
 1.56
 1.67
 17.3
 ND
 ND
 ND
 5.84
ND
10.9
36.1
ND
3.52
4.60
34.4
29.6
51.3
1.67
265
ND
5.05
ND
252
ND = Noi detected
NOTE: Meials have been blank corrected.

-------
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.I contains a complete list of these and additional sampling and
flue gas parameters for each run. The field data sheets are contained in Appendix A.I.
Polvnuclear Aromatic Hydrocarbons
Table 2-8 presents the PAH amounts in the flue gas sample for the emission tests
in total /^g 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 C.4 contains a complete list of these and additional sampling and
flue gas parameters for each run, along with the field data sheets.
2.4 PARTICULATE MATTER
2.4.1 Overview
Particulate matter emissions were measured using the front half paniculate catch
collected in the combined PM/metals train. Before performing the metals speciation
analysis, the filter and front half acetone rinse (e.g., tinsate 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 2-7. Detailed sampling
parameters are provided in Appendix C. 1 and analytical results are given in
Appendix E.I.
2,4.2 Particulate Matter Results
The results of the gravimetric analyses are summarized in Table 2-10. Exhaust
grain loadings, corrected to 7 percent O2, ranged from 0.0217 gr/dscf to 0.0413 gr/dscf,
with an average of 0.0330 gr/dscf. Emission rates ranged from 2.61 Ib/hr to 4.84 Ib/hr,
with an average of 3.69 Ib/hr.
Table 2-2 summarizes emission factors for total PM, which varied from
0.00968 Ib/ton of product to 0.0169 Ib/ton of product with an average of 0.0144 Ib/ton of
JBS342
2-14

-------
Table 2-7
METALS/PM EMISSrONS SAMPLING AND FLUE GAS PARAMETERS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
!!y$:ii:l3X$:^
Total Sampling Time (min)
Average Sampling Rate (dscfm)
Metered Volume (dscf)
Metered Volume (dscm)
Average Stack Temperature (deg. F)
O2 Concentration (%V)
CO2 Concentration (%V)
Stack Gas Moisture (%V)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Paniculate Catch (grams)

125
0.330
41.4
1.172
326
10.3
9,2
31.1
18000
510
102
0.0843

125
0.320
39.4
1.116
323
10.0
7.6
30.8
17900
508
97.9
0.0435

124
0.320
39.9
1.129
329
11.8
7.2
28.8
17900
508
100
0.0611

NA
0.323
40.2
1.139
326
10.7
8.0
30.2
17900
509
NA
0.0630
NA = Nol Applicable
                           2-15

-------
Table 2-8
PAH AMOUNTS IN FLUE GAS SAMPLE - BLANK CORRECTED
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
:ffi§;8j|!-::^^
Acenaphthylene
Acenaphlhlene
Anthracene
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
2-CiiioronapthaIene
Chrysene
Dibenz(a,h)anthracene
Dibenzofuran
7,12-Dimethylbenz(a)anthracene
Fluoranthene
Fluorene
Indeno(l,2,3-cd)pyrene
2-Methyl naphthalene
Naphthalene
Perylene
Phenanthrene
Pyrene
SiSpiillaiPSjIi
liiiEiliill
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
1810
ND
ND
ND

ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
3010
ND
ND
ND

ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
1410
ND
ND
ND

ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
87.4 a
ND
ND
ND
a Estimated Maximum Possible Concentration
ND = Not Delected
NOTE: PAH values have been blank corrected.
                                   2-16

-------
Table 2-9
PAH EMISSIONS SAMPLING AND FLUE GAS PARAMETERS
JMATHY CONSTRUCTION COMPANY PLANT 26 (1991)
                                •Hi

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
 125
0.330
 41.4
1.173
 326
 14.2
 5.6
 31.4
18100
 511
 102
 125
0.340
 41.9
1.186
 323
 12.5
 5.8
 31.0
18000
 509
 104
 125
0.310
 38.9
1.102
 327
 14.3
 5.4
 28.3
18200
 515
 95.4
 NA
0.327
 40.7
1.154
 325
 13.7
 5.6
 30.2
18100
 512
 NA
NA = Not Applicable
                                       2-17

-------
         Table 2-10
         PARTICULATE MATTER CONCENTRATIONS AND EMISSIONS
         MATHY CONSTRUCTION COMPANY PLANT 26 (1991)	
          09/07/91
          09/09/91
Oullct
Oudel
1
2
          09/10/91   Oullel
125
125
125
0,0314
0.0170
0.0237
0,0240
0.0413
0.0217
Q.Q360
0,0330
0.0719
0.0390
0.0541
0.0550
0.0946
0.0497
0.0824
0.0756
4.84
2.61
3.63
3,69
2.20
1.19
1.65
1,68
CO

-------
product. The emission factors generated from sampling Runs 1 and 3 are in relatively
close agreement, whereas the second run emission factor represents the low endpoint of
the data set.
These emission factors are slightly greater than those currently published in AP-42
for similar facilities (0,098 Ib/ton after baghouse control, from data from circa 1973-74).
This difference may be attributable to a variety of factors, including product
specifications or differences in baghouse design, operation, and maintenance between
facilities tested.
2.5 PM10/CPM RESULTS
2.5.1 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
PM,0 emissions using the constant sampling rate (CSR) procedure coupled with EPA
Method 202 for determining condensible emissions from the sampling train's back half.
The CSR employs normal isokinetic sampling procedures except that the sample
duration at each sampling point is proportional to the gas velocity at that point.
Sampling cutpoints ranged from 9.24 microns to 10.6 microns, with an average cut
size of 9.79 microns. These particle size separations were achieved with isokinetic rates
measured from 81 to 91 percent which are acceptable by the method specifications.
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 > 10 microns (cyclone fraction);
• Noncondensible PM < 10 microns (filter fraction);
• Inorganic CPM associated with the water fraction (< 10 microns); and
• Organic CPM associated with the methylene chloride fraction
(< 10 microns).
JBS342

-------
2.5.2 PMie Emissions
The average emission rate and emission factor for PM10 including condensibles
were 8.24 Ib/hr and 0.0352 Ib/ton of product, although the condensible and PM10 filter
catches for Run 2 totaled almost twice those collected in Runs 1 and 3. The sizable
deviation in condensible emissions detected in Run 2 may be attributable to several
factors, including abnormalities in fuel characteristics or an increase in VOC residues in
the recycled asphalt concrete.
The emission factors calculated for PM greater than 10 microns averaged
0.017 Ib/ton, and all sampling runs were in relatively close agreement. Also, these data
are similar to the emission factors for PM calculated from the PM/metals tests discussed
earlier.
The emission factors developed from both fractions of these tests are higher than
those currently found in AP-42. The factors for PM10 are three to six times greater than
current AP-42 data, although AP-42 literature does not discuss specific fuels used or
residual VOC contents of recycled asphalt cement for the emission factors published
(e.g., natural gas or oil).
It should be noted that EPA Method 201A recommends adding the condensible
fractions to the PM10 filter catch when compiling data for emission inventory purposes.
As seen in Tables 2-11 and 2-12, this procedure results in substantially higher PM10
emission factors due to the large quantities of condensible PM found in the back half
water fraction. The quantities of PM10 alone (from the backup filter catch only) are
shown for comparison. The average emission rate and emission factor for PM10 alone
were 1.19 Ib/hr and 0.0052 Ib/ton of product, which is substantially lower than the values
with the condensible fractions added, namely 8.24 Ib/hr and 0.0352 Ib/ton of product.
The front half instack filter catch (i.e., cyclone catch plus backup filter catch) does
not compare well with the PM filter catch performed by EPA Method 5. One possible
reason for this discrepancy is the fact that testing by these methods was performed at
different times. One would expect the Method 5 PM results to be slightly larger since
the filter was operated at lower temperatures that then EPA Method 201A instack filter
JBS342

-------
Table 2-11
SUMMARY OF PM10/CPM EMISSION FACTORS AND PROCESS OPERATING DATA
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Date
Production Rale (tons/hr)
Virgin Aggregate Rate (tons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cement Rate (tons/hr)
Percent of Raled Capacity (%)
Aggregate Moisture (%)
Burner Selling - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exit Temperature (degree F)
Stack Flow Rate (dscfm)
Stack Flow Rate (dscf/lon of product)
Stack Temperature (degree F)
Slack Moisture (% volume)
Stack CO2 (volume % dry)
Slack O2 (volume % dry)
Stack CO (ppmV)
Control Device
PM10 Emission (Ibs/ton) b
Paniculate Emission < Cut Size (Ibs/ton of product) c
Participate Emission > Cut Size (Ibs/ton of product) d
Paniculate Emission Tolal (Ibs/ton of product) e

09/24/91
212
143
58
10.9
71
4,2
51
51.7
66
347
20000
5600
328
28.8
7.1
12.0
130
Baghouse
0.0050
0.0336
O.OM6
0.0482

09/25/91
257
175
72
10.1
86
4,4
88
60.3
NT
334
16000
5270
317
37.7
7.6
10.4
120
Baghouse
0.0046
0.0447
0.0168
0.0615

09/25/91
223
152
62
9.1
74
4.2
70
58.2
NT
322
17900
6710
305
36.3
4.7 a
10.8
55.0
Baghouse
0.0060
0.0274
0.0198
0.0472


231
157
64
10.0
77
4.3
70
56.7
66
334
17967
5860
317
34.3
7.4 a
11.1
102

0.0052
0.0352
0.0171
0.0523
NOTES: Run averages were calculated from readings taken periodically throughout the duration of the
       emission test run. See Table 3-2 and 3-3 for the individual readings.
a CO2 value suspiciously low. Not used in average.
b Includes PM10 filter catch only.
c Includes PM10 filter catch and back half condensibles.
d Includes cyclone catch only.
e Includes ihc sum of all fractions.
                                                  2-21

-------
Table 2-12
PM10 EMISSION TEST RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Corrected Barometric Pressure (in. Hg)
Slack Static Pressure (in- H2O)
Average Stack Temperature (deg, 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)
Slack Viscosity (micropoise:)

29.38
-0.80
328
7.06
12.01
80.93
28.8
64.5
43000
20000
219
,S;>i-;'KfX-lBfcii**i»f;'!li;--">;o;--Ai
20.98
-0.80
317
7.60
10.40
80.93
37.7
81.6
54300
16000
209
>!fe:w:S2K^fe::ft&:&S&S^3^
Total sampling time (min)
Average Meter Temperature (deg. F)
Average Meter Pressure (in.HZO)
Average Sampling Rate (dscfm)
Average Sampling Rate (acfm - cyclone cond)
Standard Metered Volume, Vm(std) (dscf)
Percent Isokinelic
64.3
59
0.24
0.27
0,57
17
89.1
65.1
69
0.30
0.22
0.74
14
91.4

20.98
-0.80
305
4.74 a
10.83
84.43
36.3
87.5
58200
17900
207

23.78
-0.80
317
7.33 a
11.08
82.10
34.3
77.9
51800
18000
212

70.2
71
0.30
0.22
0.71
15
80.8
66.5
66
0.28
0.24
0.67
16
87.1

Cut Size (um)
Cyclone Paniculate Caich (g)
PM10 Filter Paniculate Calch (g)
H2O Back Half Paniculate Catch (g)
MeCl Back Half Paniculate Catch (g)
Total Paniculate Catch (g)
PMlO Concentration (grains/dscf) b
PM10 Concentration (grains/dscf @7% O2) b
Paniculate Cone. < Cut Size (grains/dscf) c
Paniculate Cone. < Cut Size (grains/dscf @7% O2) c
Paniculate Cone. > Cut Size (grains/dscf) d
Paniculate Cone. > Cut Size (grains/dscf @7% O2) d
Paniculate Cone. Total (grains/dscf) e
Paniculate Cone. Total (grains/dscf @7% O2) e
PMlO Emissions (Ibs/hr) b
Paniculate Emissions < Cut Size (Ibs/hr) c
Paniculate Emissions > Cut Size (Ibs/hr) d
Paniculate Emissions Total (Ibs/hr) e
10.62
0.0202
0.0070
0.0354
0.0040
0.0666*
0.0062
0.0098
0.0414
0.0647
0.0180
0.0282
0.0594
0.0929
1.07
7.11
3.10
10.21
9.22
0.0294
0.0080
0.0619
0.0080
0.1073
0.0086
0.0113
0.0835
0.1105
0.0315
0.0417
0.1149
0.1521
1.18
11.48
4.33
15.81
9.49
0.0286
0.0086
0.0279
0.0031
0.0682
0.0087
0.0120
0.0400
0.0552
0.0289
0.0398
0.0688
0.0950
1.33
6.12
4.42
10.54
9.78
0.0261
0.0079
0.0417
0.0050
0.0807
0.0078
0.0110
0.0549
0.0768
0.0261
0.0366
0.0810
0.1133
1.19
8.24
3.95
12.19
a CO2 value suspiciously low. Not used in average.
b liiCiudcs FM1G filter catch only.
c Includes PMlO filter calch an back half condensibles.
d Includes cyclone catch only.
e Includes the sum of all fractions.
                                              2-22

-------
(248°F versus 317°F). Therefore, the EPA Method 5 filter would be expected to catch
more of the condensible matter than the instack cyclone filter combination. However,
such was not the case. It is not known why this discrepancy occurred.
The PM10 emission factors and process operating data are summarized in
Table 2-11. The analytical results are shown in Table 2-12. 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.
2.6 ALDEHYDE RESULTS
2.6.1 Overview
A single sampling train was used to collect samples for analysis of 18 aldehydes
(acetaldehyde, acetone, acetophenone/o-tolualdehyde, acrolein, benzaldehyde,
butyraldehyde/isobutyraldehyde, crotonaldehyde, 2,5-dimethylbenzatdehyde,
formaldehyde, hexanal, isophorone, isovaleraldehyde, MIBK/p-tolualdehyde, methyl ethyl
ketone, propionaldehyde, quinone, m-tolualdehyde, and valeraldehyde). Four sampling
runs were performed in order to ensure representative test results.
2-6.2 Process Operation
Table 2-13 presents the aldehyde emission factors with a summary of process
operating data for the four test runs. During the emission tests, the plant was operating
at maximum production load of 97, 89, and 80 percent for Runs 1, 2, and 4, respectively,
but at a reduced load of 67 percent for Run 3. However, all runs were considered within
typical operating ranges and, therefore, all four runs were used in averaging. The
production rates were 290 tons/hr, 267 tons/hr, 202 tons/hour, and 241 tons/hr for
Runs 1, 2, 3, and 4, respectively.
Only the aldehydes detected are presented. The other aldehydes were analyzed,
but were not collected in detectable amounts. Of the 18 aldehydes analyzed, the
following 13 were detected: acetaldehyde, acetone, acrolein, benzaldehyde,
butyraldehyde /isobutyraldehyde, crotonaldehyde, formaldehyde, hexanal,
isovaleraldehyde, methyl ethyl ketone, propionaldehyde, quinone, and valeraldehyde.
JBS342

-------
  Fig 2-1 PM10 PARTICULATE EMISSIONS
                 (Ibs/hr)
0
                                      < 10 microns
                                      > 10 microns
     Runl
Run 2
Run 3
                       2-24

-------
    Fig 2-2 PM10 PARTICULATE CONCENTRATION
                          (grains/dscf)
u
Wi
'
C
•4— >
C
(U
u
C
o
U
0)
o
CO
OH
               (@ 7% 02)

             Runl
  (@ 1% O2)

Run 2
  (@ 7% O2)

Run 3
                           < 10 microns
                                                   > 10 microns
                           Note: Values
                           are reported in
                           grains/dscf and in

                           grains/dscf at

                           7% O2.
                                2-25

-------
       Fig 2-3 PM10 PARTICIPATE CATCH
                       (grams)
  0.12YX
   0.1-
C3
Cu
4)
3  0.04
   0.02
     0
                                              MeCl Back Half
                                              H2O Back Half
                                              PM10 Filter
                                              Cyclone
          Runl
Run 2
Run 3
                             2-26

-------
Table 2-13
SUMMARY OF ALDEHYDE EMISSION FACTORS AND PROCESS OPERATING DATA
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Date
Production Rale (tons/hr)
Virgin Aggregate Rale (tons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cement Rate (tons/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Burner Setting - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exit Temperature (degree F)
Stack Row 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
Acetaldehyde (Ibs x 10(-5)/tons of product) a
Acetone (Ibs x lQ(-5)/tons of product) a
Acrolein (Ibs x 10(-5)/tons of product) a
Benzaldehyde (Ibs x 10(-5)/tons of product) a
Butyraldehyde/Lsobutyraldehyde (Ibs x 10(-5)/toos of product) a
Crotonaldehyde (Ibs x 10(-5)/tons of product) a
Formaldehyde (Ibs x 10(-5)/tons of product) a
Hexanal (Ibs x 10(-5)/tons of product) a
Isovaleraldehyde (Ibs x 10(-5)/tons of product) a
Methyl Ethyl Ketone (Ibs x lO(-5)/tons of product) a
Propionaldehyde (Ibs x 10(-5)/tons of product) a
Qyinone (Ibs x 10(-5)/torts of product) a
Valeraldehyde (Ibs x 10(-S)/tons of product) a
O&£<#<'^M<£O :-&:-:£•£
My«
-------
Aldehyde emissions from this plant are most likely a function of fuel consumption and
any volatile fraction of the asphalt cement.  Because a fuel flow rate could not be
measured at this facility, the emission factors presented are expressed in Ib/ton of
product rather than lb/ft3 of fuel oil.
2,6,3  Emissions
      Table 2-14 presents the aldehyde emissions results for the four test runs.  The
date, metered volume (in dscm), O2 concentration, and flow rate for each run are also
shown.  Flue gas concentrations are given in terms of ^ug/dscm, and ^g/dscm corrected
to 7 percent O2 and g/hr.  Oxygen concentrations were collected from CEM data.
      During the emission tests, formaldehyde had the highest average mass rate, with
206 g/hr, followed by acetaldehyde, with 143 g/hr.  After blank correction,
acetophenone/'o-toiuaidehyde, 2,5-dimethyibenzaidehyde, isophoroae, isovalcfaldehyde,
MIBK/p-tolualdehyde, and m-tolualdehyde yielded insignificant amounts for any of the
runs during the emission tests. Aldehyde values ranged from 2.88 g/hr of
isovaleraldchyde in Run 1 to 467 g/hr of formaldehyde in Run 3.
      The aldehyde values for the emission tests did not change significantly from
Runs 1, 2, and 4.  Run 3 shows markedly higher values because of the low production
rate and poor combustion characteristics at the lower end of unit design specifications.
2.6.4  Flue Gas Aldehydes by Sample and Sample Parameters
      Table 2-15 presents the aldehyde 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.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
presented.  Appendix A.3 contains a complete list of these parameters for each test run,
along with the field data sheets.
JBSJ42
                                       2-28
-------
Table 2-14
ALDEHYDE CONCENTRATIONS EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Acetaldehyde
Acetone
(ug/dscm)
(ug/dscm @ 7% O2)
Acrolein
Benzaldehyde
Butyraldehyde/Isobutyraldehyde   (ug/dscm)
                             (ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)

(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)

(ug/dscm)
(ug/dscm @ 7% O2)
Crotonaldehyde
Formaldehyde
(ug/dscm)
(ug/dscm @ 7% O2)
(ug/dscm)
(ug/dscm @ 1% O2)
4090
7180
 135

2060
3620
68.1

 124
218
4.10

 100
 176
3J1

561
984
18.5

 126
222
4.17

2390
4200
79.0
2100
2750
66.9

3230
4240
 103

ND
ND
ND

 112
 147
3.5S

435
570
13.9

82.6
 108
2.63

3570
4680
 114
 7020
12200
 232

 2240
 3910
 74.2

 ND
 ND
 ND

 903
 1580
 29.9

 755
 1320
•25.Q

 669
 1170
 22.2

14100
24600
 467
4410
6250
 137

3980
5640
 123

 231
 327
7.16

 232
 329
7.21

408
578
12.7

 176
 249
5.45

5230
7410
 162
4400
7100
 143

2880
4350
92.2

 177
272
5.63

337
558
11.0

540
863
17,5

263
437
8.61

6320
10200
206
ND = Not Detected
NOTES: Concentrations given have been blank corrected.
        Aldehyde compounds analyzed, but not detected, are not included in this table.
                                                         2-29
-------
Table 2-14 (Continued)
ALDEHYDE CONCENTRATIONS EMISSION RATES
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Hexanal
Isovaleraldehyde
Meihyl Elhyl Ketone
Proplonaldehyde
Quinone
Valcraldchyde
(ug/dscrn)
(yg/dscm @ 7% O2)
(g/hr)

(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)

(ug/dscm)
(ag/dscai © 7% O2)
(g/hr)

(ug/dscm)
(ug/dscm @ 7% O2)
(g/hr)

(ug/dscm)
(ug/dscm @ 7% O2)
(8/hr)

(ug/dscm)
(ug/dscm @ 7% O2)
87-0
153
2.88

42.8
75.0
1.41

279
490
9.23

141
24S
4.67

103
181
3.41
ND
ND
ND

ND
ND
ND

180
237
5,75

266
349
8.49

108
142
3-45
165
287
5.45

155
271
5J4

906
1580
30.0

976
1700
32.3

411
716
13.6
 147
 208
 4.56

 31.0
 43,9
0.961

 312
 441
 9-67

 592
 839
 18.4

 231
 327
 7.16
133
216
4.29

76.3
130
2.50

419
687
13.7

494
784
16.0

213
341
6-90
ND = Not Detected
NOTES: Concentrations given have been blank corrected.
        Aldehyde compounds analyzed, bui noi detected, are not included in this table.
                                                     2-30
-------
Table 2-15
ALDEHYDE AMOUNTS IN
MATHY CONSTRUCTION
FLUE GAS SAMPLES
COMPANY PLANT 26
 BLANK CORRECTED
(1991)

Acetaldehyde
Acetone
Aceiopheno ne/o-Tolualdehyde
Acrolem
Benzaldehyde
Butyraldehyde/Isobutyraldehyde
Crolonaldehyde
2,5-Dimethylbenzaldehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehyde
MIBKyp-Tolualdehyde
Methyl Ethyl Ketone
Propionaldehyde
Quinone
m-Tolualdehyde
Valeraldehyde
':-X->*;?Sw',?f SS " c&TvK-
3530
1780
ND
107
86.4
484
109
ND
2060
190
ND
75.1
ND
36.9
241
122
ND
89.1

1220
1880
ND
ND
65.3
253
48.1
ND
2080
136
ND
ND
ND
ND
105
155
ND
62.9
1%^$^$?<$&&M%%
5880
1880
ND
ND
757
633
561
ND
11800
519
ND
138
ND
130
759
818
ND
344
'!*£'&^KC'Ho:W1*pO£*>X.-
2560
2310
ND
134
135
237
102
ND
3040
200
ND
85.3
ND
18.0
181
344
ND
134
MP:ifllirat
S:it^i5:^3?is^S^:
ND
3%
ND
ND
ND
ND
ND
ND
14.5
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND = Not Detected
NOTE: Aldehyde values have been blank corrected.
                                     2-31
-------
Table 2-16
ALDEHYDES EMISSIONS SAMPLING
MATHY CONSTRUCTION COMPANY
       AND FLUE GAS PARAMETERS
       PLANT 26 (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
0.490
30.5
0.863
311
13.0
 6.8
30.6
19400
55 i
98.8
 38.5
0.530
 20.6
0.582
 320
 10.3
 8.2
 39.5
18800
 531
 112
62.5
0.470
29.6
0.838
315
12.9
 6.2
24.4
19500
 95.8
 62.5
0.330
 20.5
0.581
 317
 11.1
 6.4
 28.9
18300
 517
 96.0
 NA
0.455
 25.3
0.716
 316
 11.8
 6.9
 30.8
19000
 538
 NA
NA = Not Applicable
                                        2-32
-------
2.7   CONTINUOUS EMISSIONS MONITORING RESULTS
2,7.1  Overview
      Continuous emissions monitoring was conducted at the outlet to the air pollution
control device (APCD) during the three days of testing.  Concentrations of O2, CO2, CO,
NOK, 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.
2.7.2  Continuous Emission Monitoring Results
      The CEM averages  are presented in Table 2-17. The average O2 concentrations
ranged from 10.1 to 13,0 percent by volume.  Average CO values ranged  from 4.7 to
9.2 percent by volume.  Average NOX concentrations Tanged from 94.2 to 145.7 ppmv.
Concentrations of THC were also  monitored, with the resulting average concentrations
ranging from 488.4  to 601.8 ppmv  (wet).  Sulfur dioxide values were  approximately 100
to 150 ppmv, while average CO concentrations ranged from 31.3 to 374.0 ppmv.
      All of the QA/QC procedures were followed as specified in the test plan.   The
final results are valid, as all of the CEM performance specifications were attained and 9
of the 10 runs had 100 percent completeness in relationship to the manual run times.
The QA/QC results are discussed  further in Section 6.
2.7.3  Nonmethanc Hydrocarbon Emission Test Results
      EPA Method 18 analysis of the flue gas was performed using GC to separate the
hydrocarbon species (Q-Cg) present in the flue gas stream.  Several samples were
injected into the GC during each test day. Methane, benzene, toluene, ethylbenzene,
                                       2-33
-------
Tfiible 2-17
CONTINUOUS EMISSIONS MONITORING DAILY TEST AVERAGES
MATHY CONSTRUCTION COMPANY PLANT26 (1991)
PAH/Melals
  ^Vldehyde
 PM10/CPM
 1
 2
3 a
•
 1
 2
 3

•
 1
 2
 3
09/23/91
09/23/91
09/24/91
09/23/91
09/23/91
09/24/91
09/25/91
09/24/91
09/25/91
09/25/91
08304039
1355-1606
1236-1503
1105-1214
1546-1641
0845-0958
1144-1254
1005-1120
1025-1J38
13154430
0830-1039
1355-1606
12364503
1115-1214
15514641
0845-0958
1144-1254
1005-1120
1025-1138
1315-1409
 554,2
 582.9
 515.1.,

 564.7
 601,8
 531.0
 530
S1»JK«::®SS1
iM*.?,£iz
 483.4
 56L1
 497.1
150.9
144.0
123.0
102.0
145.1
112.8
138.0
118.2
144.5
135.9
a PAH/Metals Run 3 inierrupled 1311-1334 because of down lime.
b Suspicious data could be due 10 inslrumenl problems.
-------
and xylene were determined by this method.  Total hydrocarbon emissions as methane
were determined by EPA Method 25A.
      The hydrocarbon concentrations and emission rates in ppmv and Ib/ton of asphalt
produced are presented in Table 2-18. 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 0.0913, 0.121, and 0.01 Ib/ton for the three test days.  The
average emission factors of benzene, toluene, ethylbenzene, and xylene for the first test
day were 0.00021, 0.0011, 0.00027, and 0.000098 Ib/ton, respectively.  The average
emission factors for the second test day were 0.00072, 0.00068, 0.00078, and 0.0 Ib/ton,
respectively.  The average  emission factors for the third  test day were 0.00041, 0,00028,
0.00019, and 0.00014 Ib/ton, respectively.
2.8    ASTM METHODS
      This section presents results of laboratory analysis of waste oil fuel collected
September 26, 1991.  Standard ASTM methods were used  to assess heat of combustion,
ultimate analysis (ash, O2,  carbon, hydrogen, sulfur, and  nitrogen), and chlorine content
of the sample.
      The results are given in Table 2-19. The waste fuel oil sample was anlayzed by
McCoy &  McCoy Laboratories.
-------
                                                    Table 2-18. Hydrocarbon Emission Rates and Concentrations
Date
09/23/91







Time
0920
0951
1041
114B
1407
15Z5
1534
1624
AVERAGE
STANDARD DEVIATION
09/24/91





1005
1044
1121
1316
1354
1435
•fy <^»|AvrERAGE^i^ [
. STANDARD DEVIATION :
09/25/91

1037
1115
Slack
Plow
Rate
(dscfm)
18061
18061
18061
19443
17975
17975
17975
18760
18289
517
20000
20000
20000
18185
18185
18185
; l^ll
; ' 125? *:i
16000
16000
Asphalt
Production
Rate
(tons/hr)
287
287
287
290
279
270
270
267
280 '
8
212
212
212
217
217
217
r=*-* 215
11
257
257
Methane
ByGC
(ppnw)
5.128
ND
ND
ND
ND
0.796
ND
ND
0.74
0.347
0.04
0.606
0.362
0.223
0.125
0.561
0.32
0.195
2,028
0,128
Total
Hydrocarbons
ByTHC
(ppmv)
481.1
554,2
559.4
567.6
557.5
566J
593,2
596.7
5593
153
508.1
4B9.7
492.2
738.6
547.9
508,9
547.6
85,3
609.2
545.8
Nonmethane
Hydrocarbons
(pprav)
476.0
554.2
559.4
567,6
557.5
565.7
593.2
596.7
S5B.B
15.4
508.1
489.1
491,8
738,4
547,8
508.3
547.2
85.3
607.2
545.7
(Ibs/ion)
7.47E-a2
B.69E-02
8.78E-02
9.49E-Q2
B.95E-02
9.39E-02
9,84 E-02
1.05B-01
' 9.13E-02
S3&-J
1.19E-01
1.15E-01
1.16E-01
I54&fll
1.14E-01
1.06B-Q1
1.21B-01
1.54E-2
9.42E-02
8.47E-02
Benzene
(ppmv)
0.417
0.161
ND
0.316
0.301
0.283
0.347
0309
0,27 '
Oil
0.581
0.554
0.664
0.797
0.721
0.726
0.67
0,08
0.99
0.517
(Ibs/ton)
3.19E-04
L23E-04
0
257E-04
2,36E^)4
2.29E-04
2.81 E-04
2.64E-04
214E-04
8.89E-5
6,66 E-04
6.J5E-04
7,61E^5/
8.I2E-04
7.34 E-04
7.39E-04 *
_ n 	 in 'i * J
(7.25E-Op
629E-5
7.49E-04
3.19E-04
Toluene
(ppmv)
1.31
1.137
1.075
1546
0.577
ND
1.927
1.759
1.17 -
0-63
ND
ND
_<
< 0.748
0.86
0.911
^0.811
056
o.yj
1.002
0.132
(Ibs/ton)
1.18&fl3
1.03EJD3
9.70E-W
1.49EX)3
5.33E-04
0
1.84 E-03
1.77E-03
1.10E-03
6.2E-4
0
0
1.01 E-03
1.03E-03
1.09E43
9.74 E-04
6.86E-04
43E4
8.94E-04
1.18E-04
Elhyibenzenc
(ppmv)
ND
ND
ND
ND
0.332
0.266
1.157
0.22
OO5
0.36
1.502
ND
1.179
0,349
ND
ND
OJ51
OJ7
0.261
0.068
(Ibs/ton)
0
0
0
0
354 E-04
2.93E-W
1.2TEM
256E^04
2.72EXM
4-OE4
2.34E-03
0
1.84E-03
4.84 E-04
0
0
7.78E-04
8:85 B-4
2.69E-04
7.00E-05
Xylcne
(ppmv)
ND
ND
ND
0.101
0.158
0.007
0.454
ND
Q.09
0.15
ND
ND
ND
ND
ND
ND
0
0.01
0.441
0.036
(Ibs/ton)
0
0
0
l.UE-04
1.68E-04
7.71E-06
5.00E-04
0
9.85B-05
l.WE-4
0
0
0
0
0
0
0
8.2E-6
454 E-04
3.71 E-05
JBS342
-------
                                                                                Table 2-18.  Continued
      Date
                                                 (;ppmv)
                                                         .   , ,    .
                                                         :-'/• "•'-•"•'- "•' \'-'
                                                         :(ppnw);:
                                                                                                                                                  Eihylbenzcne s
                   1149
18260
                                          241
           0.155
             5203
                                                  520.1
                      9.82E-02
                     0.378
                                  ND
                                          ND
                                          ND
                   1228
18260
241
0.162
535.4
535.2
LOlBfll
ND
ND
                                                                                                                  ND
0.259
3.25&04
                    1342
                              17900
                                           223
                       0136
                                                                   505.2
                                                                                505.1
                                               1.01&01
                                                                                                     0.224
                                                                                                               2.19E-W
                                                                                                                           ND
                                                                                                   S.31E-06
                                                                                                                           0.«M5
                                                                                                           6.64 E-06

  'CTANOARDj

ND  = Nol Detected
JBS342
-------
                                   Table 2-19

                          Summary of Waste Oil Analysis
                    Mathy Construction Company Plant 26 (1991)
Analyte
Ash
Carbon
Hydrogen
Nitroeen
Sulfur
Oxygen
Chlorine
Heat of Combustion
Amount Found
(%?$%•£; .-
2.91
83.43
11.03
0.22
0.65
1.72
0.04
18364 Btu/lb
JBS342
                                          2-38
-------
                           3.  FACILITY DESCRIPTION

      This section provides a description of the Mathy Construction Company's Plant
No. 26 asphaltic concrete plant located near New Richmond, Wisconsin. The process
equipment and production materials used and the process parameters recorded during
the emissions test are discussed.
3.1   PROCESS DESCRIPTION
      Mathy Construction Plant No. 26 is a typical continuous drum asphaltic concrete
plant with a rated production capacity of 300 tons per hour.  The plant  consists of the
following components:
      •     Aggregate storage piles;
      •     Recycled  asphalt concrete storage piles;
      •     A rotary kiln/drum mixer for aggregate drying and asphalt cement mixing;
             and
      •     A heated  asphalt cement storage tank.
      Virgin aggregate and recycled asphalt concrete must  be combined and dried to
product specifications in the oil-fired rotary kiln/drum mixer.  Both materials  are
introduced at the burner end of the  drum. Asphalt cement, an amorphous solid that
must be heated to a liquid state for injection  into the drum mixer, is then mixed with the
dried aggregate and asphaltic concrete.  The final product leaving  the drum mixer is
transferred to a hot mix storage bin  and then loaded into trucks.
      Aggregate fines become entrained in the combustion exhaust leaving the rotary
kiln/drum mixer.  The fines are then transported by the flue gas to a fabric filter, where
they are collected.  Process fugitive PM and VOCs from the drum mixer are also routed
to the fabric filter inlet.  Emissions of VOCs from fuel combustion, organic contaminants
in recycled asphalt, and the asphalt cement are not  controlled by the fabric filter, nor are
any VOC emission control devices used.  The exhaust flow is induced by a clean-air-side
fan.
JBS342                                   3~1
-------
      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 and recycled asphalt concrete storage piles and cold transport of
             these materials;
      •      Cold asphalt cement 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 of each 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 41 to  43 percent recycled asphalt and
5.8 percent asphalt cement by weight, and the drum fuel is a specification waste oil.  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 through 3-3.
3-2.1  Process Conditions During Metals/PAH Testing
      Table 3-4 summarizes the production and operating conditions  associated with the
metals and PAH test data.  Production rates for three runs varied from 217 tons per
hour to 287 tons per hour  (72 to 96 percent of rated capacity).  Data regarding fuel
consumption were not readily available because no functioning fuel flow rate  measuring
device was available.  Sampling Run 3 was interrupted by  a brief process shutdown, but
sampling activity was suspended during this time.
      P*"cc '""«T'^*'«<">Tic T\iiriTi«T
      Table 3-5 summarizes the production and operating data associated with  aldehyde
test data.  Production rates varied from 241 tons per hour to 290 tons per hour (80 to
JBS342
                                       3-2
-------
Table 3-1
SUMMARY OF PROCESS OPERATING DATA COLLECTED DURING EMISSION TESTING
MATHY CONSTRUCTION COMPANY PLANT 26 - SEPTEMBER 23,1991
   8:30
   100
195
81
11.3
285
NA a
10.5
47,0
       Fully Ojen^
   9:13
   100
187
79
11.1
270
NA a
10.0
49.8
86
Fully Open
   9:56
   86
190
82
11.1
279
NA a
10.5
52.6
       Fully Open
   10:39
   96
201
          12.0
          275
         NA a
           10.5
          55.0
                  Fully Open
   11:28
   100
198
87
11.6
275
NA a
10.5
57.8
       Fully Open
   12:00
   100
193
83
11.4
287
NA a
10.5
58.0
37
Fully Open
   14:05
   84
187
88
11.2
275
NA a
10.7
58.8
       Fully Open
   14:29
   84
186
69
10.8
285
NA a
10.5
60.8
43
Fully Open
   15:00
   64
182
79
10.7
264
NA a
10.5
61.2
       Fully Open
   15:30
   76
182
80
10.7
295
NA a
10.5
60.0
       Fully Open
   16:30
   72
180
72
10.8
285
NA a
10,0
58.2'
46
Fully Open
   16:47
Shutdown
a Not available due lo faulty planl instrumentation.
-------
Table 3-2
SUMMARY OF PROCESS OPERATING DATA COLLECTED DURING EMISSION TESTING
MATHY CONSTRUCTION COMPANY PLANT 26 - SEPTEMBER 24,1991
   8:30
34
148
65
8.8 c
269
331
 11
48.2
       Fully Open
   9:14
30
134
55
6.8 c
265
324
10.8
48.5
86
Fully Open
   9:36
48
138
49
10.0 c
275
345
10.7
                  Fully Open
   10:31
48
143
57
11.2 c
282
355
10.5
51.4
       Fully Open
   11:08
50
145
63
11.9 c
278
339
10.6
51.8
       Fully Open
   11:30
56
143
58
9.5 c
282
348
10.5
52.0
       Fully Open
   12:15
                                                                     55.6
                                                                     47
                                                                  Fully Open
   12:21
53
144
65
 8.3
275
334
10.5
                 Fully Open
   12:35
53
146
62
 8,6
275
341
10.3
55.8
       Fully Open
  13:18 a
54
147
62
J0.7
275
366
10.5
                 Fully Open
  13:36 b
52
145
56
 10.7
265
342
11.2
55.2
       Fully Open
   14:06
51
144
56
 8.9
282
357
10.0
                 Fully Open
   14:31
48
152
67
 8.6
275
344
10.0
57.0
59
Fully Open
   15:06
48
147
60
 8.7
272
334
10.0
                 Fully Open
a Plant Down
b Restarted Plant
c Value Varies
-------
         Table 3-3
         SUMMARY OF PROCESS OPERATING DATA COLLECTED DURING EMISSION TESTING
         MATHY CONSTRUCTION COMPANY PLANT 26 - SEPTEMBER 25,1991
            8:54
                                                                                56.0
                                                                               71
                                                                             Fully Open
            9;25
           72
          146
          65
          8.9
          288
          358
          11.2
                           Fully Open
            10:00
           62
          151
          68
          8,8
          299
          349
          9.7
                           Fully Open
            10:33
           97
          182
          77
         10.6
          280
          340
          10.0
          60.4
                 Fully Open
            11:10
           90
          175
          69
         10.3
          285
          330
          10.0
          60.2
                 Fully Open
            11:49
           76
          189
          76
         10.8
          275
          333
          9.5
                           Fully Open
U)
61
            12:07
           82
          173
          76
         10.2
          295
          349
          10.0
                           Fully Open
13:24
63
146
58
8.9
255
320
10.6
58.2
Fully Open
            13:36
           76
          173
          74
          9.4
          270
          324
          9.9
                           Fully Open
           14:15 a
                                                                                                 Fully Open
           14:30 b
                                                                                62.0
                                                                                      Fully Open
            14:47
           84
          167
          72
          9.8
          295
          338
          10.6
                           Fully Open
            15:00
           90
          172
          87
         10.4
          270
                    10.6
                    60.0
                           Fully Open
         a Plan! Down
         b Restarted Plant
-------
Table 3-4
SUMMARY OF METALS/PM AND PAHS PROCESS OPERATING CONDITIONS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Date
Production Rate (tons/hr)
Vi rgin Aggrega te Rate (lons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cement Rale (tons/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Burner Setting - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidify (%)
Kiln Exit Temperaiure (degree F)
Slack Flow Rate (dscfm)
Slack Flow Rate (dscf/ton of product)
Slack Temperature (degree F)
Slack Moisture (% volume)
Stack CO2 (volume % dry)
Stack O2 (volume % dry)
Stack CO (PpmV)
Conlrol Device

09/23/91
287
193
83
11.4
96
3.8
96
51.1
86
266
18000
3765
326
31.1
9,2
10.3
42-9
Baghouse

09/23/91
270
183
76
10.8
90
3-6
77
60.2
43
269
17900
3981
326
31.1
7.6
10.0
46.9
Baghouse
mizmmm
09/24/91
217
147
61
9.4
72
4.2
51
56.0
59
347
17900
4952
328
28.8
7.2
11.8
129
Baghouse
?«*;*»«:
IlfcSSiagifis

258
174
73
10.5
86
3.9
75
55.8
63
294
17933
4233
327
30,3
8.0
10.7
72.9

NOTES: Run averages were calculated from readings taken periodically throughout ihe duraiion
        of the emission lest run.  See Table 3-1 and 3-2 for the individual readings.
                                     3-6
-------
Table 3-5
SUMMARY OF ALDEHYDE PROCESS OPERATING CONDITIONS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
^&i:^i£;::3^:>:^:&&^
iMiiW'TtfSSifafcS&'S^^^o*^^
^M»a?HlPP»B|:W^^^^^^^^^^^S^^^^^^^fe
Date
Production Rate (tons/hr)
Virgin Aggregate Ra te ( tons/hr)
Recycled Asphalt Rate (tons/hr)
Asphalt Cement Rate (ions/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
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)
Slack O2 (volume % dry)
Stack CO (ppmV)
Control Device
vi£vV&$'vM'wf&3ffi*f
09/23/91
290
192
87
11.4
97
3.8
100
57.9
37
264
19400
4008
311
30,6
6.8
13.0
31.2
Baghouse
8|l|S:(filf|S;
3!$88fSS*SgsS!&S:
09/23/91
267
181
75
10.8
89
3.6
74
58.6
46
278
18800
4228
320
39.5
8.2
10.3
47.6
Baghouse
iiigKW5«;|«||:;S
09/24/91
202
138
55
9.4
67
4.2
37
48.4
86
333
19500
5781
315
24.4
6,2
12.9
374
Baghouse
3®$$$£mm
09/25/91
241
165
66
9.8
80
4.4
79
58.7
NT
341
18300
4560
317
28.9
6.4
11.1
86.5
Baghouse
:-xt-K"?:-:c$:i-:»:-:'>!*;t'm'i!'i

250
169
71
10.4
83
4.0
73
55.9
56
304
19000
4644
316
30.9
6.9
11.8
135

NT = Not Taken
NOTES; Run averages were calculated from readings taken periodically throughout the duration
       of the emission test run. See Table 3-1 and 3-2 for the individual readings.
                                            3-7
-------
97 percent of capacity).  No process shutdowns or upsets occurred during the other
sampling runs.
3-2.3  Process Conditions During PM10/CPM Testing
      The production and operating data that correspond to the PM10/CPM test results
are summarized in Table 3-6.  For three sampling runs, total asphaltic concrete
production varied between 212 tons per hour and 257 tons per hour (71 to 86 percent of
capacity). Sampling Run 3 was briefly interrupted by a process shutdown. The sampling
train was removed from the stack and capped during this interruption.
JBS342
                                       3-8
-------
Table 3-6
SUMMARY OF PM10/CPM PROCESS OPERATING CONDITIONS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Dale
Production Rate (tons/hr)
Virgin Aggregate Rate (tons/hr)
Recycled Asphali Rate (tons/hr)
Asphalt Cement Rate (tons/hr)
Percent of Rated Capacity (%)
Aggregate Moisture (%)
Burner Setting - Flame Meter (%)
Ambient Temperature (degree F)
Ambient Humidity (%)
Kiln Exit Temperature (degree F)
Stack How Rale (dscfm)
Stack Flow Rate (dscf/ton of product)
Stack Temperature (degree F)
Stack Moisture (% volume)
Stack CO2 (volume % dry)
Stack O2 (volume % dry)
Slack CO (ppmV)
Control Device
<*s$tP8iWis3:
09/24/91
212
143
58
11.0.
71
4.2
51
51.7
66
347
20000
5600
328
28.8
7.1
12.0
130
Baghouse

09/25/91
257
175
72
10.0
86
4.4
88
60.3
NT
334
16000
5270
317
37.7
7.6
10.4
120
Baghouse
¥;-:<'K'H--'K*^*^<*'-X':"X*
09/25/91
223
152
62
9.0
74
4.2
70
58.2
NT
322
17900
6710
305
36.3
4.7
10.8
55.0
Baghouse
P«pg::SS5»S8
m&WfSi&i-

231
157
64
10.0
77
4.3
70
56.7
66
334
17967
5860
317
34.3
6.5
11,1
102

NOTES: Run averages were calculated from readings taken periodically throughout the duration
       of the emission test run. See Table 3-1 and 3-2 for the individual readings.
                                        3-9
-------
                           4. SAMPLING LOCATIONS

      This section describes the locations where flue gas samples were taken during the
emission testing program at Mathy Construction Company Plant No. 26.  All samples
collected by manual methods, including PM10 samples, were collected from sampling
ports at equal heights in the exhaust stack. Samples for 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 3.7 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 five ports were used, as shown in Figure 4-2.
JBS342
-------
   Top
   View
    38"
42"
u u u u
Mathy Plant #26
        48"
                    150"
5 x 4" ID Ports
 evenly spaced
-e-e-e-e-e-j-
           14"
     o	L
                            CEM Port
         Baghouse
               Blower
              (ID Fan)
                                       Damper
Figure 4-1. Sampling Location Arrangement.
                     4-2
-------











*8.7"






3C




1



1 1 "





>
21.5"


•
12

( i







.9"
i
4.








I
3"


JO
4* *h A A A













^r
A
fr

^p


^
™



















w


^p


**.
w


• ..


Point















1
2
3
4
5













w


^p


^.
W















*


^p


^P


-A
w


















^
A
w

IV


^
™






Probe Mark














4







.
2"





I
1
41//
1
8.8"
17.4"
26.0"
34.6"
43.2"
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 particulate 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.  Particulate 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 Paniculate 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/H2O2 was of the Greenburg-Smith design; the other
impingers had straight tubes. The impingers were connected together with clean glass
JBS336
                                       5-1
-------
                                        Thermometer
         Temperature  /
           Sensor
                                                                             Thermometer
 Gooseneck
  Nozzle
                                                             Impingers with Absorbing Solution
Slack
Wall Hent Traced
     S.S, Probe
                                     Glass Filter Holder
                                                                                    v     Silica Gel
                                                                              Empty Knockout
                                          Empty Knockout
                                            Temperature
                                            K Sensors
                                                          5%HNa/»0%H,02
S-TypePftotTube
1
1
i .
Orifice 1
I I 	 r
H
S
h

i
•
i i


I' "aar \
irM
8
T
                                                                    By-pass
                                                                     Valwi
                                                                               Pump
                                                                                         Vacuum
                                                                                          Una
                         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 mir dry in a contamination-free
environment.  The ends were then covered with parafilrn. 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 rneterboxes, thermocouples,
nozzles, pilot 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 Pitot Tube Calibration.  The EPA has specified guidelines concerning the
construction and geometry of an acceptable Type-S pitot tube. A pilot 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
-------
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 run 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                                    *-5
-------
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, ihe 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 pitot 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  Paniculate 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 rneter 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
      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.
JBS196
                                         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.
IBS296 .
                                      5-9
-------
                                     Table 5-1

                                     Continued
      4.     Leak check each leg of pitot 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.
1BS2W
                                          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 particulate 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
-------
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                                             l:igtire 5-2.  Mciuls Sample Recovery Sdicmc
-------
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 irnpinger 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;
      o     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
                                       5-13
-------
 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  Participate 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
 JBS3M                                   5-14
-------
               TABLE 5-2.   APPROXIMATE DETECTION LIMITS
Metal
Chromium
Cadmium
Arsenic'
Leadc
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
(Mg/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 Limits'5
Front Half
(300 ml sample
size)
-------
   Container 3
 Acid Probe Rinse
  (Labeled APR)
    Container 2
Acetone Probe Rinse
   (Labeled PR)
Container 1
   Fitter
(Labeled F)
    Container 4
HNQ/HpzImplngers
   (labeled HN)
(include condensate
  Impinger, if used)


Reduce to Dryness
in a Tared Beaker
                                                  Desiccate to
                                                 Constant Weight
                         Determine Residue
                         Weight In Beaker
                                                                              r
                                                 Aliquot Taken
                                                Taken tor CVAAS
                                                for Hg Analysis
                                                  Fraction 2B
                         Determine Filter
                        Paniculate Weight
                         Sotubillze Residue
                          with Cone. HNOj
  AcldKy to pH 2
 with Cora, HNQ,
                                                Digest with Acid
                                               and permanganate
                                                 at 95°C lor 2 h
                                                  and Analyze
                                                forHgbyCWAS
                         Divide Into 0.5 g
                       Sections and Digest
                        Each Section with
                       Cone. HF and HNQ,
Reduce Volume to
Near On/ness and
   Digest with
   Cone. HNO,
       T_
                   Fltler and Dilute
                  to Hlnown Volume
                     Fraction 1
                                       Remove 50 to 100 ml
                                          Aliquot for Hg
                                        Analysis by CVAAS
                                            Fraction 16
                                           Dlgnst with Acid and
                                         Permanganate at 95°C In
                                           a Water Bath for 2 h
       Analyze by (CAP for
         Target Metals
          Fraction 1A
                                   1
       Analyze for
     Metals by GFASS
       Fraction 1A
                 Analyze Aliquol for
                 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 speetroscopy (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 Speetroscopy Standards and Quality
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 ^g/nrl 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
                                       5-17
-------
5.2    EMISSIONS TESTING FOR PARTICULATE MATTER LESS THAN 10
      MICRONS/CONDENSIBLE PARTICULATE MATTER
      The sampling method for fine paniculate matter/condensible participate 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 ^m), 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
-------
  Temperature
    Seraa
                                                                                  Thermometer
Cyclone
                                    Figure 5-4. PM/CPM Sampling Train
-------
caused the gas stream to swirl in a vortex; larger participates 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  P_M10/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 methylene 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 PM1P/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 PMIO, 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 pilot 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, paniculate  loading was also
known in order to calculate the required run duration to achieve a representative sample
JBS336                                    5-21
-------
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
filler, 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 PM10/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 be'nff tramnnrterl to the recoverv trailer.
         r            o     p  ~ .-._..            ^
      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,
_cycl_pne, 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 particulate
and acetone rinse was collected in a sample jar and sealed.  The liquid level was marked,
JBS336                                  5-22
-------
6i
Nozzle/
Dry bru
Cyclone / Front -hall Back-haH / / silic
Cyclone Exit / Filler Filler / Probe / Connecting Impingers |mDir
' Holder Filler Holder ' Extension ' Glassware No. TO v
ah into
IBI eel aluminum foil
(excluding ihe
turn around* cup)


















Rinse and Rlns<
brush 3X brus
wtth acetone wtrhai
(It necessary)





















land Remov
h3X flier hoi






elrom
def and
^lone place In original
petridish












Weigh lor
moisture
ga
Em
in
iGel
igers






Weigh lor
P*V moisitire
conteniB QaJn
IntoSempte
cortalner |


Inspect end
discard It
ladlqued
Addrtnslnaa Brush toose Rinse 2 Rinse 2 limes
trTaaninte any partlcuiate times wtth wtth water and
*^ vtaibteon water and addlo








HBer holder add to container
onto






hfler impinge
«H,0

Rlnge2tlme8 Rlnse2Umea
wtthMed. wtthMeO2
and add to and addlo
MeQ2 container MeC^ container
1

I
      Cyclone Rirtae
Wnoe
Finer nrwe
Filter
H,O
                        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 ancL 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), MeCi2 (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
-------
5.2.5  Analysis for PM^/CPM
      The PM10/CPM gravimetric analyses were completed 35 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  rng.  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 MeCL, sample was combined with the water sample in a 1000-ml 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-rnl 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                                   *~"
-------
           Cyclone Cede*
   Cyclone Catch
     (Mused)
                                   Determine
                                  total earn pie
                                    vofcimo
                                Transfer cartenta
                                    lotar*d
                                    break!*
     Acetone
                           Determine
                           total sample
                             voturne
                        Transfer contents
                            to tared
                            breaker
       Filter
                                              MeCl,
                                           Detennlne
                                           Iota) sample
                                             volume
                                             Determine
                                             tola! sample
                                               volume
        Desslcafe and weih
V1      to a coonuifU
Desekale and wetah
to a conslani
Dessicafe and wetah
lo a constanl weight
Desstcaie and weigh
lo a constant weight
                                                                                                     '	 Combine contents  	'
                                                                                                             In 1000 ml
                                                                                                          Separrtofy funnel
                                                                                                             MtaaUowlo
                                                                                                         separade, dialn,(save)
                                                                                                            moalalMeCU
                                                                                                           phase (mo MeCI2
                                                                                                           sample container
  Add 75 mis of
Mad jlo eeparalory
 funnel and repeal
 above procedure
                                                                                                            Repeal above
1
Tranter MeClx
cortento to tared
beaker
1
AOow lo evaporate
I
PtaceHjOlna
pre-cleaned
container and
evaporated to SO ml
on a hot plate
of equMtent
                                                                                             at room tempendure
                                                                                                under.anood
                                                                                                        d weigh
                                                                                             to a constant weight
                                                                                         Place In a tared
                                                                                      beaker and evaporate
                                                                                         lo drynesa In a
                                                                                           105 "Coven
                                                                                                                     Desslcate and weigh
                                                                                                                     to a constanl weight
                                         Figure 5-6.   PM10/CPM  Analytical  Scheme
-------
Moisture Determination
      Volume or weight of liquid in 1mpingers_
      Weight of moisture 1n silica gel 	"
                                    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 NHtOH required?
      Sample extracted  2X with 75 IsT

For Titratlon of Sulfate

      Normality 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)
       415 (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 mg.
      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 MeCl2 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 shon'n 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 pump.  The contents
of the sequential impingers were:  the first two impingers with 2,4-dinitrophenyIhydrazine
(DNPK), the third iinpinger 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 tube. 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
                                       5-28
-------
                      A
Temper rture
  Sense*
Slack
Wall
                                                                    Implnger Train
                                                                                              Thermometer
                    \
      S-Type Pttot Tube  \
                                    Manometer
                                               Tomperalure
                                                Senaora
                                                                                                           Vacuum
                                                                                                             Lino
                                                     Modified Greenburg
                                                      SmNh Impingers
                          Oifica
                            I      t
                  Ortftca

                 Manometw
                                    Figure 5-8.  Aldehyde 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 deionized 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 acetonilrile 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                                   5-30
-------
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 SamplingJ>rocedures. 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 acfrn (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   Aldehydes 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
irnnmgers 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
JBS336                                   5-32
-------
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 paniculate 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 geJ 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 QA 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.
Tne 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 resovered 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    NONMETHANE 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 (Ct - 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, QHj, CjH6, C4H10, C5H12, and C5H14) 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/FTD 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
-------
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                           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 nonrnethane 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 bv 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 pitot
tubes were calibrated before use following the directions in the  method. Also, the pilots
were leak checked before and after each run.
JBS33C                                  5-37
-------
      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   O; and CO2 Concentrations bv 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 (paniculate
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 wilh 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 impingers 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, NO^ 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 ihe
flue gas stream was split through  a manifold to the various analyzers. Total hydrocarbon
JBS336
                                      5-38
-------
measurements were made on an unconditioned, hot basis.  Therefore, this sample stream
bypassed the gas conditioner.
5.6,1   CEM 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 run. To take advantage of this
                                       C,"JQ
JBS336                                   J ">"
-------
property of SO2, the analyzer emitted UV light at 202.5 nm 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 SO, 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 Therrnox 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 ceil 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
CO, 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
-------
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 Monoxide 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 lo 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
JBSJ36                                  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 run (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, rnidrange gases for all instruments were analyzed,
with no adjustment permitted, as a quality control (QC) check. If the  QC rnidrange 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
                                        5-42
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                                Table 5-3
                 CEM Operating Ranges And Calibration Gases
               Analyte
         Gas Concentration
 CO,
       Instrument
       Range
       Span Gas Value
       Zero Gas
       Midrange QC Gas Value
       Low Range QC Gas Value
Beckman 880
0 - 20%
18%
100% N7 (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% N, (UHP)
60 ppm
20 ppm	
       Instrument
       Range
       Span Gas Value
       Zero Gas
       Midrange QC Gas Value
       Low Range QC Gas Value
Thermox WDG III
0-25%
20%'
0.2% O,
10%
5%
 S07
       Instrument
       Range
       Span Gas Value
       Zero Gas
       Midrange QC Gas Value
       Low Range QC Gas Value
Western 721A
0 - 200 ppmvd
180 ppm
100% Na (UHP)
100 ppm
30 ppm
JBS796
                                   5-43
-------
                                Table 5-3

                                Continued
               Ajialyte
         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% Nj (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
JBS19S
-------
      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 NO,, span gas.

      12.    Make adjustments to the NO, 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.
JBS336                                   5-45
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      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
      i cS i iTi G
      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.
JBS336
                                      5-46
-------
                  Stack
                   Wall
        Temperature /
          Sensor
           Temperature Sensor
                            Filter Holder
Gooseneck
  Nozzle
                                                                      Temper alure Sensor
                                                                                                      Tamperaluie Sensor
S-Typa Pttot Tube
Heal Traced
Quartz Probe
   Liner
                                                       Water Knockout  100 ml HPLC Water  Empty
                                                         Impinoer
                                                                                                                  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 brushes) 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 scxhiet and extracted in HPLC-grade water methyl alcnhnl,
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
     I.    Soak all glassware in hot soapy water (Alconox*).

     2,    Tap water rinse to remove soap.
     3.    Distilled/deionized H2O rinse (X3).'

     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)  = 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 Preliminary Measurements.  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 irnpingers
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. Sea!'"" as*»« wp.rp. nnf
                         r       J            o               DO
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 rale 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 pitot 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 fig per train.  The compounds/isomers of interest in
the analysis arc 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                                   5-52
-------
Probe Uner     Cyclone
 Front Half
Fitter House
       Filer Support
       and Back HaN
         of Filer
Filter     Housing
                                                                       1 si Impinge*
                                                                                                                                    Shlmplnger
                                               Condenser    XADTiap    (knockout)   2ndlmpinger  3rdbnpinger  4th Irnplnger   (silica gel)
                I
                                                               *           I
                                                                                                               I
  Attach
2SOmL flask
tobaBJoW

 Hkwawth
 Uathanol

MofleOmL
  botUa

Brush Hner
 and rinse
 Brush and
 rinse wtth
 melhenol
   uflrj
Brush and     Ca/etuDy   Rinse wtth
rinsawth   remove nier  msthanoJ
methanol   tramauppon    (3x)
                                   Rirnavth
                        Btusli
Thanriraa
autnaawlh
methytane
  _>_>	i^_
  cnionoe
meOiytanfi    partkulats
 cMondhi     Oflio nttf
                                   Rinse wtth
                                    mathanol
                                      (3x)

                                   Rinse wtth
                                   melhylene
                                    cMoiida
                                SecureXAD
                                   Ira
                                                            Weigh
                                                            Impinger
 Weigh
implngar
 Weigh
Implngar
 Weigh
Implngar
Check liner
  loaeal
parHculata
• removed
• noli
    3
  aBqouts
  mattirtana
             SeaJpatri
               dtoh
                                 bans and
                                  clamps

                                  Place In
                                 cooler lor
                                  storage
                                                             Empty       Empty       Empty       Empty
                                                          contents Into  contents Mo contents Into  contents Mo
                                                             botlla       bottle       bottle        bottle
 Weigh
Implngar

Discard
BlUcaged
                                                                        Rinse with
                                                                        mathanol
                                                            FUnaewth
                                                            methyiane
                                                             .T>->i.". •!• iat
                                                             CfpOtlCJO
                                                              prj
                                                                        Rinse wttt
                                                                        mathanol
                                                         RJnaewMi
                                                         mathylane
                                                                     Rinse wtth
                                                                      mathanol
                                                                                                RinaewUh
                                                                                                memylene
                                                                                                 chloride
                                                                                                Rinse wtth
                                                                                                mathanol
                                                                                                Rinse wtth
                                                                                                mathylane
                                                                                                 chkxWe
                                                                                                   (3K)
              PR
                                          CR
                                                 SM
                                                                 IR
                                         Figure 5-11.  PAH Field Recovery  Scheme
-------
                                    Table 5-5

              Polynuclear Aromatic Hydrocarbon Sample Components
                         Shipped to Analytical Laboratory
Container/Component
1
2
3
4
c
Code
F
PR
CR
IR
SM
Glassware
Filter(s)
Rinses3 of nozzle, probe, and front half
of filter holder
Rinses" of back half of filter holder,
filter support, and condenser
First, second, third, and fourth
irnpinger contents and r~nsesa
XAD-2 resin
aRinses include acetone and methylene chloride recovered into the same sample bottle.
JBS336
                                      5-54
-------
                         Table 5-6

Polymiclear Aromatic Hydrocarbon Compounds To Be Analyzed
                       Naphthalene
                       Acenapthylene
                       Acenapthene
                         Fluorene
                       Phenathrene
                        Anthracene
                       Fluoranthene
                          Pyrene
                    Benzo(a)anthracene
                         Chrysene
                    Benzo(b)fluoranth ene
                       Benzo(a)pyrene
                    2-Methylnapthalene
                    2-Chloronapthalene
                    Benzo(k) fluoran th e ne
                       Benzo(e)pyrene
                         Perylene
                   Indeno(l,2,3-cd)pyrene
                   Dibenz(a,h)anthracene
                       Dibenzofuran
               7,12-Dimethylbenz(a)anthracene
                    Benzo(g,h,i)perylene
                            5-55
-------
      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 OA/OC Procedures
      This section discusses the general quality centre! 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
-------
      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 D24G-S7, "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  Sarnpling^Equipment and Method.  Heat of combustion was determined
using an O: 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 thermoehemical 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 D15 52-90, "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 suifuric acid.
Nitrogen in the sample was converted  into ammonium salts by destructive digestion of
the sample with  a hot, catalyzed mixture of concentrated suifuric 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 alkaliaietric or
acidimetric  titratkm.
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.
-------
             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. Detailed QC procedures for all
manual flue gas sampling, process sample collection, GC operations, and CEM
operations can be found in the site-specific test plan prepared by Radian Corporation1.
This section presents the test program QA parameters and results so that the degree of
data quality can be shown.
6.1    SUMMARY
      Tests were conducted over a three-day period at Mathy Construction Company,
Plant 26, Three sets of runs were completed successfully at normal operating conditions
while the plant was operating on waste fuel oil.  No sampling-related problems that
would affect data quality were encountered during testing.
      In summary, the data quality was maintained throughout the project and this data
can be used as described. 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, with the exception of one
aldehyde run. This run was accepted because it exceeded the limits only slightly.  The
PM]0/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, a few method spike recovery values for the metals, aldehydes, and
PAH analyses were not within the QA allowance.
    ^'Emission Testing for Asphalt Concrete Industry, Site-Specific Test Plan and Quality
Assurance Project Plan,  Mathy Construction Company Plant 26," Radian  Corporation,
September 1991.
JBS342
-------
      The CEM results showed acceptable calibration drift values and QC gas

responses.  All CEM QC procedures and objectives described in the site-specific test

plan were followed.
      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 most of the runs conducted.
      The remainder of this section is organized as follows;  Section 6.2 presents the
QA/QC definitions and data quality objectives; Section 6.3 presents manual flue gas
sampling and recovery parameters, and a further discussion of method blank,  field blank,
and method spike results; Section 6.4 presents method-specific analytical QA  parameters;
Section 6.5 discusses the CEM QA parameters; and Section 6.6 presents the GC QA

parameters.
6.2   QUALITY ASSURANCE/QUALITY CONTROL DEFINITIONS AND
      OBJECTIVES
      The overall QA/QC objective in this test program was to ensure precision,
accuracy, completeness, comparability, and representativeness for each major
measurement parameter. The following  definitions were used:

       *     Quality Control:  The overall system of activities whose  purpose is to
             provide a quality product or service. Quality control procedures are
             routinely followed to ensure high data quality.

       •     Quality Assurance:  A system of activities whose purpose is to ensure that
             overall QC is being  carried out effectively. The degree of data  quality
             achieved can be assessed from QA parameters.

       •     Data Quality:  The characteristics of a product  (measurement data) that
             bear on  its ability to satisfy a given purpose.  These characteristics are:

                   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 is expressed as the  relative
                   standard deviation or coefficient of variation.
JBS342
                                        6-2
-------
                  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, which 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.
                  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.
6.3    MANUAL FLUE GAS SAMPLING QUALITY ASSURANCE
      The following section reports manual sampling QA parameters in order to
provide insight into the quality  of the emissions test data produced from manual tests
during the test program.
6.3.1  Particulate Matter/Metals Sampling Quality Assurance
      Table 6-2 presents post-test check results for all of the manual  sample  trains. The
acceptance criterion was that all post-test leak checks be less than 0.02 cfm. All
PM/metals post-test leak checks met the acceptance criterion.
      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. All PM/metals runs deviated by no more than 3 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
      v
JBS342                                   6'3
-------
                                     Table 6-1
            Summary of Precision, Accuracy, and Completeness Objectives

:"-. -^-Vr >-/-••- • Parameter Xf •;•;;:;• -^ •
Flue Gas Formaldehyde
Flue Gas Metals
Polymiclear 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
±0.3%V
±20
±2°F
Accuracy"
4%) :
±20
±30C
±20
±10
±2d
±10
±0.5%V
±10
±5°F
: Completeness11
>:>•'• (%)
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.

"Minimum 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 analyses, where:
              Percent Difference  =   First Value  -  Second Value x 1QQ
                                    0.5 (First  +  Second Values)
eMinimum requirements of EPA method 6C, based on percent of full scale.
JBS342
                                            6-4
-------
Table 6-2
LEAK CHECK RESULTS FOR MANUAL SAMPLE TRAINS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
  PM/Metals
  PM/Meials
  PM/Metals

  Aldehydes
  Aldehydes
  Aldehydes
  Aldehydes

    PAH
    PAH
    PAH

    PM10
    PM10
    PM10
09/23/91
09/23/91
09/24/91

09/23/91
09/23/91
09/25/91
09/24/91

09/23/91
09/23/91
09/24/91

09/24/91
09/25/92
09/25/91
1
2
3

1
2
3
4

1
2
3

1
2
3
1
1
1

2
2
1
1

4
3
4

1
1
1
0.33
0,33
0,33

0.50
0.56
0.4S
0.34

0.34
0.35
0.32

0.25
0.28
0.31
0.012
0.014
0.012

0.010
0.006
0.014
0.010

0.008
0.010
0.008

0.010
0.012
0.016
5
5
8

7
5
6
6

7
5
7

10
10
5
Yes
Yes
Yes

Yes
Yes
Yes
Yes

Yes
Yes
Yes

Yes
Yes
Yes
                                             6-5
-------
Table 6-3
ISOKINETIC SAMPLING RATES FOR MANUAL SAMPLING TEST RUN
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
   PM/Metals
   PM/Metals
   PM/Metals

   PM10/CPM
   PM10/CPM
   PM10/CPM

   Aldehydes
   Aldehydes
   Aldehydes
   Aldehydes

      PAH
      PAH
      PAH
09/23/91
09/23/91
09/24/91

09/24/91
09/25/91
09/25/91

09/23/91
09/23/91
09/24/9!
09/25/91

09/19/91
09/19/91
09/20/91
1
2
3

1
2
3

1
2
3
4

1
2
3
102
97.9
100

89.1
91.4
80.8

98-8
112
95.8
96.0

107
106
105
 Yes
 Yes
 Yes

 Yes
 Yes
 Yes

 Yes
Yes b
 Yes
 Yes

 Yes
 Yes
 Yes
a PM/Metals, Aldehydes and PAH lest metals specify isokinetic sampling rates must be within
  10 percent of 100 percent isokinetic. The PM10 lest method allows ioskinetic sampling rates
  to be within 20 percent of 100 percent isokinetic.
b Marginally accepted because it did not exceed prescribed tolerances by a large amount.
                                           6-6
-------
verify the full calibration, a post-test calibration was performed.  The full- and post-test
calibration coefficients must be within 5 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
5 percent criterion of the full calibration factor.
6.3.2  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 within QA allowances and are presented in Tables 6-2,
Table 6-3, and 6-4, respectively.  Note that the isokinetic acceptance criterion for
PM10/CPM runs is more lenient than for other methods, allowing the average sampling
rate to be within 20 percent of 100 percent isokinetic.
6.3.3  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 for Runs 1, 3, and 4. Run 2 was  slightly out of QA acceptance
with an isokinetic rate of 112 percent.  However, the run was  accepted because the
deviation from acceptable limits was so slight. Post-test leak check results, isokinetic
values, and dry gas meter calibration results for the aldehydes runs  are presented in
Tables 6-2, 6-3, and 6-4, respectively.
6.3.4  Polynuclear^Aromatic Hydrocarbon Sampling Quality Assurance
      The post-test leak check results for the PAH trains  are presented in Table 6-2.
All the trains met the QA acceptance criterion.  Isokinetic rates, presented in Table 6-3,
varied no more than 6 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.
6.4   ANALYTICAL QUALITY ASSURANCE
      The following sections briefly report QA parameters for the metals, PM10/CPM,
aldehydes, and PAH analytical results.  Field  blanks were collected for the PM/metals,
PM10/CPM, aldehydes, and PAH sampling trains. A train of each sample type was fully
JBS142                                    6-1
-------
Table 6-4
DRY GAS METER POST-TEST CALIBRATION RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
                                                     "<$>t£$M
                                                     yK^raKWiwipSyfft'S'ai^Sf&KSft";
                                                     %^3^M«@%^^»^^g^
                                                             ^ jirii-.-i' -;o;-;-
                                                             l.UM^RgR;,-
     N-30
     N-32
     N-33
   PAH


 Aldehydes


PM/Melals -
PM10/CPM
0.9998
L0006
0.9875
1.0218
1.0051
0.9788
2.20
0.45
-0.88
Yes
Yes
Yes
a [(Posi-Test)-(Full)]/(Full)*100
                                      6-8
-------
prepared, taken to the sample location, leak checked, and then recovered. The
analytical methods used for the flue gas samples are discussed fully in Section 5.
6.4.1   Metals Analytical Quality Assurance
       Table 6-5 presents the results  of the metals field blank analysis compared to the
test run results.  There was a noticeable contamination of certain metals in the blank.
The front-half fraction was contaminated with all of the metals except Se, Ag, and Tl.
The back-half fraction was contaminated with Mn, Ni, and P.  The flue gas samples were
blank corrected based on field blank results.
       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.  Because the
flue gas samples were blank corrected for the field blank, no corrections were needed for
the method  blank.
       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. Poor Ag method blank recoveries may be due  to the  fact that silver nitrate
solutions are light-sensitive and have a tendency to plate  out on container walls.  No
spike  corrections were applied.
6.4.2   PMia/CPM Analytical Quality Assurance
       Table 6-8 presents the results  of the PM10/CPM field blank  analysis compared to
the test run  results. Amounts of PM10 were detected in the field blank within all of the
separate analytical fractions.  The total amount detected was 3.2 percent of the average
total for the three runs. 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  mg. 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
JBS342                                    "~"
-------
        Table 6-5
        METALS FIELD BLANK RESULTS COMPARED TO TEST RUN RESULTS
        MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
                     ^fS:M;^^?S^SSS»SS®Sfi!8!»S*Si|PS:Sr:p
                     &^ssj*si¥fts*s
O
Anlimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
 15.1
 23,5
 64,3
0.550
 2,25
 101
 23.0
 31.0
 82.0
 138
 315
[4.00]
 5.18
[25.0)
 249
 [1.69]
[0.423]
 1,32
[0.106]
 0.254
 1,26
 1.07
 0.355
 1.84
 2.59
 64.9
 [1,69]
[0.634]
 [10,6]
 14.4
 15.1
 23.5
 65.6
0.550
 2.50
 102
 24.1
 31.4
 83.8
 141
 380
[569]
 5.18
[35.6]
 263
 11.8
 20.2
 40.0
0.425
 3.10
 105
 19.4
 28.3
 94,0
 99,8
 306
[4.00]
 7.45
[25.0]
 268
 [1.58]
[0,421]
 1.66
[0.105]
 0.716
 3.07
 2.89
 3.50
 24.8
 4.69
 73.1
 [1.68]
[0.631]
 [10,5]
 24.3
 11.8
 20,2
 41.7
0.425
 3.82
 108
 22.3
 31.8
 119
 104
 379
[5,68]
 7.45
[35.5]
 292
 9,58
 27.0
 79.8
0.275
 4,70
 27.8
 37.0
 36.8
 105
 13.3
 360
[4.00]
 5.05
[25.0]
 316
[1.58]
[0.421]
 1.33
[0.105]
[0.210]
 1.30
[0.421]
0.969
 2.01
 2.04
 67.5
[1.68]
[0.631]
[10.5]
 5.84
9,58
27.0
81,1
0,275
4.70
29.1
37.0
37.8
 107
15.3
428
[5.68]
5.05
[35.5]
322
 9.38
 16.1
 45.0
0.400
 1.18
 24.5
 2.60
 8.13
 55.3
 15.3
 112
[4,00]
[1.50]
[25.0]
 69.5
[1.68]
[0,447]
[O.I 12]
[0.112]
[0.224]
(0.671]
[0.447]
[0.335]
0.447
0.369
 50.2
[1.79]
[0.671]
[11.2]
[1.68]
 9,38
 16.1
 45.0
0.400
 1.18
 24.5
 2.60
 8.13
 55.7
 15.7
 162
[5.79]
[2.17]
[36.2]
 69.5
        [ ] = Minimum Detection Limil
-------
Table 6-6
METALS FLUE GAS METHOD BLANK RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Nickel
Phosphorous
Selenium
Silver
Thallium
Zinc
[1.50J
[0.400]
[0,100]
[0.100]
[0.200]
[0.600]
[0.400]
[0.300]
0.330
[0.300]
[30.0]
[1.50]
[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]
[ ] = Minimum Deteclion Limit.
( ) = Estimated Value.
                                   6-11
-------
Table 6-7
METALS METHOD SPIKE RESULTS
MATHY CONSTRUTION COMPANY PLANT 26 (1991)
                    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 26 (1991)
Analysis
',-•;• • -::
.:"•" --;,-.... . . '.
Filter
MeC12
H2O
Cyclone
Total
Run 1
(grams)
0.0070
0.0048
0.0036
0.0207
0.0361
, - .•:• :'-•.-<-•.-.-:•
• . •<. .• _.;•:-. ' '-'-'•:-
y. -(grams)lll
0.0080
0.0087
0.0628
0.0296
0.1091
•"*
il<|niins>;;'.::
0.0086
0.0035
0.0287
0.0288
0.0696
1 ISH
:\:'x;'(grams)ii
0.0004
0.0006
0.0008
0.0005
0.0023
                              6-13
-------
the water blank and the methylene chloride blank was less than 3 mg, as specified in the
test method.
6.4.3   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 flue gas samples were blank-corrected.
       The aldehydes method blank results for the flue gas samples are presented in
Table 6-10.  Acetone and formaldehyde were  detected in the flue gas method blank at
low levels. Because the samples were blank corrected for the field blank, they were not
blank corrected for the method  blank.
       Table 6-11 presents the method spike results for the aldehyde  analysis.  All spike
recoveries were within the ±20  percent of the 100 percent criterion except for
acetophenone/o-toiuaidehyde at 70 percent recovery, acrolein at 23 percent recovery,
crotonaldehyde at 25 percent recovery, and  quinone at 64 percent recovery. No spike
corrections were applied.
£ A A   TD I r*«  1
VF.T.T   fc Q.iViiUv*^m_
       Table 6-12 presents the PAH field blank results compared to the test run results.
Naphthalene was detected in the field blank at an estimated level.  The flue gas samples
were blank-corrected.
       TVi*a PAU m^+l-if\,r1 Vfclortl' r^ciilt£ fXr tliA -fliio rrnc comrilefcC1 ires  r\r£*c£*rt+t*d 1*1
       A HW M, A *-*.*. i.ilWV4AlwfVJ LSAUlAJt. J. WtJ U IfctJ A.UL LJ.1W .LJ.UW r *T^ tJUA.J.!LSl.^iJ U.A W  L/l ^ J W14IWU IAA
Table 6-13.  Naphthalene was detected in the flue gas method blank at estimated levels.
       Table 6-14 presents the method spike results for the PAH analysis. All spike
recoveries were within the QA criterion of ±20 percent of 100 percent except for
nitrnnhpnol  np-ntarhlnrnnhpnnl and Hi-n-hiitvlnJithsilatp   Mr» cnilv  rnrr/a/'tinnc u«»rp
	»,j	., r-_..—-...—- —j,—-—_-, —~ — — ..^.j.j—.,u_~^._.  - ._ _r—».  .	_«.,M-~J .,..—
applied. Table 6-15 presents the PAH surrogate recovery results.  2-Fluorobiphenyl was
out of the laboratory control limits for Run 1, Run 3, and the Method Spike, but
nitrobenzene-d5 and terphenyl-d!4 were within control limits for all sample runs.
6.5    CONTINUOUS EMISSION MONITORING QUALITY ASSURANCES
       Flue  gas was analyzed continuously for O2/CO2, CO, SO2, NOX, and THC using
EPA Reference Methods 3A, 10, 6C, 7E, and 25A. Daily QA/QC  procedures were

JBS342                                   6-14
-------
TABLE 6-9
ALDEHYDE FIELD BLANK RESULTS COMPARED TO TEST RUN RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Ace (aldehyde
Aceione
Acelophenone/o-Tolualdehyde
Acrolein
Benzaldehyde
Bulyraldehyde/Isobutyraldehyde
Croionaldehyde
2,5-DimethylbenzaIdehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehyde
MIBK/p-Tolualdehyde
Valeraldehyde
3530
2180
[23,0]
 107
86,4
 484
 109
[24.0]
2070
 190
[18,0]
75.1
[23.0J
89.1
1220
2280
[23.0]
[13.0]
65.3
 253
48.1
[24.0]
2100
 136
[18.0J
[18.0]
[23.0]
62.9
5880
2280
[23.0]
[13.0]
 757
 633
 561
[24.0]
11800
 519
[18.0]
 138
[23.0]
 344
2560
2710
[23.0]
 134
 135
 237
 102
[24.0]
3050
 200
[18.0]
 85.3
[23.0]
 134
[11.0]
 3%
[23.0]
[13.0]
[21.0]
[18.0]
[18.0]
[24.0]
 14.5
[20.0]
[18.0]
[18.0]
[23.0]
[18-0]
[ ] = Minimum Detection Limit
                                            6-15
-------
Table 6-10
ALDEHYDE FLUE GAS METHOD BLANK RESULTS
MATHY CONTRUCTION COMPANY PLANT 26 (1991)

Acetaldehyde
Acetone
Acelophenone/o-Tolualdehyde
Acrolein
Benzaldehyde
Butyraldehyde/Isobutyraldehyde
Crotonaldehyde
2,5-Dimethylbcnzaldehyde
Formaldehyde
Hexana]
Isophorone
Isovaleraldehyde
MIBK/p-Tolualdehyde
Methyl Eihyl Ketone
Propionaldehyde
Quinone
m-Tolua'ldehyde
Valeraldehyde	
[0.580]
 2.74
 [1.20]
[0.710]
 [1.10]
[0.940]
[0,940]
 [1.30]
 1.24
 [1.10]
[0.940]
[0.980]
[[1.20]
[0.940]
[0.730]
[0.940]
 [1.20]
[0.980]
[ ] = Minimum Detection Limit.
                           6-16
-------
Table 6-11
ALDEHYDE METHOD SPIKE RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Acetaldehyde
Acetone
Aceiophenone/o-Tolualdehyde
Acrolein
Benzaldehyde
Butyraldehyde/Isobutyraldehyde
Crotonaldehyde
2,5-Dimethylbenzaldehyde
Formaldehyde
Hexanal
Isophorone
Isovaleraldehyde
MIBK/p-Tolualdehyde
Methyl Ethyl Ketone
Propionaldehyde
Quinone
m-ToIualdehyde
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%
NS = Not Spiked
NA = Not Analyzed
                            6-17
-------
Table 6-12
PAH FIELD BLANK RESULTS COMPARED TO TEST RUN RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

Acenaphthylene
Acenaphlhlene
Anthracene
Benzo(a)amhracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)pery!ene
Benzo(k)fluoranthene
2-Chloronapthalene
Chrysene
Dibenz(a,h)anthracene
Dibenzofuran
7,12-Dimeihylbenz(a)anthracene
Fluoranlhene
Fluorene
Indeno(l,2,3-cd)pyrene
2-MelhyInaphthalene
Naphthalene
Perylene
Fhenanthrene
Pyrene

[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[20000]
[10000]
[10000]
[10000]
[10000]
1810
[10000]
[10000]
[10000]

[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[20000]
[10000]
[10000]
[10000]
[10000]
3010
[10000]
t-i f\n/~\j~ii
flUlAAJJ
[10000]

[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[10000]
[20000]
[10000]
[10000]
[10000]
[10000]
1410
[10000]
n rwvn
JIUIAJVJJ
[10000]

[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]
[50.0]
(87.4)
[50.0]
ren m
l-"J'"J
[50.0]
( ) = Estimated Values
NOTE: PAH values have been blank corrected.
                                    6-18
-------
Table 6-13
PAH FLUE GAS METHOD BLANK RESULTS
MATHY CONSRTUCnON COMPANY PLANT 26 (1991)
Acenaphihylene
Acenaphihlene
Anthracene
Benzo(a)anthracene
Bei\zo(a)pyrene
Benzo(b)fluoran(hene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranlhene
2-Chloronapihalene
Chrysene
Dibenz(a,h)anthracene
Dibenzofuran
7,l2-Dimethylbenz(a)anthracene
Fluoranthene
Fluorene
Indeno(l,2,3-cd)pyrene
2-Methylna phthalene
Naphthalene
Perylene
Phenanlhrene
Pyrene	•
 [50,0]
 [50,0]
 [50,0]
 [50.0]
 150.0]
 [50.0]
 [50.0]
 [50.0]
 [50.0]
 [50.0]
 [50.0]
 [50.0]
 [50.0]
 [100]
 [50.0]
 [50.0]
 [50.0]
 [50.0]
(0.370)
 150.0]
 [50.0]
 [50-0]
[ ] = Minimum Detection Limit.
( ) = Estimated Values
                                6-19
-------
Table 6-14
PAH METHOD SPIKE RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Phenol
2-Chlorophenol
1,4-Dichlorobenzene
N-Nitroso-di-n-propylamine
1,2,4-TrichIorobenzene
4-Chloro-3-methylphenol
2,4-Dinitrotoluene
Penlachlorophenol
Di-n-butylphlhalate
4.Nitrophenol     	
84.8%
94.2%
95.6%
104%
109%
99.9%
98,4%
26.6%
2.15%
53.0%
                             6-20
-------
Table 6-15
PAH SURROGATE RECOVERY RESULTS
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)

                              rwlo^iiSiSix::':^:^:":^:'^;!:
2-Fluorobiphenyl
Nilrobenzene-d5
Terphenyl-dl4
132%
102%
85.1%
107%
102%
90.3%
135%
122%
85.8%
59.4%
39,4%
44.8%
99.2%
81.8%
101%
143%
105%
127%
30% to 115%
23% lo 120%
18% lo 137%
-------
followed in accordance with the QA/QC guidelines in the reference methods and Radian
standard operating procedures.  These procedures are fully detailed in the site-specific
test plan,  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.
6.5.1  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 had to be within ±2 percent of
full scale for  the linearity check to be considered acceptable.  The results of this check
for the different instruments are presented in Tables 6-16 through 6-21.
      In addition to conducting the linearity check, 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 in order to conserve gases that were available in limited
quantities, or if the span gas was closer to the observed concentrations. Because
production runs were limited, drift check was not determined between every manual run
in order to allow for completion of as many manual method tests as possible while  the
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 span-gas observed response was compared iu  uic initial span-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 was met in all cases except for one
inter-run check of the NOK analyzer;  however, the overall drift for this analyzer over the
entire test period was determined as  -0.4 percent, which is within ±3 percent limit.
JBS342
                                        6-22
-------
Table 6-16
METHOD 3A OXYGEN ANALYZER AND DRIFT SUMMARY
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Instrument: Therrnox WDGm Serial Number: 35983-1
Full Scale Concentration: 25 %V
V:;;Pate^t:
;;: .:Timet-; .
QC Gas
Certified
Gas Cone.
bc*v)
Observed
Gas Cone.
(%V)
Difference
(%V)
Difference
Percent
Scale
(%)
Multipoint Linearity a
9/23/91
9/23/91
08:12
08:12
Zero:
Span:
0.0
18.0
0.0
18.0
0.0
0.0
0.0
0.0
Inter-run Drift Summary b
9/23/91
9/23/91
9/23/91
9/23/91
9/24/91
9/25/91
11:06
12:40
14:45
16:46
15:12
15:55
Mid:
Mid:
Mid:
Mid:
Mid:
Mid:
7.99
7.99
7.99
7.99
7.99
7.99
7.7
7.7
8.1
7.5
7,8
7.4
-0.3
0.0
0.4
-0.6
0.3
-0.3
-1.2
0.0
1.6
-2.4
1.0
-1.4
Test Period Drift Summary c
9/25/91
15:55
Span:
18.0
18.4
0.4
1.6
a Multipoint Linearity - Difference Percent Scale = (observed cone - certified conc)/rull scale * 100%.
b Inter-run Drift - Difference Percent Scale = (current cone - previous observed conc)/full scale * 100%,
c Drift Summary - Difference Percent Scale = (final observed cone - initial observed conc)/fiill  scale • 100%.
                                                6-23
-------
Table 6-17
METHOD 3A CARBON DIOXIDE ANALYZER AND DRIFT SUMMARY
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Instrument: BecEman 865 Serial Number: 0103778
Full Scale Concentration: 20 %V
Date
Time
QCGas
Certified
Gas Cone.
(%V)
Observed
Gas Cone.
(%V)
Difference
,(%V)
Difference
Percent
Scale
(%)
Multipoint Linearity a
9/23/91
9/23/91
08:12
08:12
Zero:
Span:
0.0
17.0
0.0
17.0
0.0
0.0
0.0
0.0
Inter-run Drift Summary b
9/23/91
9/23/91
9/23/91
9/23/91
9/24/91
9/25/91
11:06
12:40
14:45
16:46
15:12
15:55
Mid:
Mid:
Mid:
Mid:
Mid:
Mid:
9.91
9.91
9.91
9.91
9,91
9.91
10.3
10.3
10.4
9.8
10.2
10.5
0.4
0.0
0.1
-0.6
0.4
0.3
2.0
0.0
0.5
-3.0
2.0
1.5
Test Period Drift Summary c
9/25/91
15:55
Span:
17.0
17.2
0.2
1.0
a Multipoint Linearity - Difference Percent Scale = (observed cone - certified conc)/full scale * 100%.
b later-run Drift - Difference Percent Scale = (current cone - previous observed cone)/full scale * 100%,
                                                   jt
c Drift Summary - Difference Percent Scale = (final observed cone - initial observed conc)/full scale * 100%.
                                              6-24
-------
Table 6-18
METHOD 6C SULFER DIOXIDE ANALYZER AND DRIFT SUMMARY
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Instrument: Western Research 721 AT2 Serial Number: 90-721AT2-7654-1
Full Scale Concentration: 500 ppniV
Date
Time
QCGas
Certified
Gas Cone.
(ppmV)
Observed
Gas Cone.
(ppmV)
Difference
(ppmV)
Difference
Percent
Scale
(%)
Multipoint Linearity a
9/23/91
9/23/91
08:12
08:12
Zero:
Span:
0.0
295.0
0.0
295.0
0.0
0.0
0.0
0.0
Inter-run Drift Summary b
9/23/91
9/23/91
9/23/91
9/24/91
9/25/91
11:06
12:40
16:46
15:12
15:55
Span:
Span:
Mid:
Mid:
Mid;
295.0
295.0
98.0
98.0
98.0
295.0
302.0
101.0
105.0
106.4
0.0
7.0
-3.0
4.0
1.4
0.0
1.4
-0.6
0.8
0.3
Test Period Drift Summary c
9/25/91
15:55
Span:
295.0
293.0
-2.0
-0.4
a Multipoint Linearity - Difference Percent Scale — (observed cone - certified conc)/full scale • 100%.
b Inter-run Drift - Difference Percent Scale = (current cone - previous observed conc)/full scale * 100%.
c Drift Summary - Difference Percent Scale = (final observed cone - initial observed conc)/full scale * 100%,
                                              6-25
-------
Table 6-19
METHOD 7E NITROGEN OXIDES ANALYZER AND DRIFT SUMMARY
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Insfrumeot: TECO 10AR Serial N&nfe: 25558-221
.,..,- -. • - . • ..-.•.•- • •. - . . . . .'•:-, . , . - 	 .,......,-.. ....
M Sl^e Conception: 250ppmV ' ^r^SS'.
Date
;^ Tinier'
QC Gas
^Certified''.
Gastoricr
(ppmV)
JWifiiii
"Gaii;'Cflnc|:
• tffimyfll
iMHerence
(ppmV)
Difference
Percent,
Scale
(%)
Multipoint Linearity a
9/23/91
9/23/91
08:12
08:12
Zero:
Span:
0.0
201.0
0.0
201.0
0.0
0.0
0.0
0.0
Inter-ma Drift Summary b
9/23/91
9/23/91
9/23/91
9/24/91
9/25/91
11:06
12:40
16:46
15:12
15:55
Span:
Span:
Mid:
Mid:
Mid:
201.0
201.0
97.0
97.0
97.0
192.0
201.0
99.0
96.0
104.0
-9.0
9.0
2.0
-3.0
8.0
-3.6
3.6
0.8
-1.2
3.2
Test Period Drift Summary c
9/25/91
15:55
Span:
201.0
200.0
-1.0
-0.4
a Multipoint Linearity - Difference Percent Scale = (observed cone - certified conc)/full scale * 100%.
b Inter-run Drift - Difference Percent Scale = (current cone - previous observed conc)/full scale • 100%.
c Drift Summary - Difference Percent Scale = (final observed coac - initial observed conc)/full scale • 100%.
                                              6-26
-------
Table 6-20
METHOD 10 CARBON MONOXIDE ANALYZER AND DRIFT SUMMARY
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Instrument: TECO48 Serial Number: 4829758-236
Full Scale Concentration: 500 ppraV
Date
Time
QCGas
Certified
Gas Cone.
(ppmV)
Observed
Gas Cone.
(ppmV)
Difference
(ppmV)
Difference
Percent
Scale
(%)
Multipoint Linearity a
9/23/91
9/23/91
08:12
08:12
Zero:
Span:
0.0
474.0
0.0
474.0
0.0
0.0
0.0
0.0
Inter-run Drift Summary b
9/23/91
9/23/91
9/23/91
9/24/91
9/25/91
12:40
14:45
16:46
15:12
15:55
Span:
Mid:
Mid:
Mid:
Mid:
474.0
92.1
92.1
92.1
92.1
482.0
92.5
93.7
92.1
90.0
8.0
0,4
1.2
-1.6
-2.1
1.6
0.1
0.2
-0.3
-0.4
Test Period Drift Summary c
9/25/91
15:55
Span:
474.0
466,0
-8.0
-1.6
a Multipoint Linearity - Difference Percent Scale = (observed cone - certified conc)/full scale * 100%.
b Inter-run Drift - Difference Percent Scale = (current cone - previous observed conc)/full scale • 100%.
c Drift Summary - Difference Percent Scale = (final observed cone - initial observed conc)/full  scale * 100%.
                                              6-27
-------
Table 6-21
METHOD 25A TOTAL HYDROCARBON ANALYZER AND DRIFT SUMMARY
MATHY CONSTRUCTION COMPANY PLANT 26 (1991)
Instrument: Ratfisch55 Serial Number: 212291
Full Scale Concentration: 1000 ppmV
.'fDate
Time
QCGas
Certified
Gas Cone.
(ppmV)
Observed
Gas Cone.
(jppmV)
Difference
(ppmV)
Difference
Percent
Scale
(%)
Multipoint Linearity a
9/23/91
9/23/91
9/24/91
08:12
08:12
11:58
Zero:
Mid:
Span:
0.0
95.3
810
0.0
95.0
810
0.0
0.3
0.0
0.00
0.03
0.00
Inter-run Drift Summary b
9/23/91
9/23/91
9/24/91
9/25/91
12:40
16:46
15:12
15:55
Mid:
Mid:
Span:
Span:
95.3
95.3
810
810
94.5
102.5
811.0
817.0
-0.5
8.0
1.0
6.0
-0.05
0.80
0.10
0.60
Test Period Drift Summary c
9/25/91
15:55
Mid:
95.3
97.6
2.6
0.26
a Multipoint Linearity - Difference Percent Scale = (observed cone - certified conc)/full scale • 100%.
b Inter-run Drift - Difference Percent Scale = (current cone - previous observed conc)/full scale * 100%.
c Drift Summary - Difference Percent Scale = (Final observed cone - im'rial observed concVfull scale • 100%.
                                              6-28
-------
6.5.2   Line Bias Checks
      Radian performed all multi-point and QC 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 the line bias checks described in
Methods 3A, 7E, and the test  plan.
6.5.3  Leak Checks
      Because 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.
6.6   GAS CHROMATOGRAPHY QUALITY ASSURANCE
      EPA Method 18 analysis of the flue gas was performed using a GC to separate
the hydrocarbon (Q-Cg) species in the  gas stream.  At the  beginning of each test day,
and 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).  The calibration drift values are shown in Table 6-22.  A Post-test Response was
not conducted on the second day  of testing. Most of the drift values were within the  QA
allowance criterion of 10 percent.  The compounds that did not meet  this criteria were
benzene on the first day of testing, and pentane, hexane, ethylbenzene, and xylene on the
third day of testing.
JBS342
-------
        Table 6-22
        GC RESTONSE FACTOR DRIFT VALUES
        MATHY CONSTRUCTION COMPANY PLANT 26 (i;99l)
Dale
Compound
Methane
Ethane
Propane
Butane
Penlane
Hexane
Benzene
Toluene
Elhylberuene
Xylene
9/23/91
Pre-Tesl
Response
Factor a
3.7905E-05
1.8466E-OS
1.2269E-05
8.9445E-06
7.2191E-06
6.2334E-06
6.2892E-06
5.1461E-06
4.3137E-06
3.9692E-06
Post-Test
Response
Factor a
4.0398E-05
1.8494E-05
1.2237E-05
9.1091E-06
7.2154E-06
6.30B8E-06
5.5769E-06
ND
3.9281E-06
3.7633E-06
Drift
(%) 1.
-6.,'i 8
-0.15
0.26
-1,34
0.05
-1.21
11.33
ND
8.94
5.19
->V;' 1 9/24/91
Pre-Test
Response
Factor a
3.8790E-05
2.0130E-05
1.2860E-05
9.1560E-06
7.3835E-06
6.4075E-06
6.1030E-06
2.9780E-06
4.8500E-06
4.9210E-06
Post-Test
Response
Factor a
ND
ND
ND
ND
ND
ND
. ND
ND
ND
ND
Drift
(%) b
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
9/25/91. ,-s-B •.:•;: v
Pre-Test
Response
Factor a
3.2275E-05
1.5665E-05
I.0435E-05
7.7740E-06
6.3380E-06
5.4855E-06
5.1640E-06
5.9850E-06
4.0110E-06
3.8220E-06
Post-Test; :
Response
; Factor a
2.9360E-05
1.4370E-05
9.S230E-06
7.0230E-06
5.6400E-06
4.8820E-06
5.3010E-06
6.4060E-06
4.4210E-06
4.4090E-06
Drift
4%) b
9.03
8.27
8.74
9.66
11.01
11.00
-2.65
-7.03
-10.22
-15.36
u>
o
        ND = Not Determined
        a  Response Factor = Calibration Gas Concentration (ppm)/Peak Area Count
        b  Drift Percent = ((Post-Test Resfionse Factor - Pre-Test Response Factor)/Post-Test Response Faclor) x 100
-------
             APPENDIX A

EMISSIONS TESTING FIELD DATA SHEETS

           A,l   PM/Metals
           A.2   PM10/CPM
           A.3   Aldenydes
           A.4   PAH
-------
APPENDIX A.1




 PM/METALS
-------
                         SOURCE  SAMPLING  FIELD  DATA
PLANT NAME
                                                                            Page  /  of,
SAMPLING LOCATION
DATE
                             3d
                                       RUN NO.
                                       TIME FINISH
                                       DIAMETER _
  DUCT DIMENSIONS   43    X  _____	
|r PTCFJQCefr     DGMCF  | ,15      NOZZLE DIA. J 9 /     inches
                          _ TEST DURATION _
                          _ft INITIAL LEAK RATE
                            FINAL LEAK RATE  •
                                                                                       min.
                                                                                   S"'Cfm
BAR PRESS	
STATIC PRESS
                        H2O
                                         OPERATOR
                                                  -r&P
Travers
 Point
         Clock
         Time
              Dry gas mater
               reading It3
                           -p
                         lnH2O
lnH2O
 Stack
Temp. F
              Dry gas meter tamp
Inlet
Outlet
Hoi box
Temp.
Probe
Temp
  Last
Impinger
Vacuum
 in. Hg
                                                5"!
                                                r/
                                 . JL
                          .-25
 6
          lo
          'i
                 Tt.l
                                                $3
                                                                           47
                          -61
  J
                  JfcO.1
                          fo

               Itfk-o
                                                       Al

                                        55J?
                /3.
                                                   7>
        /on
                                          toe,
                                                K
                                                       70
               Ji
                                                          ?
                                                        71
                                                                             m,
 3-

                          .ffl
                                 ,43 I  ••
                                                 77
                                                        73
  CONSOLE #_
  FILTER f JL
                                       PROBE LENGTH _
                                       LINER MATERIAL.
AMBIENT TEMP,
WEATHER
REMARKS I/, „
         -  65"
-------
                  MOISTURE AND IMPINGER CATCH DATA SHEET
impinger
Number Solution Appro*, ml
1 MT —
2 hUc^/HzO, Sot
HKWMzfl, 9^
'4 Mt -""
s Sil^lrfl QkWfcLj
6

Total Impinger Weight Gain (\Nc)j\S^mL grms
Vf o Final Meter Volume = ft3
Vi = initial Meter Volumes tt3
DGMCF as Dry Gas Meter Correction Factor =
Vm = Metered Gas Volume = (Vf-Vi)(DGMCF) =
Tm D Average Meter Temp. = F+460 = R
nu ss nnistef Prassurs (BaiorTistriC Prsssurs) —
Weight
Configuration in grams
k/yjljC?*^ Final 9 " T /* " & *
Initial "T^f[^pa| L/<^5.^
tMiaG-S Final 639,1
Iniiial fff':^5'tp
w/)Ofcr-> p"13' (03~jt$
Initial ^^6(?
I/HWI 6 "^ Final 4^iO^
Iniiial 4^« I
»W)£> fe^ Final "7^?* 3
initial -73/.V
Final
Initial

Analyst 	

%C02
' <*>G2
M3 CONDENSED WATER
FILTER WT. GAIN
PROBE WASH WT, GAIN
in LJn
— "'•• « "a
Weight J^^ » "1
Gain £4*7^
Weight
Gain 3i '
weight
Gain [ |
Weigh!
Gain 0- ^
Weighi
Gain {OH
Weight
Gain


%H2
%CH
grns
	 nflms
	 gms

                                                                                    JBc_
Vm (std)
             (17.64)(VmKPm)  (17.64)(	ft3)(	*Hg)
                  Tm                    (	 R)




   (stri) = Volume of Water Vapor = .0472(Wc) = .0472(^	g) =	ft3
Vw(std)
                                                    ft3
Bws = Moisture Fraction =
Vw(std) + Vm(std  _ M3
                                                      ft3 = ,
Rtvann Daw 2/91
-------
                                                                                     r.ft;:f -;.<:
                            SOURCE SAMPLING  FIELD  DATA
     PLANT NAME
          Nua
SAMPLING LOCATION.:
DATE
     b
                                                                  Page.
                                                                           ol
TIME START.
DUCT DIMENSIONS	
PTCF / &?CO   DGMCF  <• 75"
BAR PRESS	• Hg
STATIC PRESS ^&&-    H2O
                                  RUN NO
                                  TIME FINISH
                                  DIAMETER _
                                              ..Mgfete-2-
                                                            TESTDUflATTON
                                                                                  mm.
                NOZZLE DIA.
                                                    inches
                       .11 INITIAL LEAK RATE Q.
                         FINAL LEAK RATE _L
                                         OPERATOR
     Travers
      Point
       Clock
       Time
Dry gas mater
 reading «3
                       -p
                      inH2O
 •H
inHZO
 Stack
Tamp. F
Dry gas meter temp
  Inlet    Outlet
Hot box
Temp.
Prooe
Temp
  Last
Impinger
vacuum
 in. Hg
.Ml
                              ^1.
                                                       7 I
                                           221

                                         J/S'
                              1
                                                   7-S"
                            ,7
                                                   7s"
                                          13
            IH3L
                            -rf
            mm
                                            7%
                                     O^
            WH7
li
           MS)
                               31
                               7?
                                                7J
                                                  79
       ^
     X
                                                                         SI
                   MM

                                   ,31
       5"
                                                 76
                                            n
                                                                     35L
                   ^a.s
                                           -77
                                                        5T,
                                                             J8-Q
                   SZZ
                                    is
                                    1/7
                              Jt_
                              _ZL
                                                             I
     ;6Q6   TpT3i3
                                         J/6
                                            X,
     CONSOLE #
     FILTER #
                  JST
     AMBIENT TEMP,
                                   PROBE LENGTH    O
                                   LINER MATERIAL_Cja_
     WEATHER
     REMARKS
-------
                  MOISTURE AND IMPINGER CATCH DATA SHEET
impinger
Number Solution Approx, ml

2 Hyck/MzOsL 9^*?

3 HlJ^ /Hz$z 3&2

4 KT 	

5 SiU&J ^pb%j

6


Total Impinger Weight Gain (We) £ / **«• (^? arms
Vf » Final Meter Volume = tt3
Vi a Initial Meter Volume= ft3
s
DGMCF = Dry Gas Meter Correction Factor =
Vm = Metered Gas Volume - (Vf-Vi)(DGMCF) =

Tm as Average Meter Temp. = F+460 = R
r*rn = mctsr rrsssurs luSrcrnctric P rsssurs) —
Weight
Configuration in grams
(UCQ&"~J> Final *17tfii
Initial 4"l5iM
WW)6'S Flnal 'iQl- (
Initial t^\^l
MM>6-£ R"^ 60:^
initial ^£-Ji^
MfiD^'^S Final *4I3,3
Initial USl,^
(MflDu>"^> F|n3' (oT,^(a
Initial |^4-^y
Final
Initial

Analyst

%co
%CO2
- W32
ft3 CONDENSED WATER
FILTER WT. GAIN
PROiE WASH WT. GAIN
in Hn
Weight
Gain y~\ 7* -ST
Weight ,
Gain £/3 , *4
Weight /
Gain <3*(/T
Weigh!
Gain | , 1^™
Weigh!
Gain *7 i r
weight
Gain



%N2
%H2
%CH-
ams
gms
arns

vm (std)
             (17,64)(Vm)(Pm)  (17.64)(	f!3)(	'Hg)
                  Tm                   (	  R)



Vw(std) » Volume of Water Vapor = .Q472(Wc) = -0472(	g) =




                          Vw(std)                	ft3
Bws «• Moisture Fraction =
Vw(std) + Vm(std
                                                       ft3
                                    _tt3
                                    ft3
                                                                     nm*«9n O*w 2/tl
-------
                        SOURCE  SAMPLING FIELD  DATA
PLANT NAME
          rAc«.-Uv

                                                                         Page,
                                                                                .oi
SAMPLING LOCATION
                                      RUN NO-
                                                            TEST DURATION
PTCF,,,	
BAR PRESS	
STATIC PRESS _l£L
                                                         _
                                                         _ft INITIAL LEAK RATE l>        TIME FINISH
OUCTDIMENSIONS    *f 3'   x   ?S> "      DIAMETER			....—, 	
              DGMCF  aiH?£J j. 75 NOZZLE PIA. , / 11   inches     FINAL LEAK RATE /I  OlJa-t-6clm
                   -* Hg
                        H20
                                      OPERATOR
Travers
 Point
        Clock
        Time
              Dry gas meter
               reading ft3
                          •p
                         lnH2O
IHH2O
 Stack
Tamp. F
             Dry gas meter temp
Inlet   Outlet
Hot box
Temp.
Prooe
Temp
  Last
Impipger
Vacuum
 in. Hg
                                                fr
               1*0
                                       JttT
                                                      C~7
                                                            30 /
       1151
                          72
                                                I
                                                7t
       130*
 O
       I3O1
                                31
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                                                74
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                                                      I/
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               j£
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FILTER # 1
                                                      $
                                      PROBE LENGT
                                      LINER MATERIAL  r\
AMBIENT TEMP.	

WEATHER    P. C
                                                     J
                    u
REMARKS
-------
                                  ? !•• , J « V, A c  5
                   ;•.;;		— ~  on nun  	
                  .lirofSTURE-AND 4MP1NGSWJATCHJ2ATA SHEET
                  ••™-     ...               -
impinger
Number Solution App*t». ml 	 Corffigufd
-1-- • >• ' r'V ) T"-'T • --IJ5- siJuO ; M*t>(y
' ! :
'1 1 A ^f* >I 1 i IK "*"^ rf-v «N 1 _• .t
«£ 1 1 »v»"fr f n/.(_;-t_ ' ij*&f nopw „

i i
	 - !
"' • • i j rf" 	 . . 	 — ' ~" "" /* „„£
^ Ml > , " IMBDL? -
'- - • - - • . • --, , _J_
. ; i
-- 5 ^lUttt.GM j3€0(Cf) 1 ^HoHC^""-^
, • - . .' ) ;
; 	 I 1
6 .: . . F - -, . . ._._

'"—-.-_
Weight
IterK1 in grams
S> . ,..lfma\ ~1$3)\
""TniUal it^fl.V

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Initial IffCt^O

Initial J/f^ 2^
Flnai ifS^l
Initial £|^HL
-------
APPENDIX A.2




  PM10/CPM
-------

PLANT/'*" ^'^^ *^C
DAIE f-ZV
---


SAMPLING LOCATION J/X?t »S

TRAVERSE
POINT
NUMBER
£ /
2
3
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1
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-------
rp» /nii
-------
                        SOURCE SAMPLING  FIELD DATA
PLANT NAME.
                                                                                  ol.
SAMPLING LOCATION Sr^M^
DATE TIME START
DUCT DIMENSIONS X
PTCF nnMCF
BAR PRESS • Hq
STATIC PRESS • H2O
RUN NO PMlO- 1
-•} (_|-jj 'TJU&FINISH.
DIAMETER
NOZZLE DIA Inches
^E^P n, ORRBAJPftc-

^.JIST DURATION
iHlNlfftAL LEAK RATE
RNAL LEAK RATE

mln.
clm
> elm

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Point
































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Time
































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reading M3
































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inH2O
I
































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FILTER «
AMBIENT TEMP.

WEATHER
                                       PROBE LENGTH _
                                       LINER MATERIAL,
REMARKS
-------
                  MOISTURE AND IMPINGER CATCH DATA SHEET
impinger
Number
1
2
3
4
5
6
Total Impii
Vf o Final
Vt = Initial
DGMCF =
Solution Approx. ml
M WiL JCO
Ql M.J.O !oO
HT •—
S,U.G,i XXto



•* / rs /
nger Weight Gain (We) fH&tp grms
Meter Volume a ^ tt3
Meter Volumes fi3
Dry Gas Meter Correction Factor =
Vm * Metered Gas Volume = (Vf-VMDGMCF) =
Tm = Aver
Om • fcjah
ape Meter Temp. = F+460 s R
=r prgeeyro fRarrtmatrir! PrA^.mirfl^ =
weight
Configuration in grams
BvV0bG?~:> Final iT\,lL
Initial tO~t^
Pip |i G?"~-* Final *0\S*i\
initial (^'5^,3'
mQlfl^irS Final tffyieL?
Initial ^vifS,"]
JHOJp t?~lS Final C?SZfl.O
Initial tS!'^!
Final
Initial
Final
initial

Analvst N/ i-i—

%C02

tt3 CONDENSED WATER
FILTER WT. GAIN
PROBE WASH WT. GAIN _
in. Ho
Weight _-
Gain (31. l
Weight ..
Gain \\i\
Weight
Gain OnO
Weight . .
Gain 4, 1
Weight
Gain
Weight
Gain

%N2
%H2
%CH
gms
	 gms
gms

Vm (std) i
             (17.64)(Vm)(Pm) (17.64)(	ft3)(	BHg)
                  Tm                    (	 R)




Vw(std) = Volume of Water Vapor = .0472(Wc) = .0472<	g) =




                         Vw(std)                	tt3
Bws = Moisture Fraction =
Vw(std) + Vm(std
                                             ft3
                                                      ft3 =
                                                             ft3
                                                             ft3
                                                                      iiion Om W
-------
                         SOURCE SAMPLING  FIELD DATA
PLANT'NAME r IftrUvi     ?-•
SAMPLING LOCATION^
DATE  l-iS-W  TIME START -VOZ-S'
  DUCT DIMENSIONS	
7 PTCFJ^J    DGMCF,
                                       RUN NO..
                                       TIME FINISH
                                       DIAMETEFI _
                                NOZZLE
BAR PRESS   oHj
STATIC PRESS __U
                        H2O
                                         OPERATOR
                                                                          Page.
                                                                                   .01
                                                              TEST DURATION.
                                                          .ft INITIAL LEAK RATE ,
                                                            FINAL LEAK RATE _
                                                   _min.

                                                   _cfm
Travers
 Point
          Time
              Dry gas meter
               reading R3
                           •p
                         InHZO
lnH2O
 Stack
T«mp. F
                                                Dry gas meter temp
Inlet   Outlet
Hoi box
Temp.
                                   Pfeee
  Last
Impinger
Vacuum
 In. Hg
/r  '
        &
      (71
                                                        63
                                       7/f
? *
                                    ft
      £L
                         L3=-
                                  t<
                                          y
                                                                           (, 0
Qj_
 I
                                                            Zf Z
                  6 7
                                   fl
                                       32J
               -If- ff
                                         322.
                                                                    f/
                                                                           ff
      H)
                           /•z
                                       32.5
                                                                     tr
                                                                           r/
               73-^
                                         32.2
                                                                           .T2-
      tfof
                                                        6?
                                                                     'f
      Ik?
                                                  72-
        £Z£_
                         LL
                                               22.
                                                     6 7
                         j.of.
                                  ll
                                                        44
                                                            3/0
                                                                     /f
               -77 -?r
                                 If
                                                 .22.
                                                            !££.
                                                                     / 1
                                  /f
                                                  7Z
                                                            3/4
                                                                    /v
                                                      67
                                                               Jfi
                   12
                                  /t
                                         7/3
                                                             311
                                                                     /f
                 i. Wo
                                                               3/V
                                                                    ff
        ZiZ.
                         .Jl^
                                                75
                                                             70f
                                       306
                                                                     1 1
                                                                            &L
       Zf
                         .-33
                                                               Jo?
                                  ff
                                                                            60
                                       PROBE LENGTH	£.
                                         LINER MATERIAL.
                                                                                 C - -;
WEATHER
REMARKS
                                                         ^^
-------
                                  MOISTURE AND IMP1NQEH CATCH DATA SHEET
implnger
Number
               Solution
                 hT

              6l\\LtLJJ>t
                                  Approx, ml
                                  loo
Configuration
Weight
in grams
                                                                 Final
                                                                 initial
                                                                 Final    (oil
                                                                Final
                                                                Initial

                                                                Final	
                                                                Initial   "]W.
                                                                 Final
                                                                 Initial

                                                                 Final
                                                                 Initial
                                                                                      Weight
                                                                                      Gain

                                                                                      Weight
                                                                                      Gain

                                                                                      Weight
                                                                                      Gain

                                                                                      Weight
                                                                                      Gain

                                                                                      Weight
                                                                                      Gain

                                                                                      Weight
                                                                                      Gain
                                                                                                   .7
Total Impinger Weight Gain (Wc)_

VI a Final Meter Volume =	
                                     >grms
                                    ft3
Vi a Initial Meter Volume=
                                ft3
OGMCF => Dry Gas Meter Correction Factor
Pm a Meter Pressure (Barometric Pressure)
                                                         Analyst.
Vm - Metered Gas Volume = (VI-VI)(DGMCF) = •.  •      H3.

Tm = Average Meter Temp, = F+460 =     '    R
                                                in1, rig
                                                                 %O2
                                                                 CONDENSED WAJER
                                                                 FILTER WT. GAIN  	
                                                                 PROBE WASH WT, GAIN,
                                                                                      %CH
                                                                                         _gms
                                                                                            -flilS
               Vm (std) -
                             (17,64)(Vm)(Pm)  (17.64)(
                                  Tm
                                                                 'Hg)
                                                                R)
               Vw(std) = Volume cf Wa'.sr Vapor = .CM72(Yyc} = -0472' _ g)
                                          Vw(std)
                                                                     113
               Bws • Moisture Fraction =
                                          Vw(std) + Vm(std
                                                               tt3
                                                                        f!3 =
                                                                                tt3
                                                                               ft3
-------
                         SOURCE  SAMPLING  FIELD  DATA
PLANT NAME.
                                                                           Page;
                                                                                   .ol.
SAMPLING
DATE 4--
              TIME START
DUCT DIMENSIONS          X
PTCF  'W      DQMCF /-ffrtl,
BAR PRESS	
STATIC PRESS _i£J
           NO  pyuio-3
       TIME FINISH    _      TEST DURATION	
       DIAMETER  W-y*y  '   ft INITIAL LEAK RATE &
                                                                                       min,
NOZZLE DIA.
                                                    inch as
                                                              FINAL LEAK RATE
                                                                                       ctm
                   .'HO
                         H2O
                                        OPERATOR
Travers
 Point
               Dry gaa meter
                reading ft 3
                          lnH2O
                                   -H
                                 lnH2O
         Slack
       Temp.. F
                                               Dry gas mater temp
Inlet
Outlet
Hot box
Temp.
Probe
Temp
  Last
Impinger
Vacuum
 in..Hg
                                   it
                                                 7?
                                                              2* '7
                                                                       tf
               ti-
                                                 73
                                                             2.1/
               92- 7 J
                                   ft
                                                 •73
                                                                       ff
                                                                             GO
      hi
               f ?-.
                                   ft
                                        3/Z-
                                      f f
                                                                       If
                                   'f
                                                              zrf
                                  tr
                                  tf
                                        1/6
                                   ft
                                                       67
                          t'f
                                   rt
                          L-L
                                   K
                                                 75-
                                                                       /I
                                                        7V
       Z£Z_
                                                                       'f
      ^L
                                                                       f f
                                   tt
                                                 72.
               /
-------
                                 MOISTURE AND IMPINQER CATCH DATA SHEET
impinger
Number
   Solution
Approx. ml
Conliguralion
in grains
i Dl> Hz-O j£O
D£H^> ioo
"a MT
4 5cli£fc.L8£l f^&l) ft]
s
• i

Total Impinger Weight Gain (We) 1 S S. o 6 grms
Vf = Final Mater Volume o fl3
Vi • Initial Meter Vo!ume= : ft3
DGMCF B Dry Gas Meter Correction Factor =
Vm = Metered Gas Volume « (Vf-Vi)(DGMCF) = ' . •
Tm B Average Meter tamp. = F+460 = R
Pm a Meter Pressure (Barometric Pressure) = 	
m^pfc»"-> Final /^?' 7
initial fj~7s,#
I^0|)6>'^ Final $"?/• *•/
Initial SSS..^
fVWD^S Final tf9&,j
Initial Lfflij^'
IMfitJcJ"^ Final <£> S" ? 6
Initial ^9$3j(0
Final
Initial
Final
Initial

Analyst

%CO2
%O2
tt3 CONDENSED WATER
FILTER WT. GAIN
PROBE WASH WT. GAIN
_ in. Hg
Weight
Gain
Weight
Gain
Weight
Gain
Weight
Gain
Weight
Gain
weight
Gain
%N2

%CH

gms


Hb.T
' S.5
\.(o
H.o
ffc£ °





gms
.gms

,   Vm fstd)
                             (17,64)(Vm)(Pm)  (17.64)t
                                                              R)
               Bws = Moisture Fraction
                                         VwfstdU Vmfstd      ft3
                                                                              tt3
               Vw(std) o volume of water Vapor = .0472(Wc) • .0472^	y)

                                         Vw{s!d)       -          .  -ft3
                                                         ,ft3
-------
APPENDIX A.3




 ALDEHYDES
-------
                         SOURCE SAMPLING  FIELD  DATA
PLANT NAME
           Mo. I" l\
                     f

  SAMPLING LOCATION 5 Till \L
DATE
               . TIME START.
  DUCT DIMENSIONS    *f ^   X  "W
/ PTCF l-0d^9.   DGMCF  /. f 3       NOZZLE DIA, . J-*U
                                       RUN NO.
                                       TIME FINISH
                                       DIAMETER
BAR PRESS
STATIC PRESS
                    * Hg
                 . 7    H2O
                                                                          Page.
                                                                                 .of,
                                                            TEST DURATION  ^ j
                                                                                     min.
                                                   inches
                                                           ft INITIAL LEAK RATE  >
                                                            FINAL LEAK RATE .
                                                                                
-------
impinger
                  MOISTURE AND IMPINQER CATCH DATA SHEET
                                               Weight
Number
1
2
3
4
5
6
Total Impinger
Vf o Final Meu
Vi = Initial Meti
DGMCF = Dry
Vm = Metered
Tm « Average
Solution Approx. ml
BNPH 3too
DMPU 2®o
Kf —
^^l ^^



Weight Gain (We) V5 1« 5~ grms
jr Volume = ft3
ar Volume- ft3
Gas Meter Correction Factor =
Gas Volume - (Vf-Vi)(DGMCF) -
Meter Temp. = F+460 = R

Configuration in grams
*Hcc C3~!> Final o 3>(f£"~~
Inllial t'SjTil^
tG"^? Final ^3^2-
Initial Cs32..O
,^-S Final 4/73?
Initial U13 "I
WJDv7""-^ Final C^a i* f
Initial 4?SC»r7
Final
Initial
Final
Initial

Analyst
%co 	
%C02
'%O2
ft3 CONDENSED WATER
FILTER WT. GAIN
PROBE WASH WT. GAIN
in Mn
Weight . ^
Gain (ifl, I
Weight
Gain IO»-'2-
Welght
Gain • '« •^—
Weight
Gain /« 2-
Weight
Gain
•Weight
Gain

%N2
%H2
%C!_.
	 fms
	 gms
qms

             (17.64)(Vm)(Pm) (17.64)( _ ft3)(
               Vm (std) =
                                                               Hg)
                                 Tm                   (	  R)




               Vw(std) = Volume of Water Vapor = .0472(Wc) = .0472(	g) =




                                        Vw(std)                	ft3
Bws a Moisture Fraction =
Vw(std) + Vm(std
                                             ft3
                                                                     fl3 =
                                                              H3
                                                             ft3
-------
SOURCE SAMPLING FIELD DATA
PLANT t
iAMEMa-V-Kul^^
SAMPLING LOCATION S "rCtf Ic
DATE'/' 21
DUCT DIMENSION;
TIME START
5 v/" x 75"'
Q^tyfefr /,f2.
RUN NO.


A\ALUioi-2,
TIME FINISH '
DIAMETER ft
NOZ2LE DIA. <-2/ 7 inches
Page_l
TEST DURATION
o. f
min.

INITIAL LEAK RATE £> O/JUf dfm'fj
FINAL LEAK RATE rt VCl* S*>f" cfm
BAR PRESS 2 ? "Z-V • Hfl /L
STATIC PRESS • H2O

Travers
Point
	
£ '
I
1
V
(,"
	
/? /
1
/
H
f
	 	
r '
2
7
i
s
_
^ /
f.
j
k
>






CONSOl
FILTER
AMBIEN
WEATHI

Clock
Tim©
/ v y£
?k' i-
f/
f !•>'
>~fe
f!r.r
' r?
/6 <>/•>"
Cf
oc ,.)-
C'l
Jd II. f

Zy.i'l
32
?y.»'
3T
if.V
/4 4*^*
{(>//<&&
A&p
'








Dry gas meter
reading fl3
/^ 6 fy
tl.O
/ 3- "i
11 f
/6 2_
/ 7- 3"
/ 7. >"
/^•f
2.4 •>
2_j , ?
7-3. 1
2y, 7
n
2.6- °
2.7 /
2>V-~t
36- 1
-3/5'
3/- $~
32,090
A~*&*&+*
/








pa 4/-? y
»
TTEMP, &&
:R

*P
inH2O
— -
» 'I
- f T
^'









OPERATOR & ^

Stack
Temp. F

?2,1
3 / Cj
?/ >"
"7 /' fjf
3 12.


~33-6
72-/
2 2.^_
•j zr
5/^


72.2
52-2.
?z^
"£2-&
*)/&

?sr
>v .










Dry gas meter tamp
Inlet

76
-7$
# f
9 J
vy


$"i>
%i~
$*!
% d>
?&


?y
&?
¥s~

v&










Outlet

7y
7 f
76
76
7£


76
76
7 7
7 7
7 7


7f
7#
7'
"^ (Sir
*"7 ^^~

/^ /^










Hat box
Temp,

2-13
2.?1
^_&sJ?
*3f /^4/
2S^


2-ffV
T^fo
2-go
2 7%
Zr/


£70-
2-f^
5 £?¥ *"
*7 M ^
2*1}

I.??











Probe
Temp

































Last
Impinger

^ 'L
5V
50
V?
i" /


y ?
$~ ^
3"~ 3


5~&
¥*t
fc
$~<3
y£

ry










Vacuum
in. Hg

?_
7_
i
•^_
7_


z.
2.
2.
2_
Z.


"Z^
i*.
2-
2_
7

Z-











	 .
































/
PROBE LENGTH £
LINER MATERIAL ^ £/r/y




REMARKS
-------
                                MOISTURE AND IMPINGER CATCH DATA SHEET
impinger Weight
Number Solution Approx. ml Configuration in grams
1 OKJPI4 ^.^^ faopt5 "3 Final ~7fa(e,¥
Initial (s"i 1~* 2-
2 DM? H dO^ t (p~~> Final \0wO^"\
Initial (Q$ #, j~
3 $AT 	 KHCfc&'S Final V^f.7
Initial ^ 75". 5.
-------
                            SOURCE  SAMPLING FIELD  DATA
  PLANT     _____

           ^^71  t
  SAMPLING LOCATION > TUL lC
  DATE  /'^H-ll TIME START
  DUCT DIMENSIONS   HI"   X
T PTCF J. <3£3pt  DGMCF _L__L_
  BAR PRESS  J f? / H-_
  STATIC PRESS  - f). £
                               J? f "
                              RUN NO.
                              TIME FINISH
                              DIAMETER
                                                               Page
                                                                                  of .
                                                          -3
                                                             TEST DURATION
                                  NOZZLE DIA.
                                 	tl INITIAL LEAK RATE Q.OJL 1+fi
                                 .Inches    FINAL LEAK RATE 0-^iehf^6'c
                      _'Hg
                           H2O
                              OPERATOR
                                4
    Travers
     Point
 Clock
 Time
               Dry gas mater
                reading tt3
           *p
         lnH2O
 -H
lnH2O
 Stack
Temp. F
Dry gas meter temp
  Intel
Outlet
Hot box
Temp.
Probe
Temp
  Last
Implnger
Vacuum
 in. Hg
                   Yl/75
                             O2.
                         ±5-
                                       31O-
                                    y.j

           §3-5
                  .IS'
                                        J/S)
                                          JCJ /
       £
                                                     o±
«. *-
~3HL
                                          7/fr
                     52.
                                                   JOO
                                                                         5O
                                                              3£1
                                    .7L
        ^J_
                                    • S3
                                                     51
                         Jl_
                                                        S'S?
          M.
          122.
   T
                                          J-?/
           VI
$LZ_
                                                                -TO
W
                                    7ft
                                      at
                     jf
       ^t-3
                                                                           JT3
                    5-2
                                      It
                   .SL2L
     .41
           . s-
                          ,57
                               7A
                                        J3L
                   ^4
       3
                J2L
         ^3_
                                                                -TO
           15*
    CONSOLE #.
    FILTER » __
                              PROBE LENGTH _
                              LINER MATERIAL.
    AMBIENT TEMP. _ J23L
                                                    Jto-
    WEATHER   OJf/ras-t /Or,
    REMARKS
-------
                 MOISTURE AKlD IMPINGER CATCH DATA SHEET
Impinger
Number Solution Approx. ml
2 t>MPl4 3^3
MT ^
4 Si 1 i£&,6ei <7@%)&i
5
6

Total Impinger Weight Gain (We) 2 o i. ,  Metered Gas Volume = (Vt-Vi)(DGMCF) =
Tm o Average Meter Temp. = F+4SO = R
Pm = Meter Pressure (Barometric Pressure) =
Weight
Configuration in grams
Initial l0CJtJ.*-i
(d~£ - . ~lti -*J
HpO&~2> Final fJl. /
initial Ijflb.n
frffD&'-'S Final ^-77,7
Initial 4W»V
|Mfip ^—S Final 7 "?^1
initial 74?j^
Final
Initial
Final
Initial

Analyst
%CO
%CO2
%O2
ft3 CONDENSED WATER
FILTER WT. GAIN
PROBE WASH WT. GAIN
in, Hg
Weight
Gain
Weight
Gain
Weight
Gain
Weight
Gain
Weight
Gain
Weight
Gain
%N2
%H2
%CH

ams



35,7
3,%
'I3o






gms
_gms

Vm
                                      _t!3)(	«Hg)
                 Tm                   (	 R)




Vw(std) • Voiume of Water Vapor = .G472(Wc) = .S472(	g) =




                         Vw(std)                	ft3
Bws = Moisture Fraction
Vw(std) + Vm(std _ H3
                                                     ft3
                                   ft3
                                  fl3
-------
\
SOURCE SAMPLING. FIELD DATA
flA * i 1 if I/
PLANT NAME |Vy2-rKUf ^ JLLs?
SAMPLING LOCAT1
DATE '7-35-^1
DUCT DIMENSION!
PTCF IpOOL
ON *?S-W*<_JC
TIME START
? ?£" X L|-j"
DGMCF /• /S
RUN NO.
TIME FIN
DIAMETE
NOZZLE DIA. .
AlA* k^4^ 4
SH
R J^5 ft
Incnas
i^m* -1
W
^^WL^iX^
Page ol

TEST DURATION
min.

INITIAL LEAK RATE# OOf ^ 9'cffli
FINAL LEAK RATE ^ /^ i> i " IfSl
BAR PRESS p?c;.f:> 'Ha 	 ^
STATIC
Travers
Point

£ '
_'
—
,H
^
_£W
Dj
3
3
H
C"
ST) r
iT'
Jr
"7
'-f
c-
•%${/
f- 1
9
3
u.
I
^
^'7
,4!
2
••£
u
r
CONSCM
FILTER
AMBIEN
WEATHI

PRESS • H20

Clock
Time
//44 .
11% 5
<;>j€?
if 1 -j-
•'•Ti
i U" <•'
1/1, — '
/d?O ->
£ux- *>
rfb5
/•&7S "
Pio
\3\3 5~
jfflH
)«? ii/. S
/«'.^
«?„?), s
tf;^
/P-t- S"
]<3%
Ml $

3^-S
WtfH
^'i'f.T
/^-'!i
Dry gas met ef
reading H3
H- 55
/
'|
"
'33, 6> f
33,7

' JH, 1
3^^' •* 7
e# /I/. ^\2
9
TTFMP /,/)
ER

!nH2O

j_S^
,^'
,S'^
,1^
;i"i

'S
1 1^
41
•f7
, f 2

7?G
.76
»7i
.^R
, so

,J5
• S"/
- r*
,5V
£j JU
, ^3
,aa
,ff


.*/_r
•4-"^
'.^^
,TD
1 , ^(?

,^j
'.3*?
• ^
, i^V
.«

,30

• ^
. Pf .
.AC

_^& ••
• *3.
.Jg
./">
, ItJ-

Stack
Temp. F

7.2 C
3/^
3m
.-?,m
^i"7?

3p3
726'
J-3 s
3-? 9
3^5"

~jfeS
3^^!
3^O
,3^0
3-|q

3/7
3^
J/l
J/


J^^
3>^
3GLs
^^
3o 3

Dry gas meter temp
inlet

•70
~1 J
7"
7M
-,-v

71
1~i
7?
7^
7?

"^3
7*4
73
/ *^k
71 .

~7 /
• 73.
71
7 ' -
70

12
73

'73

Outlet

(*%
iec\
7p
7S)
"?()

71
-] \
7
11
•7 i
t
7J
L72
-7^
7(


L 7/
?/
7£>
' 7C
7/J

7 ^
"7 >,
"!c^
~l(
ia
Hoi box
Temp.

3.2O
jt'Z.'j.


.-Pxt)
ffl^g"/
5?6
^^(^
*P S 7

J7^f
^7,5,
P~°7 /-/
/ /
f77~7
^75"

^7^?
>?V£
^r f j
i^9-------
                  MOISTURE AND IMPINGER CATCH DATA SHEET
mplnger
Number Solution Appro*, ml
i DKiPl4 9-&o
t>MPH 9*o '
,3 PIT 	
4 'Silitic^' ^S&ZTeJ
5 " • ,
6

Total Impinqer Weight Gain (We) 1 ^ '* • « grms
VI o Final Meter Volume = tt3
Vi = Initial Meter Volume* ft3
DGMCF = Dry Gas mdt@f Correction Factor -
Vm = Metered Gas Volume - (Vf-Vi)(DGMCF) -
Tm = Average Meter Temp. - F+460 - R
Pm = Meter Pressure (Barometric Pressure) =
Weight
Configuration In grams
Wdjp t? Final a^7^,"/
Initial f/ft&Q ' •
G-$ ' Final fB.5"
Initial M^l, p
f -< ^. , '-'tyt/1?
IHOD t? O Final i 7 Y>
Initial ^J2J
|flt«t)6r"^ Final 7¥?'f
Initial "J*4(' (f
Final
Initial
Final
Initial
*
Anaiysl
-------
APPENDIX A.4




    PAH
-------
                       SOURCE SAMPLING  FIELD DATA
PLANT NAME.
SAMPLING LOCATION
                   f^
                                                                       Page_/	o(.
  DATE f*8'9l    TIME START £*g JO
  DUCT DIMENSIONS   *f3"^   X   j*g
f PTCF.
                                     RUN NO. PAH-I
                                     TIME FINISH	 TEST DURATION	' "^'    min-
                                     DIAMETER	
                              NOZZLE DIA.
                                                inches
                               _lt INITIAL LEAK RATE _.
                                 FINAL LEAK RATE
                                                                               fefm
  BAR PRESS	* Hg
  STATIC PRESS   "". tl
                       H2O
                                     OPERATOR
                                                                  » «<
Travels
 Potm
       Clock
       Time
               Dry gas mater
                reading H3
 •p
inH20
                              "H
                             inH2O
 Stack
Temp. F
Dry gas meter temp
  Inlet
Outlet
Hot box
Tamo.
Probe
Temp
  Last
Impinger
Vacuum
 in, Hg
 ,\
                                      721
                                               SI
                                                    $0
                        ^11
                                                    JT2.
                                      31?
 <
                                                    5*1
               '30-
                                                    7*
                                                   ,5-6
                                                                       ^
                                                    4-
                                V 5
                V?
                                      33A
\
       /CCS
               5/A
                                                                         vv
                                                            f
               S3.0S"!

                                                                                    ro

                        .is   Mo
                                                   41
                                                                         r/
                  TL
  ±
                 M
                                                    (,
CONSOLE*.
FILTER #	
           /I'
                                      PROBE LENGTH,
                                      LINER MATERIAL,
AMBIENT TEMP.,
                                                   «J<«*>
WEATHER
REMARKS fa z m.Qj]
         Xi£.
                       <*i*~ '9il
-------
impinger
                                MOISTURE AND IMPINGER CATCH DATA SHEET
                      Weight
Number Solution Approx, ml
M.T .—
2 HPLC $*£ foo
3 MPLCtUo loo
4 MT —
S SiU£aleM '~e?0C("5> ^'na' ^ ^*°- 7
InUlal^^g'Ifai., |_4^/ 7a g
Final
Initial

Analyst
%CO

• %O2
ft3 CONDENSED WATER
FILTER WT. GAIN
PROBE WASH WT. GAIN
•n. Hg
Weight
Gain 3 JO. 2.
Weight
Gain 
Gai,/ 3H 7
^

%H2
%CH
pms
	 gms
cms

                            (17.64)(Vm)(Pm)  (17.64)(	n3)(	*Hg)
               Vm (std) =
                                    f!3
                                 Tm                   (	R)



               Vw(std) = Volume of Water Vapor = 0472(Wc) = .Q472f	^g) =
                                   Jt3
                                        Vw(std)
                          Jt3
               Bws = Moisture Fraction
Vw(std) -t- Vm(std __ _ ft3
                                                                     f!3 =
-------
PLANT NAME
                       SOURCE  SAMPLING FIELD  DATA

                    *26,	
                                                         Page.
                                                                              ol
SAMPLING LOCATION
DATE ?-JVff  TIME START	
DUCT DIMENSIONS    H3 "   X
PTCF M15   DGMCF^
BAH PRESS	' Hg
                        RUN NO
                        TIME FINISH.
                        DIAMETER _
                                           .PAH-Z
                                                         TEST DURATION,
                                                          !",,
                                                        ft INITIAL LEAK RATE  l.A/CUteff '
STATIC PRESS  ~C< ll    ' H2O
                 NOZ2LE DIA. .hi    inches     FINAL LEAK RATE
                                   &e
                                     OPERATOR
                                                                                    4 33li
Travers
 Point
        Clock
        Time
Dry gas meter
 reading ft3
 •P
lnH2O
 -H
lnH2O
 Stack
Temp. F
Dry gas meter temp
  Inlet
Outlet
Hot box
Temp,
Probe
Temp
  Last
Impinger
Vacuum
 in. Hg
                                .11,

       N/o
                                                                        o
                70,
                                                    70
                                                          na
                                                             5"-?
                                                    7/0
               71.1
                                              1
                                      M-
                                                    71
                                                                        Hi
   3
                                              n
       Ml
                                              1
                   ,  /
                                21
                                                                        s
                 K. r »
                         '11
                                                          J~c\
                                                                       JO
  s
               f ^
                                      3/1
                                                     72
                                52
                                       1-20
                                       n
                                                             a
                                              71
                        ,6*
                                                                        T3
              101.*
                                             7$^
                                      7S
                 , \
                                             ^76
              JOV. (,
                %
                        M2.
                        M£
                                                    7S
                                      J/o
                                                    74
                                                                       a
CONSOLEi
FILTER #_
              -33
                                     PROBE LENGTH _
                                     LINER MATERIAL,
AMBIENT TEMP,
WEATHER
REMARKS
-------
                                  MOISTURE AND IMPINGEH CATCH DATA SHEET
impinger
Number
               Solution
               4Fl£
                  M|
Approx. ml
Configuration
Weight
in grams
                                                                 Final
                                                                 initial   <4S7.*|
                                  loo
                                   10
                               Initial

                               Final
                               Initial

                               Final
                               Initial

                               Final
                               Initial

                               Final
                               Initial
                                                                                      Weight
                                                                                      Gain
                                     Gain

                                     Weight
                                     Gain

                                     Weight
                                     Gain

                                     weight
                                     Gain

                                     Weight
                                     Gain
                                                                                                  .
                                                                                             ~~(i,\
Total Impinger Weight Gain (Wc)5'» \.

Vf = Final Meier Volume =	
                                     _grms
                       Analyst.
                                    ft3
Vi = Initial Meter Volume=
                                tt3
DGMCF = Dry Gas Meter Correction Factor =
                               %CO2,
                               %O2_
Vm = Metered Gas Volume = (Vf-Vi)(DGMCF) =	

Tm = Average Meter Temp. = F+460 «	R
Pin = Meief PfwssUnB {nil GI i is tr ic Pressure) =
                               CONDENSED WATER  .
                               FILTER WT. GAIN   	
                               PROBE WASH WT. GAIN.
                                                                                       %CH
                                                                                            _gms
                                                                                         _gms
                                                                                             grns
               Vm (std)
                             (17.64)(Vm)(Pm) (17,64)(	ft3)(	'Hg)
                                          Vw(std) •»• Vm(std  	ft3
                                                                        03 =
                                                                                f!3
                                  Tm                    (	  R)   '

               Vw(std) = Volume of Water Vapor = ,0472(Wn) = .0472(	g) =	ft3

                                          Vw(std)                 	ft3
               Bws = Moisture Fraction =	.	=	
                                                                                       Rwicion Dan 2/V1
-------
PLANT NAM
                       U
          SOURCE  SAMPLING  FIELD DATA

      *34,	
                                                                             Page,
SAMPLING LOCATION
      Cl M-
                   TIME START
DUCT DIMENSIONS H.3'
PTCF
                             X ____ 1 •>'
                       RUN NO
                       TIME FINISH.
                       DIAMETER _
                                                   1 nH "  3
                                             TEST DURATION
                   DGMCF
                                   	ft INITIAL LEAK RATE
                 NOZZLE DIA.    !ci (    inches     FINAL LEAK RATE _
      BAR PRESS  ,-W- a      Hg
      STATIC PRESS  "C .?'#    ' H2O
                                      OPERATOR
                                                                               .of
                                                                     H»
                                                                   ctm
      Travers
       Point
       Clock
       Time
Dry gas meter
 reading H3
           •p
          inH2O
lnH2O
 Stack
Tamp. F
             Dry gas meter temp
Inlet
Outlet
Hot box
Temp,
Probe
Temp
 Last
Impinger
Vacuum
 in. Hg
             IM
                                                                                0?
                                                     7
                              .73
                                36
                                        7O
                                                           7/
            fln
JJ.
                                                                          J3

                                                                        rz
             lie

                                                    76
                                                     73
             Mil
               P/
                                7C
                                                           rv
                                                ^
,317.5
        3
       /J/7
       *
                                                                                      JTL
                    •S-S'G
                                 n
                                7S
                                                           $-3
                                                       67
                              ,4
                       n
      C
                                              76
                                        7V
                                                          S'S
        «a
                                      37
                                               1
                                        71
                                                    76
             /
-------
                  MOISTURE AND IMPINGER CATCH DATA SHEET
impinger
Number Solution Approx. ml
mr —

2 UPLL m° (co

3 UPLCWeD I0o

MT —

5 ^»itau£»t( tf&bfar}
V
6


Total Impinger Weight Gain (We) «5o^A qrms
Vf = Final Meter Volume = ft3
Vi = Initial Meter Volume= ft3

DGMCF - Dry Gas Meter Correction Factor =
Vm = Metered Gas Volume = (V(-Vi)(DGMCF) =

Tm • Average Meter Temp. = F+460 = R

r^II — mtJlBI r~IB%SUIC! 1 DdiuiliainC rioooLMu) —
Weight
Configuration in grams
Initial 457. S""
m^^ Final SJ33
initial ^wS.1^/
jvuj^)fe^ii Final 5y?S»|
Initial S"GG,J
Mob^1"^ Final *f7^S~
Initial ^7^1 '2-
r^Ot) 6"^ Final 'To^i'1
Initial [DOi^
Final
Initial

Analyst

%CO
%C02
" %0z
tt3 CONDENSED WATER
FILTER WT. GAIN
PROBE WASH WT, GAIN _

!f!. He
Weight _
Gain jlici2—
Weight
Gain ~^), [
Weight
Gain 0, "2—
Weight
Gain 6*^*
Weight ^ ,N
Gain D/6
Weight
Gain



%N2
TOrlt
^^D^*n
- • Q^ns
§ms
ams


Vm (std) =
             (17.64)(Vm){Pm)  (17.64)(	tt3){	• Hg)
                  Tm                    (	 R)

       = Volume of Water Vapor = .0472(Wc) = .0472(	g) =

                         Vw(std)                	ft3
Bws = Moisture Fraction =	=	
                         Vw(std) + Vm(std  _ tt3
                                                       tt3 =
                                                             _ft3
                                                             .03
                                                                     H»v»lofi Dou 2TB1
-------
    APPENDIX B




PROCESS DATA SHEETS
-------
                  .JJ
                  tL-ff'k'
tMllifi
                BuilMf
                  2
                          TFH
         fPM
                                                Gwnwn
                                                        Cw
                                                                                          to
                                                                                                ttantafily
                                                                                                    12
                                                                                                         OfiO»-v>
               il
                                      JLii.
                                                                                                          II
                                   OZ
                iOA
gSO
l&iJ
                                                                                       Go
         a^a
H
                                                                       D,
                                                                                                           M
               I2!fcJ
                                                                l£
                                     1-6,0
                                                                                                           U
                                113
                                  C
                                IL'1
                                           •if"?
                                                 Jo
                                    -111,
                               ha.
                                                                                                    M
Lie? ?
                                 Ml/
-------
                               - 4-
                             5, 
                                                                   -SzA^2
            2

          F»*IUHi
                                                   CwrMnt
                                                         T-mp


                                                          PF
                                         CM
                                                                           MMuriSavbtw

                                                                                             10
                                                                                                   ttemteily
                                                                                                              12
                  lea.
                                                                                           1^7,0
                    oo
                                                                        JO.O
                                                                                                              U
                                    ^0_
                                                                  Sfi.
lOCjfl
                                   Zo\
                  joo
Ii31
                                                                                                              U
tt.00
                    00
iLit
                                                COLS
                                                                                      14
                                             n
                                                                        it,7
                                                                                                              v»
                                                                        IP. S"
                                                                                                               •« 1
                                                                                                               41
5 :
                                                    LfitZ
                                               4o^
                                             ^L
                                                                                                               I'
-------
«  -Vll   nt.LDU-4
-------
              APPENDIX C

SAMPLE PARAMETER CALCULATION SHEETS

            C.1   PM/Metals
            C.2   PM10/CPM
            C3   Aldehydes
            C.4   PAH
-------
APPENDIX C.1



 PM/METALS
-------
FACILITY : Mathy #26
DATE:      9-23-91
LOCATION:  STACK
RUN NUMBER:      1.00

SAMPLING PARAMETER    TM
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
Particulate Catch  (g)
                              125.00
                               29.38
                               29.37
                               -0.17
                              326.04
                             1596.00
                               41.83
                                0.33
                               64.68
                              395.60
                                9.22
                               10.33
                               80.45
                             1.00060
                                0.84
                             0.08430
Average Sampling Rate (dscfm)
Standard Metered Volume,Vm(std)
Standard Metered Volume,Vm(std)
Standard Volume Water Vapor,Vw
Standard Volume Water Vapor,Vw
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity,Vs (fpm)
stack Gas Velocity,Vs (mpn)
Volumetric Flow Rate (acfro)
Volumetric Flow Rate (acnun)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
Concentration of Particulate
Concentration of Particulate
Concentration of Particulate
Concentration of Particulate
   (dscf)
   (dscm)
  (scf)
  (scm)
(grains/act)
(g/acm)
(grains/dscf)
(g/dscm)
Concentration of Particulate  (grains/dscf @12% CO2)
    0.33
   41.40
   1.172
   18.65
   0.528
   31.06
   0.689
   29.89
   26.20
 3577.88
 1090.54
39654.84
1123.025
18016.18
 510.218
  102.35
   94.55
   1.146
   18.23
 0.01428
 0.03267
 0.03143
 0.07191
 0.04090
-------
FACILITY : Mathy #26
DATE:      9-23-91
LOCATION:  STACK
RUN NUMBER:      2.00

SAMPLING PARAMETER    TM

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 Heter Temperature  (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration  (%V)
Oxygen Concentration  (%V)
Nitrogen Concentration  (%V)
Dry Gas Meter Factor
Pitot Constant
Particulate Catch  (g)
  125.00
   29.38
   29.37
   -0.17
  323.24
 1596.00
   40.68
    0.33
   75.86
  372.60
    7.55
   10.01
   82.44
 1.00060
    0.84
 0.04350
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 CO2
Concentration of Particulate  (grains/acf)
Concentration of Particulate  (g/acm)
Concentration of Particulate  (grains/dscf)
Concentration of Particulate  (g/dscm)
Concentration of Particulate  (grains/dscf §12% C02)
    0.32
   39.42
   1.116
   17.57
   0.498
   30.83
   0.692
   29.61
   26.03
 3536.56
 1077.94
39196.88
1110.056
17932.35
 507.844
   97.92
   85.04
   1.442
   14.49
 0.00779
 0.01783
 0.01703
 0.03897
 0.02707
-------
FACILITY : Mathy #26
DATE:      9-24-91
LOCATION:  STACK
RUN NUMBER:      3.00

SAMPLING PARAMETER    TM
Total Sampling Tine  (min.)
Corrected Barometric Pressure  (in. Hg)
Absolute Stack Pressure,Ps(in. Hg)
Stack Static Pressure  (in. H2O)
Average Stack Temperature  (cleg. F)
Stack Area (sq.in.)
Metered Volume,Vm  (cu.ft.)
Average Meter Pressure  (in.HZO)
Average Meter Temperature  (deg. F)
Moisture Collected (g)
Carbon Dioxide Concentration  (%V)
Oxygen Concentration  (%V)
Nitrogen Concentration  (%v)
Dry Gas Meter Factor
Pitot Constant
Particulate Catch  (g)
                              123.50
                               29.38
                               29.34
                               -0.58
                              328.52
                             1596.00
                               40.78
                                0.35
                               71.39
                              341.40
                                7.18
                               11.77
                               81.05
                             1.00060
                                0.84
                             0.06110
Average Sampling Rate (dscfra)
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
Concentration of Particulate  (grains/acf)
Concentration of Particulate  (g/acm)
Concentration of Particulate
Concentration of Particulate
(grains/dscf)
(g/dscm)
Concentration of Particulate  (grains/dscf @12% CO2)
    0.32
   39.85
   1.129
   16.10
   0.456
   28.77
   0.712
   29.62
   26.28
 3459.67
 1054.51
38344.71
1085.922
17925.08
 507.638
  100.24
  122.05
   1.272
   16.44
 0.01106
 0.02531
 0.02366
 0.05414
 0.03954
-------
APPENDIX C.2




  PM10/CPM
-------
 FACILITY  :  MATHEY 26
|DATE:       9/24/91
|LOCATION:   STACK
I RUN  NUMBER:     RUN 1
 SAMPLING PARAMETER
PM10
 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.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
                                      64.25
                                      29.38
                                      29.32
                                      -0.80
                                     327.81
                                    1596.00
                                      17.53
                                       0.24
                                      59.16
                                     148.60
                                       7.06
                                      12.01
                                      80.93
                                    0.98750
                                       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 (fpro)
 Stack Gas Velocity,Vs (mpm)
 Volumetric Flow Rate (acfm)
 Volumetric Flow Rate (acmm)
 Volumetric Flow Rate (dscfm)
 Volumetric Flow Rate (dscimm)
 Percent Isokinetic
 Percent Excess Air
 Fuel  Factor,Fo
 Ultimate CO2
                                       0.27
                                      17.30
                                      0.490
                                       7 .01
                                      0.198
                                      28.83
                                      0.712
                                      29 .61
                                      26.26
                                    3872.25
                                    1180.26
                                   42917.42
                                   1215.421
                                   20050.32
                                    567.825
                                      89.07
                                     128.15
                                      1.259
                                      16.60
-------
 FACILITY
            MATHEY 26
| DATE:       9/25/91
| LOCATION:   STACK
I RUN NUMBER :     RUN 2
(SAMPLING PARAMETER
                       PM10
jTotal Sampling Time (rain.)
(Corrected Barometric Pressure (in. Hg)
|Absolute Stack Pressure,Ps(in. Hg)
jStack 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)
jCarbon Dioxide Concentration  (%V)
(Oxygen Concentration (%V)
(Nitrogen Concentration  (%V)
|Dry Gas Meter Factor
 Pitot Constant
                                                             65.10
                                                             20.98
                                                             20.92
                                                             -0.80
                                                            316.82
                                                           1596.00
                                                             20.49
                                                              0.30
                                                             69.02
                                                            185.00
                                                              7.06
                                                             12.01
                                                             80.93
                                                           1.00320
                                                              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 (%VJ
 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 (dscmra)
 Percent Isokinetic
 Percent Excess Air
 Fuel Factor,Fo
 Ultimate CO2
                                                              0.22
                                                             14.40
                                                             0.408
                                                              8.72
                                                             0.247
                                                             37.72
                                                             0.623
                                                             29.61
                                                             25.23
                                                           4895.15
                                                           1492.04
                                                          54254.63
                                                          1536.491
                                                          16048.63
                                                           454.497
                                                             91.42
                                                            128.15
                                                             1.259
                                                             16.60
-------
 FACILITY :  MATHEY 26
I DATE:       9/25/91
I LOGATION:   STACK
IRON NUMBER:     RUN 3
 SAMPLING PARAMETER
PM10
1
| Total Sampling Time (min.)
(corrected Barometric Pressure (in. Hg)
[Absolute Stack Pressure, Ps( in. Hg)
(Stack Static Pressure (in. H2O)
j Average Stack Temperature (deg. F)
[Stack Area (sq.in.)
j Metered Volume, Vm (cu.ft.)
| Average Meter Pressure (in.H2O)
j Average Meter Temperature (deg. F)
(Moisture Collected (g)
j Carbon Dioxide Concentration (%V)
j Oxygen Concentration (%V)
[Nitrogen Concentration (%V)
| Dry Gas Meter Factor
|Pitot Constant
1
70.22
20.98
20.92
-0.80
304 .90
1596. 00
21.83
0.30
70.98
185.00
4.74
10.83
84.43
1.00320
0.84
|Average Sampling Rate (dscfm)
|Standard Metered Volume,Vm(std) (dscf)
jStandard Metered Volume,Vm(std) (dscm)
(Standard Volume Water Vapor,Vw (scf)
(standard Volume Water Vapor,Vw (scm)"
(stack Moisture (%v)
jMole Fraction Dry Stack Gas
|Dry Molecular Weight
(wet Molecular Weight
|Stack Gas Velocity,Vs (fpm)
(stack Gas Velocity,Vs    ALDHDS
|Volumetric Flow Rate (acfm)
 Volumetric Flow Rate (acmm)
 Volumetric Flow Rate (dscfm)
 Volumetric Flow Rate (dscmm)
|Percent Isokinetic
j Percent Excess Air
[Fuel Factor,Fo
(ultimate CO2
i	
           FLOW AND ISO'S CALC'ED
           FROM AVG OF OTHER
           TRAINS

           MTLS/PAH'S AVG
    0.22
   15.29
   0.433
    8.72
   0.247
   36.33
   0.637
   29.19
   25.13
 5249.47
 1600.04
58181.67
1647.705
17869.49
 506.064
   80.80
   94.37
   2.124
    9.84
-------
APPENDIX C.3




ALDEHYDES
-------
FACILITY : Mathy #26
DATE:      9-23-91
LOCATION!   STACK
RUN NUMBER:      1.00
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,Vii  (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
                                                             29.38
                                                             29.37
                                                             -0.17
                                                            310.72
                                                           1596.00
                                                             31.05
                                                              0.81
                                                             71.18
                                                            284.50
                                                              6.83
                                                             12.98
                                                             80.19
                                                           1.00320
                                                              0.84
Average Sampling Rate  (dscfrn)
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
                                                             30.47
                                                             0.863
                                                             13.41
                                                             0.380
                                                             30.57
                                                             0.694
                                                             29.61
                                                             26.06
                                                           3759.20
                                                           1145.80
                                                          41664.46
                                                          1179.937
                                                          19443.32
                                                           550.635
                                                             98.83
                                                            158.17
                                                             1.160
                                                             18.02
-------
FACILITY : Mathy #26
DATE:      9-23-91
LOCATION:  STACK
RUN NUMBER:      2.00
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
                                      38.50
                                      29.22
                                      29.21
                                      -0.17
                                     319.56
                                    1596.00
                                      21.41
                                       1.03
                                      79.87
                                     284.50
                                       8.24
                                      10.30
                                      81.46
                                    1.00320
                                       0.84
Average Sampling Rate  (dscftn)
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  (mpra)
Volumetric Flow Rate  (acfmj
Volumetric Flow Rate  (acmm)
Volumetric Flow Rate  (dscfm)
Volumetric Flow Rate  (dscmm)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
                                       0.53
                                      20.57
                                      0.582
                                      13.41
                                      0.380
                                      39.47
                                      0.605
                                      29.73
                                      25.10
                                    4231.62
                                    1289.80
                                   46900.49
                                   1328.222
                                   18760.40
                                    531.295
                                     112.25
                                      91.79
                                      1.286
                                      16.25
-------
FACILITY :  Mathy #26
DATE:      9-24-91
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 (sg.in.)
Metered Volume,Vra  (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
   29.38
   29.34
   -0.58
  315.36
 1596.00
   29.71
    0.81
   63.14
  202.90
    6.22
   12.93
   80.85
 1.00320
    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 (dscmre)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
    0.47
   29.60
   0.838
    9.57
   0.271
   24.43
   0.756
   29.51
   26.70
 3486.43
 1062.66
38641.30
1094.322
19490.62
 551.974
   95.79
  153.37
   1.281
   16.31
-------
FACILITY : Mathy #26
DATE;      9-25-91
LOCATION:  STACK
RUN NUMBER:      4.00
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  (cleg. F)
Stack Area (sq.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
                                      28.98
                                      28.94
                                      -0.58
                                     316.76
                                    1596.00
                                      21.27
                                       0.36
                                      71.54
                                     176.60
                                       6.43
                                      11.09
                                      82.48
                                    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
                                       0.33
                                      20.50
                                      0.581
                                       8.33
                                      0.236
                                      28.88
                                      0.711
                                      29.47
                                      26.16
                                    3525.45
                                    1074.56
                                   39073.78
                                   1106.569
                                   18260.28
                                    517.131
                                      95.96
                                     103.63
                                      1.526
                                      13.70
-------
APPENDIX C.4




    PAH
-------
FACILITY :  Mathy #26
DATE:      9-23-91
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. 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
                                      29.38
                                      29.37
                                      -0.17
                                     326.04
                                    1596.00
                                      42.08
                                       0.37
                                      60.70
                                     399.70
                                       9.22
                                      10.33
                                      SO.45
                                    0.98750
                                       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 (dscnun)
Percent Isokinetic
Percent Excess Air
Fuel Factor,Fo
Ultimate CO2
                                       0.33
                                      41.42
                                      1.173
                                      18.85
                                      0.534
                                      31.27
                                      0.687
                                      29.89
                                      26.17
                                    3577.70
                                    1090.48
                                   39652.79
                                   1122.967
                                   17960.14
                                    508.631
                                     102.72
                                      94.55
                                      1.146
                                      18.23
-------
FACILITY : Mathy #26
DATE:      9-23-91
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. H2O)
Average Stack Temperature  (deg. F)
Stack Area (sq.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
                                     125.00
                                      29.38
                                      29.37
                                      -0.17
                                     323.28
                                    1596.00
                                      43.49
                                       0.36
                                      72.30
                                     398.10
                                       7.55
                                      10.01
                                      82.44
                                    0.98750
                                       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 CO2
                                       0.34
                                      41.88
                                      1.186
                                      18.77
                                      0.532
                                      30.95
                                      0.690
                                      29.61
                                      26.02
                                    3542.92
                                    1079.88
                                   39267.33
                                   1112.051
                                   17931.93
                                    507.832
                                     104.03
                                      85.04
                                      1.442
                                      14.49
-------
FACILITY : Mathy #26
DATE:      9-24-91
LOCATION:  Outlet
RON NUMBER;      3.00

SAMPLING PARAMETER
PAH
Total Sampling Time (min.)
Corrected Barometric Pressure  (in.
Absolute Stack Pressure,Ps(in. Hg)
Stack static Pressure (in. H20)
Average Stack Temperature  (deg. F)
Stack Area (sq.in.)
Metered Volune, 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
             Hg)
 125.00
  29.38
  29.34
  -0.58
 326.60
1596.00
  40.52
   0.33
  73.41
 325.00
   7.18
  11.77
  81.05
0.98750
   O.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 CO2
                                       0.31
                                      38.93
                                      1.102
                                      15.32
                                      0.434
                                      28.25
                                      0.718
                                      29.62
                                      26.34
                                    3466.96
                                    1056.73
                                   38425.48
                                   1088.210
                                   18139.15
                                    513.701
                                      95.60
                                     122.05
                                      1.272
                                      16.44
-------
         APPENDIX D

D.I   Multipoint Linearity/
      Drift Summary Tables
D.2   CEMDAS Printouts
D.3   Stripchart Tracings
-------
     APPENDIX D.I

MULTIPOINT LINEARITY/
DRIFT SUMMARY TABLES
-------
 INSTRUMENT:
                        JZT
                                 SERIAL NUMBER:
 SPAN GAS CONG.:
    RUN
  NUMBER
DATE
TIME
                             CERTIFIED
                             GAS CONC.
                                OBSERVED
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 SCALE,(%)
 MULTIPOINT LINEARITY (1)
 MP1
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 (2) Difference Percent Scale = (current observed cone. - previous observed conc.)/span value * 100%.
  ND indicates no da La is available.
-------
 INSTRUMENT:
                                                         SERIAL NUMBER:
                                                         ?/
 SPAN GAS CONC.:
    RUN
  NUMBER
             DATE
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                                          CERTIFIED
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 MULTIPOINT LINEARITY (1)
 MPI
                               Zero:
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-------
INSTRUMENT; 4e/£*j£&tJ &*&»£d/ 70 1 ^~^> SERIAL NUMBER: ?O-?$/flT)--Jt'&'
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(/^"*1
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-------
INSTRUMENT:
                                               SERIAL NUMBER;
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-------
INSTRUMENT: £>£Cj£&/*AS Bg>£~ SERIAL NUMBER: d'0 3 ?%£>
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-------
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                          SC/S   ^
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                                  SERIAL NUMBER:
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 NUMBER
            DATE
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                                          CERTIFIED
                                          GAS CONC.
                                 OBSERVED
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MP1
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-------
INSTRUMENT: &/££>/zf?&£/ s&*S&jgCtf ?J/ /f/2 SERIAL NUMBER: 9$ - %///?& -J~£^-
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MP1
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-------
INSTRUMENT; /&£Q •?£ SERIAL NUMBER: ¥2<)9?S8-H£
SPAN GAS CONG,: ^oo />&*£/
RUN
NUMBER
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PERCENT
SCALE (%)
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-------
   APPENDIX D.2



CEMDAS PRINTOUTS
-------
                        SUMMARY
            09-23-1991   06:12:27
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-------
09-23-1991
0Tiie
09:56:21 f
09:57:21
09:58:21
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10:03:20
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-------
                            CAUttATION SUHHARY
                            09-23-Wl   11502:56
                 CfiLIBRftllON FILE NAffi =D;\CENDfllfi\0923CAL5.CAL
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                     Press  Shifl^rtSt to Print Out Table
                             Prill  (O to Continue

RA&IfiN CORPORATION      0923RUNB

Field Testing and Process  Engineering Dept.
Continuous Efiissiufis rtonitorinq Data
llfiTHY 14
NE« RICHflOHD.SI
Perforied for:               EPS
Date Printed -  09-23-1991   Current  Tiie  = 11:03:52
fils Hits = D:\CEBDATfl\092391.PRN   Calibration File:D:\CEHDATft\0923«L5.CflL
 09-23-1991      02      THC      S02      CD      C02     NOI
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-------
                             CALIBRftTIOH SUIfflflHY
                             09-23-1991   lj:G4;45
                 CALIBRATION FILE NflBE =D:\CEHDATA\0923CAL6.CAL

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                             Pmi  to Continue
Field Ifslirnj and Process Engineeriftg Dept,
Continuous EiissionE Monitoring Data
HATK'J' 16
IjEU RICHMOND,Hi
Per1ijr
-------
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-------
-   *3f
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 09-23-199]
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                         CEH IMSTHUSENT DRIFT SUIWfiRY
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SADifiS CORPORATISM      0924RUN1

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09-24-1991
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-------
                          CALIBRATION 5UFINARY
                          09-24-1991   11:37:52
              CflLIBRATlQN FILE NAHE »D:'\CEM)flTA\0924CfiL2,CAL
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                       CE* INStfil'ftENT DRIFT SUHHflRY
                           09-24-1771   11:58:01
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   092WJN2
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-------
09-24-1991
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RAD1AH CORPORATION
                        W2<
                                      Btpt.
Field Testing and Process Engi
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RADIAN CGRPOfifiTIQN      «

Field Testinq and Process EngiawriiM) Dept.
Continuous Eaissions Monitoring Data
HATHY la
NEN RICHMOND,XI
Perfoned for:               EPft
Date Prints-: =  09-25-i??!  Current  Tise =  07:00:07
File Naae - S:\CEHBftTA\0?2^!.?SS   Cii-Dratisn  Fi!e:i;: iCE«DAT«\«924CAL2,[iL
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                     CALIBRATION  3UMflAR>
                     09-25-1991    07:29:36
         CALIBRATION FILE IMH£  =D:\CEHDflTfl\0925CALl.CAL
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RftBIAH CORPORATION
Q925WHil
Field  Testing arti Prccsss E.nginming Dept.
Continuous Esissions Monitoring Data
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Date Printed = 09-25-1991  Current Tiie = 07:40:55
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09-25-1991 02
Tiif I
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    APPENDIX D.3



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APPENDIX E




 GC DATA
-------
- :  : E .
f H F S H
P K  U D
    H ft  F: E J  •:, y e
    STT i"-  .3
    PLOT
*   PLOT
STOP
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STOP
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-x   R U H  »
START
          IF
     6.397
     1.369
    — IS. 848

     1 1 . 5BM
     12. 7S4
                         5 TOP
                     SEP  22,  1991   1 5 s &2:0 4
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                                                                                           1 8 .
P.UHB
                                 I •? 9 1   15192:04
       CONSTRUCT I OH
A F. E H V.

,
,
1 ,
1 (j.
1 1 .
1 5 .
1 b .
1.' .
i a ,
' Z 3 .

RT
337
651
36-5
226
584
247
136
147
23*
99 2

H R £ H T '
974
4 1 5 3
135'?
1 7 3 6 6 £ 5
694
1543172:
725
71479
2:336262
2793893

.'PE
VB
BB
PB
PB
PB
Be
BB
Be
BB
ve

ia IDTH
.091
. 159
. 323
.216
. 965
. 174
. 876
. 332
. 337
.633

AREH:-;
. a i a ? s
,94595
.01504
19.21337
. 38769
17.07326
. 88302
. 79832
31.93236
.33.98284
TOTAL
R U N
ZERO
» T T  2 •*•
C H T  T3 p
H P:  R E J
THRSH
PK  UD
            O
            3
            1 . 0
            a . 94
-------
                                                                                   11.403
        STOP
RUN*
                     SEP 22,  1991   15:30:32
      CONSTRUCT I OH
-------
                               S E F  22,   i
F U M *
                                   i e P  i £ ,   1-591    15:44:5;
  R T H'('  C 0 H "3 T R U C T I Q N
A P E
                        H ft E A  TYPE    U I 0 T H
                        L Q 0 8      P B      . 8 1 o
                        9631      B B      , () '? 5
                                                             A R E fl ^
                                                            .32345
                                                        9 9 - o 7 6 5 4
T 0 T ft L  H R E A =   3 1 I £ 3 9
M U L  F M L T 0 R = 1 , B 8 y S E + % 0
RUM  PM
Z £ F: Q
rt T T  i "
C H T  S P
AP  R E J
T H R S H
F K  U D
                 u
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                 1 .
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f  U M »
                                                            S E  r-    £  £  ,     i  '? 9 I         I  5  :  J  -i  :  4 0
M H T H  i     C 0 M 5 T K U C T  I 0 N

n F. E n "-;
                  R T                   ,1 ?. E n     7 ',' F  E       U I  u T H                   A P E N !;
             .6*3                 3 5 '? 9 r?     1    6  P          .  8 ' j s       L  9 o .  6 >3 9 £) 0

TOTAL    ri R E ft =       j 5 9 'J'?
M U L.    F H C T 0 F. =  L .  8 0 u 0 E * W €'
R U H    P A F: A It E T E R S
Z E S 0          =       y
«T T    2'"    =       -i
C H T    5 F'    =       1 .  y
ft R    P. E J    =       5 O 0
T H R S H       =       £
F K    U D       =       a  .  u 4
-------
                        k
   RUN*     7      S E P £ 2 ,  t 9 9 1   1 5 : 5 2 : 1 8
T H P T
    	  1F
        STOP



RUN*     ?          SEP22.  1991   15:52:13


MHTHY CONSTRUCTION

ft R E ft K
      RT      AREA TYPE  yiDTH       ftREftH
    . bas       aa4   PB    , aa~      . es 199
  19.313    1?£9492   BB    .215    39.94893
TOTAL HREft= 1738376
MUL FACTO R=i,
-------
!- fi 1  3 r'  =   1 . U
*r~.  R E j  =   5 y 0
T H S i H   =   £
P K  lil G   =   0 . y -t
                             0
                        if k3,f \i-4 I    06: 25: 0
         STOP
FOJH*
                         i E P  £ 3 ,
                                          6 b : 2 5 i
I1ATHY  CONSTRUCTION
M P: E M ';
        RT
       TYPE   ULOTH
  3 3S    PB    .012
6 3 3 2 Q    BB    .134
                                          1.27312
TOTAL  H
MUL  FMCTOR=I.
RUN  PARADETERi
ZERO    =   6
h T T  2 ''•  =   3
C H T  S P  =   1.9
ftR  REJ  «   598
THP.SH   =   £
P K  UCi   =   d.84
-------
        r'    .»
•••  R U H  II
START
         IF
        STOP
                    i E P  £ 3 .
                                    8 6 s 2 7 :
fiUHH
                       i E P
                                I '> * 1
                                           7 : -i
MftTHY  CONSTRUCT 1 OH
H P, E H V.
       RT       MREH TYPE   UIDTH
      185       7 .d B b   P B    .331
      ,93      3 2 S 7 2   V B    . * 3 9
                                     18. 18-188
                                     81 , 31596
TOTAL  A
11 u L F
               -48173
ft U M  PflRftMETEP.S
ZERO    *  6
fi TT  2~ =  3
C H T  S P =  1.0
flR  REJ
THRSH
PK  UCI
           see
           2
           0. 6
-------
>    R U H  »      lo        S E P  2 3 ,   1 3'? 1
's T ^ F T
            'IF
     D.
          3 T 0 P
RUN*      1 &               S E P  2 3 .   1991    Q £ : £ 9 : 5 5


H M T H V  CONSTRUCTION

ft R E ft 5:
         RT          fiREfl   TYPE    WIDTH          AREAX
      .*:35         3641-4   I  BP     .*•??>    180.6^886
T 0 T M L  ft R £ H =
MUL
R U H  PHfiAMETERS
ZERO    =    9
ATT  £•"• =    3
C H T  S P =    1.6
ftp  P.EJ =    58S
THRSH   =    2
p K,  u D   =    o. a 4
-------
 ••      ft U H    B         11
"? T A K T
         ----     I F
                  5 T 0 P
R U H »            11
                                             S E P    i 3 ,     1 9 9  1      Si ii :  S £ :  1  3
                                                                  0 .  ~  0 4
                                                   i E P    £ -j ,    1991
M H T H Y   C 0 H S T  R U C T  I 0 H
               RT                AREft   TYPE      UiDTH
              '04           £47335        BB         .338
 TOTAL   ri F: E H =   a 6 ~ 3 "3 5
 M U L   F H C T 0 R = 1 .  9 0 0 0 E +
 RUN   P A ft H M E T E R S
 ZERO         =      
-------
                             rr
   RUN*
   F T
                     > E P £ -3 .  L '?'? 1   <3 
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E  = E X T t ?, fi F, L  '; T H H D M F. D
I  ~  I H T E r H r« L  •< T M H D •-< F. D
N  = H u F: M H i, I ; r. T I U 11

C -, L I 6  F R 0 C E D U R E  L E » '• I .- r4 ] ;

F E F :•.  RTU  i     5 . y y e 1 :
HuH-FEF  ;;  RTU   [     1S,.Jyy::

F. r  6 ft 'i E D   ON  H R E H  OR  HEIGHT   I A *.- H 1 :
C H L H        F: T           H M T            H H H E
1

2
3
•4
5
b
.

.
1
3
7
1
7-13 * ;i "•

'?•< ?
, 5^4
. 8 «3 -5
. 5 ^ 0
1 . 67>i
( S - . 7 4 ;j
: J 5
: 1 4
: 1 4
: 1 4
: 14
= 1 4

. U
. 5
• 2
. f>
.*
. 5
                                          NETHnKE
                                          E T H H H E
                                          P R u P H H E
                                          P E N T ft N E
                                          PEHTnHE
                                          HEXANE
GROUP  P E ft K -=  CV -- H •• 1 =

CALIBRATION  OPTIONS
R F  Of  uncalibrat*d  P « a k i  [ y . % » W 8 E * <•) 0   J •   j . 9 2 2 E - o 5
R * P 1 a c s  calibration   I' i '•  C Y .-• H * ] :
[j \ -. * b 1 €•  n o i l - r u rt  R T   u P fj a «, *   C V -' N * ] :
SAMPLE  H M T   [a.3y50E+90  Is
M u L  FACTOR   Li.a a e a E + o e  ]:

 "   LI i T:  TIME     S
    y . 0 0 e  I N T G  *  =   2
    u.aee  IHTG  *  =   s
   2 5 . s a e  -5 T o R
 ••   DELETE   TIME  25   S

.r   TIME  £7   STOP
•»   PUN  H    16        SEP   £3,  1-591   33:43:33
START
                                                                                                            1,555
                                                                                                        II  .3 . 7 4 3
          STOP
-------
hw TH'i     C  OH i 7 RuC  I  I  C-rl

ESTu-nREn
                   R  T    T '(' P E                       H R E H        WIDTH                 HEIGHT     C  H L It     C  0 H C  .                        M  M  M E
              .  ~ I  r          F B              2 i  ?,~ J  E - >J /
M  U L    F M C T 0 R =  1   .  ij u 6 y E - C-i y
E  U H    F H R rt M E  T £ R •=.
IE R 0          =       y
H  T T    ^'''"'    =       o
C  H T    •=. f-    =       l  .  y
nR    P- E J    =       588
T  H R S H       =       I
F  K    U D       =       'j .   1 2
-------
• -~ !_ "t
               0 >3 "5 * 1 U (3 . 4
               '5 •" . -3 J
  = C H L I 6 F P 0 C E D iJ r. E
  = RETENTION T • M £ U I H 0 011 '=
  = T n 6 L t E H 7 F I E i
  = P E H K  u F: 0 U F S
  = C M L I B 0 R T I 0 H i
        **#
5 E C I I 0 N TO  BE E D I T E 0 : .3

C M L n :  2
F. T i
ft H T :  1 y i . 1
M M T - H F: E H :
SECTION TO  BE EDITED:
*   RUN*   1;
 T H P T
                SEP 23,  1991  83:59:0;
        8.497
      STOP
             0.715
64
RUN*    17
                  SEP 2 3,  1991  0 9:5 9 s 0 7
MhiTHV CONSTRUCTION

ESTD-AREft
     F;T TYPE
    ,497   F' B
    ,715   V B
                  AREA  UIDTH
                 L 1 0 9 4   ,293
                 57173   .137
        HEIGHT CALtt CONC.
           .J3B
          6974   1R     2.25b  METHANE
TOTAL ftREA=  63567
w u L FACTOR-i.aaeaE
(t U H  P ft R ft M £ T E ft S
2ERu   =  y
HTT  2'* =•  3
C H T  3, P =  L . 8
6R  REJ -  593
T H R S M  a  a
P K  U D  =  a . 1 2
-------
                                                                   0 ,,"34
               •iTOP
                                                                                                            X
f. U H
                                            i E F   15'    1991     3 3 :  'a i :  i 1
i'l n T H Y   C U N S T fi U C T i 0 1'i
E -3 *  LJ ~ H R E
                      '/ F £
                        Ps
  H K. E M     U I  D T H
5 r a 2 L        ,  i i ;-
                                                                                                       COriC
                                         56:34        IF.
                                                                                                                                 MET HU
T 0 T M L   M r E rt =     t« 7 o ^ 1
Fi U L   r H C T u R. = 1 . 0 i-j 0 0 E T- 0 0
f, UN   p ft R A11E T ESS
Z E ? d       =      0
ATT   ;"   =     3
C H T    S F   =      1 . d
n F;   R: E j   =     50 
-------
   C - i. I 5   3

 0 , r ', .5
 i . -? -i 6
 L . 5 3 4
 J . r '? 3
 7 . 5 v :j
. 1 . 67*
-------
-------
HHTHY  CONSTRUCT ION
E 3 7 U -


•
1 .
1 .
3 ,
3,
i.
3.
6,
6 .
b" .
, 9 .
i e.
1 0.
1 L .
. 12.
i i.
15,
I*.
Iri.
1 7 ,
13.
SO,
23 .
24 .
"RE*
R T T
70 I
3 3 3
4^4
H T TJ
1 "3 I
625
«^ 4 .•*
474
745
4i7
7 15
a 85
•i32
139
474
•i-f i
5 i i
492
•32-e
81 9
42-S
435
3 15
*82
526
b 3 S

i1 PL
P6
B&
C b
E&
BB
P&
BB
se
&&
P6
66
66
P&
86
66
SB
BB
6B
68
BB
66
PB
BB
PB
BB
VB

nREH
1 7 o ," o 4
i o ? 0 0
j i J I y a
Q J ^ '-* i
i >3 3 2 3' i
4 7 2 e
54 19
I :J S 4 2 1
22*42
15914
2 1 3 l •?
l---?5,- JT6
1 >s 0 y 9
5 2 "i o
7 1 '5 4 5
o-(622
1 : j 4 o 3 3
2 S ,3 4 9
254639
73*'*
4 3 3 6 5
54251
5393-2
131631
1 2 2 1 o 3
4 5 5 0 6

Lu I &TH
.073
, -38 4
.1,4
. 039
.157
.ill
.104
.He-
.123
.132
.175
. 4 i i
.273
. 155
.271
. 254
.292
. 7b d
.233
.136
. 2 15 2
3 B "•"
,412
.5*9
. "3 &,"
. 'SsO

H E i G H T C M L ft
4 0 4 fl 5 [ R
5345 2
3 1 £ 4 4
I 7 j i 3 j
1 U 9 4 3
6 C 2
3 15 15
1 t 4 6 r
3 0 7 3 4
2 3 1 . j
1 9 o 3
? 3 B S 4 7
979
5 c 6
442'5
5 5 
-------
UN I
                                                              _^  \':l\l
1 3 . 4 y 8

1 J . 5 7 5

12.454
1 £ . 3 6 7
13.^86
14.992


15.454
1 5 , "t 2 5
1 6 . .3 4 7

1".335

18, 172
2 6 . 8 L •»
2 3 . J a £

24.313

    STOP
-------
,^- H

ftT 1
- 5 '• ?
1.144
I - 4 i i
V i J . 4 8 3
1 1.575
12.454
I i . 9 6 7
1 a . 4 0 a
i 5 , 4 5 4
15. J25
1 i .347
17. j i 5
13. 172
20.31?
24 . i 1-5
TOTAL SREr
s ~ r LJ C 7 !

" V F E
c b
8 B
£ a
oB
£6
56
BB
F B
BB
D &
o B
BB
BB
B D
V D
SB
BB
F&
^25.36-
• -, f

fiREH
1 1 i 7 o 4 5
[,2o3
i -i o 3 ^ r
277o,
1 4 B 7 I -j
i-5i5
10445
2 2 0 '5 6 0
1 C-i 582
4 7 Q 0 5
2 '5 2 1 o
•? 4 y 7 -?
1 3 2 * 6 y
ISIS
*i'J
50
CX
WIDTH
- i -5 r
. i j, "i
i -J •' J Q
, i Q J
. rj "/ w
.145
. 1 4.3
. 2o2
. -J 7 4
. i PS .B
.235
. 17'?
. 2 8 S
. .3 3 1
. 5 V 1
. 57 -j
.18£

 GhT
 7 J5
 •350
J 1 -1 .i
,404
i 1 0 3
i 5 S 7
N 13
;295
5524

 434
                                                              15679
                                                                 9 3 3
                                                                -.-,,««
                                                                il 1  1 i'
                                                                1473
                                                                2'? 5 4
                                                                -3 3 1 '5
                                                                 1 21
                                                                        C H L B  C Q H C .
  . Q .2 >3
1.464
5.036
5.506
  .821

  i "j 1 ,2.
5 . 7 5 4
  .075
  .410
3 . <9 Q Q
  .415
1.544
i . 1 46
3 , i 5 0
5. 2Q3
  . 052
                                                                                                    H E ,'l M H £
M U L   F H C T u ft = 1 .  S u 0 w E -MO u
R1J H  PARAMETER 5
Z E F: 0      =    ti
n T 7  j "•  =    j
C H T  s F   =    I . 6
H R  fiE J  =    53d
T H F. S H    =    i
f K  U D    =    13 . 1 c
-------
   SUN  9
                                                                                           i1.571
          STOP
R U H »
MNTH V  C 0 H 3TR UCTi u K
                        E P-  2 J ,
E i T D •
   ift t H
   R T  TYPE
   '16    B B
3 . 6 9 2
7 , 44T
BB
BB
BB
   I L . 5 7 .3  I  B H
                                        1 0 : 2 T : 3
          AREA  WIDTH
 793967
1171181

2041939
5355725
.lei
.203
                      HEIGHT CALft COKC.
                       71342    1 R      1 !
                                          1 39262
                                          ie?7 ia
                                          1D? 3S3
                                          I 7 oo tl b
                                                             1 J .
                                                                      H H M E
                                                                      METHnNE
                                                                      ETKnUE
                                                                      PROFANE
14.944   P E11T H N E'
14,332   P E H T ft N E
14.563   H E ;< H N E
TOTAL AREM
M U L
R U H  P H P. M M E T E B.
ZERO    =   Q
r.TT  2*'- =   3
L H T  & P =   1.8
MR  REJ -   56y
THRSH  =   i
F K  U D  =   8.1
-------
                                                       * 1 ta   S

                                                       ,  >^,,Y/ft'
                                                                                           j - 4 i -5
                                                                                           j . -f ^ .-
          19.353
i i . 5 4
l£. -4 1 7




1 3 . y 15 5

13.341




1 4 . y -t 5
                                       15,425
-------
                                                                I d i 4 1 l 5 j
H A T H V  C U ri -3 T R U C T  i u r

E-iTO-HrtEn


1 .
1 ,
i .
j .
;.
1 1 .
1 2 .
1 3 .
1 4 .
1 j ,
l 5 .
1 6 .
1 7 ,
1 3 .
29 .
"e. "i ,
24 .
KT i
Sr'r
i 5 J
450
22=i
4 i'?
6-5 -j
542
4 L 7
34 1
045
425
•* 1 J
.305
365
083
3fll
266
3 S 3
i i Fc
r D
a B
b c
Bb
5 b
B D
Bo
B B
& E
68
D D
S£
o B
SB
V6
V B
BB
BB
rtfit
< i o j ;>
I 1 o 0 0 3-
J7 36
i • 3 i i 3
3-4 62
^ - l • ;•
5 o 2 J
L .3 4 L ~
.5-33
1 1 54
2 i3 3 7 9
4*4
4540
S 3
20703
1S765
11667
5655
"

J
6
^
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4
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^
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52
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63
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-------

                                                                                                    t . t 2
                                                                                                    o , U i j
i s. ? a -i
17.515
-------
  •j h H         is                     D t P   2 ;> •   i •• ? i      11:111-11
[1 rl T n  I   C Q H S 7 r, U C T I  U hi
            ,  ..    ~ y -  £               H R £ M     iii i 0 T H           ri t i G rt 7   C n L ft  *- u f i»- .                N M M E
         . o .j o       F  B           4 5 01 c - j       . v ^ 5             *L i 7 7 i                      i  r.»»5 5
         . .? 4 5        06             j k 1 i 5       .0-15             I i 4 5 -4       i  F.               .  j S "7     M E T H M h E
         . '3 =J 7        CD             • 3 5 b '3 -"       • 'J d, -J             « "j -9 3 J                        I .  4 Ij ,"•"
       i  . i 2, ;•        cb           c \ T* -3 .i 1       . c >J 1             i $. ^ 6 5                        -i •  r> £ 1
       1  . -i Q y        E.  D               I r 5 i       , Q i u                 o' I 5                          .  1 i «i
       i  . 5 0 Q        £  6               ? 4 9 ?       . 0 -i -3               4 i 5 j                          ,  3 ~ 3
       -i « ij j 5        &  B           i 7 2 4 •* i       .^O^               &olo         •            I  0 .  o o S
       7.515        Ft.               5 ill ™ j       . i .3 7                 .357                          .  1 i '5
  0 T n L   H R E M = L 8 i 7 3 u 4
  U L   F n C 7 0 K = i , o U 'J 0 E » Q u
F: U K  F M r M f'l E T E R "3
2 E R 
-------
'- M s-  l  5 r  n T  i 0 N   0 F ^ I 'J h' 3
'• f*   Oi"    u n o -a  I i b r- a ', * >y   P €• a k  &    C .»  .  J c i 0 E -  >} -5    3  !
P- •= r-'  1  = c  €   c -a  1 i b r a ',  i -i ri     i  i ',    ['(' .  M <•  1 :
D  i i  a b  L  *   r» o  j ;, - r u n   R 7    y P a  i t. =    £  V f H  >• j :
S M M F  L E    H H 7    I y . 4 u >j d E " -J u    3 :
H u L    r M  C T 0 R    [ I . o S 'j d E T vj 0    j :

       Or    »   .3

t i^ i_  I  c ^.  n T  I 0 N   u r' T I 0 N a
f F   -j  T    u n c 3  i ; o r' i '• f- '"J   >"•• f.  3 t,  »    L j  •  ? i i 81 -  £' 5    j  •
r, •! P  i  .a c  *   Call b r -a t  i >j n     t' i T,    [ y ,  ft * J :    y

f    =    ft '}  I Ci  I -  I, o - P v 1 n V
L    =    I i  n « i r    •, 1 •=- a i v   5 •a y  a r « >
N    =    n o  n -  i i n € .3 r    '.. a y a d r  a i  i o >
C  j k  i b r  a  ', i o n    f IT.   [ K •• L .-' F1 *  1 ;
D  i 5  a fc i  s    P o e  i. - r- '.i n   E T    g r- d  -lie    C  V x N  <• ] :
S  n M  F L £   M M T     L fj . 0 0 H) 0 £ * Q O    ] :
M  U L    F H C 7 Cl R     C i , '3 0 8 Q E ^ % 0    ] :
 i-     R U M   »        2 •(
  T n F: 7
                                            S E P   i 3 ,    t 9 'i  I       11:48:56
            1.438
         - J ,  4 5 o
         d .  ?  I 3
         7,  4??
         a,  693
          1  1 .
          13.455

          14.  157


          15.535
-------
     21.*;
          TIMETABLE SI0P
RIJ H *
                         SEP  2;
H H T H V  C Cl N 5 T R U C T i 0 H



1
1
1
1
1
1
1
L
1
2
2
£
1 .
3 ,
6 ,
8 .
8 .
•j .
1 .
2 .
3.
4 .
"5 .
6 .
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3.
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3 .
4 ,
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4
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" 1 BB
3 & 96
56 FB
3 u B B
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260
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1
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3
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9
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99
3
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5
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5
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B&
BB
V6
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6B
BB
BB
BB
66
BB
VB
e&
BB
F &
1 1 i
1
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MR EH
6 7 "i '3
1 4 5 J
1914
1624
SiSali
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. 377
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3681'? . £ y 8
5
5
7329
4613
. 36
. 24
7
1
6 5 -j 6 4 .213
1 2
I

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b 3 3 3
389334

4
23
1 3
3
ii443
3546
5600
. 28
. 27
.65
- 34
. 13
D
L
3
1
1
. 238
. 93
fr
-J
1625 .749
1235

d
25353 . 439
HEIGHT CML* C
51b 13
7663
2753
3 9 3 9 5 -
3 0 7 1
2b3b
3776
4996 b
7457
7 1«
1933
14663
595
2591
3936
4849
2416
563
0 H C .
45. "oa
.449
.359
1 . 230
.329
1.444
2.249
2 . 142
.413
5 . e2Q
.453
. i 4 9
11.779
.253
1.7*3
9 . 2 4 u
7 . 123
j . 136
1.014
                                                                          N rt M E
                                                                          P E N T H H E
                                                                          H E X MI-IE
T 0 T '» L  ft R E ft = Z 5 1 2 6 4 2
MUL
ftUN  PARAMETERS
ZERO     *   g
-------
-------
R U M
                               V",
                                 «(<
 10.573
 15. 
-------
k U fi A
H U   1J n j_ I &   p £ H t-. i  r 0 U H U
nF. E^;.
            FT            n r. En   T  l F t     Id I U T H
    I 0 .  5 ~ 3         '. -It 6 6 I -3       r E       .144
    I^i618        ~J D .3 r 7 r       5 b       .  .j r  o
    I '3 .  i» 3 4         i  ? ,7 'r 5 i       r 6       i  J'? 2
    - 2 .  "-> ~ fj            i e 3 5       F i       .036
    2 3 .  '3 7 •'•}            2 3 2 r       66       .4 ; i ~
    ^.'j,-3'4*:'            *ibo4       B&       .44^
    2 4 .  i l 0        2 I ? 0 6 l       B &       -  .7 <3 i
      M h. t H -
id. -3 0 4 5 i
5 0 i d o & 3 <
i o. 3 r o 2;
    .2472"
T 0 T M L   Hf.EM=l-J657l4
P1 U L   F n C T 0 r = i  . 0 0 U Q £ -^ 0 0
R. U N   r H p. ri M £ T c. R.
IE F, 0       =     f<
H T T   5 •"•   »     3
C H T   S p   =     t .  u
MT.  P. E J   =     500
7 H F. i H     =     2
F K  U D     =     8.1
-------
                                                                                                                        —,
           "3 I U
P. ijli
                                              i ? '5 i
                                                        ;  = 155155
r c
F6
                                            Ul i u i n
                                              .351
                                                        1R
                                                                                li H PI C
                                                                     4 . 03U   METKMHE
  TOTAL  HfttH=   liSO'.--
   SUH  P H ft n M t T t R S
   ZERO      =    «
   rtTT  i'-  =    5
   CHT  =r  =    l.a
    AR  nEJ  =    508
                                                        \
      K  WO
-------
 :  U H  A
                F. T
   M RE H      WIDTH
•"> i 3 •) e          .101
HEIGHT   C HL *    C u H
     .5 343         1  R
                                                                                                                                                                 H H M c
                                                                                                                                                         '3*       J') E T H H H t
T i j T  M L   fiP, EM=      33346
M U L    F M C T 0 F. =  i  .  0 
-------
   w T rf  (     '- u f <
i -  H F. £ H
       F, T    T V F' E
  ,  7 3b    I    or
                                                          H F. E rt
                                                          4 i o 5
                                                                               I 0 T H
H eIG H T    C rt L #    C  U11C  ,                      NAME
      5333          i R                      .591       M£ T H N li E
TOTAL    A R E M =       j •?  I  6 3
N U L    F  M  C  T 0 fi; = i  .  u i3 u y E + a 6
ft U H    F  A R H li £ T E R S
IE r: u          =      0
MTT    i        =      .3
C H T    S  P    =      1 .  8
H R    R E  • j    =      583
T H F: i H        =      2
F K    y D        =      0,12
-------
     10.644
                                                                                        1 1 . 7 i -4
          STOP
 RUN*
                       SEP 2 3 r
                                I 9 •
                                       13! e -a; 12
 MM T H V CONSTRUCTION



1 .
3.
3 .
-: t
•B ,
I 0.
1 1 .
RT r
743
945
5 90
1 23
3 1 6
595
•3 15
644
734
i'PE
BB
BB
PB
VB
BB
BB
6B
&B
BB
AREA
379577
"76304
1158298
29349
1 6 0 S 8 6 9
2617564
3788
5962
2 3 1 3 7 3 i
y IDTH
.097
.1397
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. I 63
.283
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. 282
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HEIGHT  CHLH COHC.
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132791    2        14.664
177141    3        14.365
   627             1 . 1 @ a
164311    4        14.3£5
165913    5        14.784
   992               .149
   493               .234
175322    6        1 4 . 6 a 3   H E X ft N E
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D B i 0 5 5 7 ,135 3 7 o 0 1 . i •'? S
b 6 7 i i: i ? .357 3 3 £ '9 i . 7 '5 5
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8.931
10,342
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1 1 . -145
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TOTAL H RE M= 37 313 7
H U L  F H C T 0 R =1 .  QOQ0Et0Q
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LEVEL
LEVEL
LEVEL
C rl L 0
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L
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1.554 1
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3,772 1
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7.347 1
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ft M T MMT/AftEft
i . 5098E + 0 1 3 .
i . Q256E+S2 3 .
'S.960iE-ei 2.
i.AseeE+ei i.
1 . 42a0E + 0 1 1 .
i.384eE+e2 i.
!.,460iE + iSl 9.
9 . 7 3 1 6 E + 9 J 3 .
1.4680E+81 7.
I . 4560E + B1 6 .







924FE-
3 5 9 1 E -
99B0E-
8399E-
243TE-
2553E-
2252E-
89 58E-
268 1E-
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65
05
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i L L t' - n L F 1 L £ H M M E


k  LIST'  c PI L I 6  o   "i


ILLEGAL FILE N H Ms


>•  L I ? T :  Tnriri  =   i,


>•  L I i T :  C M L I E>  LEVEL c.


! L L. E G H t. FILE H A M E
             34
                      SEP 23,  1 9 9 1    1 6:Q a:5 0
    10.335
    10.5 '3 -3
    11.765


    12.655
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325
593
765
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65<3
136
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6 '? 5
544
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23553
45644
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106530
374514
6110
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144313
623919
116327
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. 130
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.381
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10453
1 1 54
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4715
3 0 1 3
2336
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5037
7229
1 4 8 S 6
534
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4054
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1337
C A L it C U U C .
2 .462
1.632
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. 2 1 3
. 134
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4 .217
1.767
5 .549
1.425
1 . 132
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2 . 346
6 .421
4 , 173
14,638
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2. 023
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11. I 9 «
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24.470
4.562
2.767
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T 0  T H L     hi R E  rt = 2 2 S 3 5  U 0
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CHT    SP    =        1.9
-------
-------

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18.318
16.595
11.763


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14. 333
16.236
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536
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66
66
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22973
26277
62331
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3697 1
26372
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53273
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54164
133763
121133
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TOTAL   ARE»:«=:4691S7
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H T T  2'"  ~    3
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THP-SH    •=    2
PK  UO    -    d.12
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1 1
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4476 ,645
4
317 .446
                                                 HEIGHT  CnLfl  COIIC,          NAME
                                                   UJ41t)     2          1.042   ETHMI4E
                                                    4 3 a 7                1.311
                                                    2 3 0 2                 . 3 •> 1
                                                    2 d 1 5     4           .112'   S iJ T H H E
 24^7
  3 S3
 3886
  1 79
 533-1
 7361
13396
  3 6 ?
 2552
  9ij4
 2128
 32,57
 295-5
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1 2 ,
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426
163
104
746
045
442
543
1 73
3 9 9
5 15
624
543
698
496
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                                                                                  H E X ft H E
TOTAL  AREM=lc40945
MUL
RUN  PARAMETERS
ZERO
ATT a "
CHT SP
to R R E J
THRSH
PK UD
S
=
m
=
=
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        s T o P
RUM*
                     SEP 23,  1991   17i50i5
MflTHY CONSTRUCTION
E3TD-AREft
      R T TYPE
    .745    B6
    .956    &B
   t.£85    BB
   3,359    B B
   3,994    B B
  11.302    P &
   AREA
 356619
 7 S 4 a 4 2
1 1 s 0 3 3 5
2023450
   4718
2 2 9 a :3 9 4
DTH
108
ie&
1 10
164
203
390
219
HEIGHT CrtLIt CQHC.
652€il
130551
175048
Io3e46
165912
931
174970
1R
2
3
4
3

6
15.
1-4 .
1 4.
1 4 ,
M.

14,
3
*
4
7
"7
1
S
24
i 0
91
73
47
85
e~
H A M E
M E T H ft H E
E T H ft N E
PROPANE
BUTftHE
P E H T A H E

H E X H H E
TOTAL
nut FACTOR-i.eeeec+ae
RUN. PflRflMETERS
2 E R 0   =   8
-------
-------
                        3 c. r  » j
                                                                    >>
M Midi  C 0 ti i 7 r, u >. I I 0 f i
E ^ s G ~ H F., E M
        R T  T i1 F E
Ld 1 U T H       HEIGHT C M L *  C 0 H C ,
  .033          -t,"" 4 7    I r,.
                                                                                11 (i 11 E
                                                                        . .~y i    MET HritiE
1 U L  F ii C T 0 R = 1 . €' Q 0 0 E * U U
R U ti F' A R A M E T E R 9
ZERO    =   0
M T T 2 "'  -   j
C H T 3 r  =   i . Q
AF;  RtJ  =   5u«
T H R S H   =   c
F K  kj D   =   0.12
-------
fun  1
                    1 0 . o <5 ->
                                                                             13.715
                                                                  25. 06-*
-------
              i M £ , i-i 6 L £  i i u r
•< U H *
              STRUCT i CM
t3lU-nrEn
         n 7  T i" F E
       « / j LI     b B

   i 0 . 6 o 3     Bo
   i 6 . ;5 4 y     8 S
   1 ^ . ? '? 2     F 8
   2 5 , -j 6 J     P B
                                         bi i D i H
                            4 T 5 5 5 "5      .59?
                            c '5162 8      . 19 '5 5
H£IGHT  CHUS  i^ONC.            rl^PlE
   r.Jili     IF:          i.SJt    PlETHnHE

  i -t 0 3 0                  " . 0 i 3
T ij T r» L  H p. £ H = 2 5 9 I -4 =• 1
W U L  F H C T 0 F. = I .50 0 0 t -»• 0 0
RUN  P
Z E F: 0     =
H T T  £ "  =
C H T  S P  =
HR   S:EJ  =
7 H R S K    -
F K   U D    =
                1  . 6
                500
                6.1
-------
                                i E P  i 4 ,    1 ? ? ;     3 -i : 4 j : 4 ji
RU N «        43
                                   > E f'   £ -t ..   I -?'? 1    8 6 :  4 '? : 4
MHTHY   CONSTRUCT I OH
£ S T D - » F. £ H
           F. T   T Y P E
       .5*5      P6
       .753      B B
 flfiEA    WIDTH
 3338      . 2 5L
> I 6 I 3      , 0" s "3
HEIGHT  C AL *   C0 H C,              NAME
     255                      .151
   5583      1 ft              .'"-"Ij     METHANE
TOirtL   H R E H a
MU L  FACT Q R-U
F: U K  P M R M M E T E R S
2 E R 0      =     0
HTT  2A  =     3
C H T  S F  =     1.3
AR  RE-J  =     508
T H R S H    =     I
P K  U 0    =     0 . 1 2
-------
                                            ." 4 a
                                                                                    0. :-4-.j
                                                                                    1 . 5 a 4
                                                                                    11.746
         STOP
RUHR
                     SEP  £4,  1991   07:34:89
PI A T H Y CONSTRUCTION
1 . 5%4
 .614
          TYPE
            BB
            8B
            BB
            PB
            68
            PB
   AREA
 289279
 66325?
1368131
206714?
197 1943
22S31 14
U IDTH
 .696
 .892
 . 185
HEIGHT CflL* COMC.
          1R      13
          2        12
          3        13
          4
                          . £19
121648
168556
166369
163485
17212?
642
238
                            18.396
                            14.372
                            14.234
NAME
M £ T H A N E
ETHAHE
P R 0 P fl H E
eUTftHE
P E N T ft N E
HEXAHE
TOTftL fi|REfl=33127£9
MUL
RUH PARAMETERS
ZERO    =   0
ftTT 2'  =   -3
CHT 3P  =   1 .0
AR REJ  -   588
T H R S H
p K U 0
       S
       8.12
-------
    B U H  »     43       S c. F  .i 4 -   rr '•• 1   .J 7 : c 4 : a fj
                                                                                              11.7-43
R U N »
                        SEP  24 ,
                                         87124:48
MATHV CONSTRUCT 1 OH
ESTD-AREA
       R T  TYPE

.
1 ,
3 .
'j *
7.
1 1 .
736
933
584
316
283
652
74S
BB
BB
BB
BB
BB
BQ
PB
  flREH
339761
                     1151474
                     1594363
                        2113
                     1932493
                     2262450
UIDTH
 . 096
 . 997
 , 193
 , 163
           .282
           .219
HEIGHT
 67321
1-33510
177725
163324
    596
163956
171959
1R
2
3
A

5
6
COHC .
     15.291
     14.731
     14.379
     1 4.705
       . 993
     I 4. 449
     14,230
UrtME
METHflME
ETHftHE
P R: 0 P fl N E
BUTRNE

P E N T ft H E
HEXAHE
TOTftL
MUL  FftCTOR-l.e000E*eO
RUN  PARAMETERS
ZERO    =   9
ftTT  2"  =   3
CHT  SP  =   1.0
AR  REJ  =   590
THRSH   =   0
-------
     -UH   4
                                          
-------
       .  Fun  »
       T A P T
c
               IF
          i a. 4 15
          1 5.
          17 . 4 7 5
          13.31!
            .355
                          j c r  i
-------
            T i M £ T A 5 L t  STOP
F, U H *
                              '5 E P  24-  l£9 I    39:03:2;
H u T H V  C u i i j T R U C T I fj II
HO  CrtLiB   PEr,Ki   FOUND
         RT
   I 0 . -4 1 T.
   i r, 475
   n r- E «  TYPE   U I D T H         H F; E A :;
 5650'    B B     .146     11.94314
l 3 1 r t, 3    B B     .  y 0 Q     2 i . r'? G o 2
213610    B 6     .484     35.16122
1 '3 3 4 -314    PS     .  i 3'3     "3 1 . '3 'S'3 3 3
TuT«L  fc R S fi =  6 y •» o ~ 5
HUU  F«CTOR=1 .OOBQE
RUN  PARfiriETERS
~ E F; 0    =    9
C H T  'i P  =    1 . 0
SR  REJ  =    5uy
THR5H   -    -J,
P K,  bl D   =    0.04
-------
^,'r
                :-. u H  *
                                         SEP  2. •> ,   1  ? ? 1    3 j : 4
I
>

                      a '3
                       >TOF
            R U N »      "3
                                           SEP   14.   i 'j 'J 1    3 '5 s 4 6 '• 5 -1
            H h T H V  C 0 t-i 'i T r. U C 7 i 0 H
                     R T  T '(' F E
                     99  I  6P
                           3 -3 b 1
                                       WIDTH        HEIGHT  Ch*Llt  COHC.            It A ME
                                        .134           "3.3 5 3      i R          i . a 0 S    Pt E T H rt fl E
            T 0 T H L  fi R E A =    i 3 6 I
            HUL  FACTOR=1,OB99
            RUN  PARAP1ETERS
            ZERO     =    W
            H T T  2"  =  - 2
            C H T  S P  =    1 . 6
            HR  R.EJ  =    599
            T H R •-, H    =    4
            P K  U D    =    0 . 5 4
-------
F.Ul-il
                                         2 -t >   1 '5 9 1     a -J : -4 3 ; 5,~
M ri T K V  C 0 H i T r, U C T I 0 H
E S T D - in f. E H
          fi T   T',' P E
       , 7 •} y      86
  H KE M    WIDTH
•31484      ,  0 9 o
HEiGHT  CAL*   COH(
   5 -! 5 o      IF;
          MM ME
. '? 4 t    M ETHANE
T u i H L  n R E A =    o 1 4 3 •»
M U i-   r h C T 0 R = 1 . 0 0 3 Q E +• B
RUN  PftftHMETERS
ZERO      =    0
HIT  £"  =   - a
CHT  SP  =    1,9
HR  F:EJ  =    59Q
T H R S H    =    4
F K  UO    =    S.Q4
-------
              :'= T 0 P
RiJrtD         80
                                       ; E P   24,   I '3 ; I    0 'r : 5 £ :  I 3
    T H
  H             !
                      K lj C T I 0 H
            F. 7   T (' F E
            3 '5       6 B
   rtfiEA     WIDTH
> 5 '5 4 c Q       .119
HEIGHT   CrtLI*  COHC,               HhME
  53630       1 R           1 4.8 3 i     M E T H H N E
M U L   F H C' T 0 r. = i  .  U 3 0 8 E + 6 0
R U II   F M R H H E T E R S
ZERO       =     Q
rt T T   2  "   =   - i
C H T   'a F   =     l.Q
Mr.   RE J   =     3US
T H F: S H     =     4
F K.   Li D     =     0.04
-------
         STOP
                                 14.  1351
H M T HY  C u N '-i T r, U C 7 I 0 N
E ? T u - A R E H
        RT  TYPE
     . T4-4     EB
H R E ft   UIOTH
-3 1 0 6     , a 3 S
HEIGHT CMU*  COHC,           HAilE
 4 -t 1 3.3    1 R        10,05-3    M E T H H H E
TOTAL  H R E H =  i.59ly>i
WUU f HI". TOR= I . &G&0E *QO
R U H P ft R ft M E T E F: S
ZERO     »    6
ATT 2"'  =  -2
C H T 5 P  =    1.9
AR  REJ  -    see
THRSH    =    4
F K  UD    =    a . 9 4
-------
                      i  T 0 F
R 1J N *             3 j'
                                                                                                                                                                                                                                . -U .
                                                          3 E F-    34-      I  9 9 1
E  i T 0 - H R  E  ^
                 RT     '
,' P E                     M P £ M       WIDTH
  r B               252516          ,  0 'J  6
HEIGHT    C  A  L tl    0 0 N C  ,                      N ft M E
   •1 3 9 6 •*           IF;                   9,795       r
-------
                                                                          I VJ I  .J ~) '•  ^ .
                STOP
F.UtU
                                              'I E P   3 -I  -    15 ""-1 I      I 0  :  8
 "l rt T H 'r!   L. 0 N 'i T F U C  7 I 0 11
EbTu-nREn
              R T   T ••! P t
          .  7 5'?        B B
                                              AREA     WIDTH
                                            3 5 r I 5        .  1 y 3
HEIGHT   CALB   COHC.                  HnHE
     5 -4 •> 3        i P.               1 . 0 1 £      ft E F H H H E
TOTAL   ft R E H =     33715
         FA C TO F: =1.00 6 0 E + 0 0
RUM
Z E F: Q
HIT   S "
CHT   SP
HR   FEJ
THRSH
P K   U 0
                       1  .  "3
                       Sue
                       -t
                       9.84
-------
F .J I-   0
          TF"
                                                                                                                                                                            3 .  ? £ t
                                                                                                                                                                             1 0 . 5 <) i
                                                                                                                                                                               2.563
                                                                                                                                                                             15.5bi
                                                                                                                                                                             16, 4 8 8
                                                                                                                                                                             1 3 . 4  1 9
                                                                                                                                                                             Z 3 . 6 o 3
-------
               T 1 M £ T H £ L E  3 T 0 F
                                     SEP  i 4
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n H T H Y
                   ' RIJ C T i 0 N
      D - M F. E ri



I
1
3
=,
6
7
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i 4 .   L * 3 L   I y = -M ; i y     r
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                                                                 i . 4 "5 ~
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                                                                 11.
                                                                 15.5 3 3
                                                                 £ 3,640
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                                            i. J -    t > 7 i
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457
492
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p
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PS 5 " BE
1 2. 54y SB
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535
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1.560
j .  5 b 2
1,87 9

2 .  S 3 3
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TOTnL   dF:EA=  615140
M U L  F H C T I "J R = 1 . fi Q y o E + a 0
R U H  FARftMETE F: S
IE R i J      =    Q
ATT  2"  =  -2
C H T  5 F  *    i ,  0
AR  REJ  =    5oti
T H R S H    =    4
F k  U D    =    u .  a 4
-------
EiTD
Fcr  :~.  F T Id:      5,oOO    HOri-r.EF  '.  r.I'ui:     3.000

LEVEL;   i                   R E C n L I B F. M T I 0 M S i   I
LEVEL:   i                   P- S C A L I 6 P, A T I Q H 'j :   i
L E V E L :   .;.                   F. E C A L I B F. A T I 0 l-l S '•   1

C H L I*        P: T         L V      AMI         M M T . H R E n
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   c        o .  •; i o       i  1 . 4 5 0 3 E •>- 0 1   1 . 3 S 3 9 E - 0 5
   3        1.545       1  1 . AiB0 E + 0 1   1 . i 4 3 7 £ -u 5
                          i  1.-3U4SE + 02   l,i5v3E-iJ5
   4        -3 .  ."* 3 £       I  I , 4 e fl S E * vj I   r . 2 i" 5 2 E - I? i
                          2  •> . 7 i i a E + V 1   b , S 9 5 b E - u 6
   5        •" .  ? 7 7       i  1 . 4 6 3 a E * 0 1   7.2SSlE-Ois
   i       i 1 .  '5 1 3       1  1 , 4 5 9 0 E *• 0 I   6 . 2 1 I 6 E - >3 Q

C M L #        r< A H E
   i    METHANE
   2    ETHANE
   .;    P R 0 P H N E
   4    BUTANE
   5    P E H T A N E
   i    HEXAHE

CALI6RATIOK  QPTIOHS
R F  of  u n c a 1 i b r a i e d  P * a k s  ....   i . '•> £ Z tl E - 3 5
C .s 1 i b r a i, i o n   fit	 . , .  P
G i i a b 1 e  POST.- r g n  R T   u f> d a ', €  . .   HO
s ft hi P L E  ft n T	 ,	  a.aaaoE + QQ
M U L  FACTOR	   l.a800E + S6

»    EDIT    CALIB  3   a
 1  »  CMLIB  PROCEDURE
 2  =  RETENTION  TIME  WINDOWS
 3  =  TABLE.  ENTRIES
 •4  =  PEAK  GROUPS
 5  =  CALIB  OPTIONS

 SECTIOH  TO  BE  EDITED!   3

 C M L * :    l I S
 RT :
 M M T :
 M H T , MREH:    3,-»:35E-e5
 NAME:

 CftL H :

 SECTION  TO  BE  E D 1 T E Ci!

 *    EDIT   CAL IB     a

 1  =  C A L I  B  PROCEDURE
 2  =  RETENTION  T I 11E  U I H D 0 U S
 3  -  TABLE  ENTRIES
 •4  =  PEAK  G R Q IJ p S
 5  =  CALIB  OPT IONS
-------
                 .3 , '•> -i !• 6 - -J 5
C H L * !    2
f. T :
H t'l T :
H 11T - S p E H :
H M M E :
2 , >J 1 -3 E - y 5
t » L It :     3
F T :
h M T :
n Pi T , M F, E M :
li ri n E :
1 . 2 S 6 E - 0 5
C A L * :    4
P T :
M M T :
A rt T .' A F, E ft ••
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C H L # :     5
ftT :
ft W 7 :
ft 11T -' ft F; E H :
M H M E :
7 . -3 'd 3 E - «
RT ;
AMT-'MREM:    s.
   CTION  TO  BE  EDITED:
-------
                                                                                    §:§?§
                                                                                    i. -M :•
16. 5'33
1 1 , b 7" 8
                                                                                    14. 195
                                                                                    15.551
                                                                                    13.
                                                                                    23,6
-------
PI n T ri Y   ;; o H i T r. U C T I 0 N







1
1
i
1
1
2
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TOT
MUL
R U H
2 Eft
nT T
CUT
riR
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P K
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- o .; 0
i.o; o
1.44V
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7.521
>;i * 5^3
i . 
66 52V23
& S S 2 5 1 7
SB 251107
V B 243151
F- B I 7 ii 2 i :3
B B 107577
= 127-3977
= i , a u »3 e E T e a
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4
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. 0 3 i
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.144
.221
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                                                                   HEIGHT   CnLB  C OiiC .
                                                                                                                h n I'l E
                                                                                                                M E T H « H E
  4*4 6
  5 i o 4
1  1737
  4131
  j 364
  2743
1 .  5 3 15

1 .  U 5 d
4.270
2 .  0 7 19

*? .  S 4 S
                                                                                                                F £ N T H H E
                                                                                                                HL I'. n
-------
.'-/   lu.S-M
    i a. a u;
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  0 d »
n H T r! V   C 0 H S T R U C T 1 Q N

HO   CMLJS  PEHK'i   FOUND
» R c n:.
            r T             n p. E M   r  f f c     a I Q T n              n f, c. n",
    10.544       I o Q 0 1 j l       ft,       . 2. 1 4       i i'.  5 o 1 i 5
    i 'j , ^ v ^         "a 5 ii "5 «' I       f* o       . '3 ^ d         .3 .  ,-  5 1 '3 j
    L j , .= Q 7       ^ 5 !3 6 i 0 0       f 6       .-410       j 4 .  S 4 ^ s 7
    2 4 , S 1 5       i 5 c j '; r b       F'S       . ." S -3       3 i .  o ~ 4 I -3

T 0 7 H L   M F. £ S = r 4 5 a * 4 .~
M U L   P H C T 0 R = i . u « 0 0 E - S O
RUM  PRRnllETERS
ZERO       =    fl
nTT  S."  -   -2
C H T  S P  =     1 .  «
nR    F.EJ  =     559
THRbH     =    -1
F1 K    U D     =     u .  Q 4
-------
u H  »     .3.3
10.57 I
15.613
24 . 3-J3
-------
MH7 HV  C 0HSTRUCT ION
                                      (&
HO  Cn L I 3  r E h K i  F 0 U I J D
H F, t n ',
         f . T         r, K E n F r' P E   WIDTH
   1 0 . T. T i      i 5 o 0 7 t.    E- &    . £ 0 '3
   I '3 . -3* i ^      ^ ^ -9 ii y -5    D E    .411
   i 4 . 3 i -s      i I S ; 5 i    r' 6    . i 5 4
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                                              I 5 , •? y i -~ -J
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T 0 T H L  M r. E M =  ii 0 i J -S I
M U L  FriiLTGR =1. 5 6 w & E ••- 8 8
r, U H  r H R H t'l £ 7 E P. D
Z E R 0     =   &
M T 7  i    = — ^
C H T  S P  '   t ,  6
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T H F. 3 H    =   4
F K  U D    =   0.04
-------
E :TD
r E F   •'.   R T U :       j .  0 u 8     H 0 M ~ n. t F   '.   F. T U :       3,00 -j

LEVEL:   1                         FECnL I 8PnT I  DNS;    i
LEVEL:   2                         F £ C ri L I B F- A 7 i 0 N i :    i
L E V t. L :   5                         F E '„ n L I & r. n T !  0 H 2 J    i

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                                  i   1 .  5 0 5 0 E •»• 3 1     3 .  .3 -1 j tj E - u 5
                                  2   L .0 c 5 0 E » 0 i     S.3591E-G5
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                7.563         I   1 .  4 6 Go E * u 1     7 ,  3 S 3 3 E - ti 6
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C A L »           H ft M E
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    o     P R 0 F H H £
    4     BUT ft HE
    5     P E H T H N E
    D     HEKHHE
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P F   of   u n c a 1 i b r a i * d   B e •» V, 5   ....   .j. .  5 i i 8 E - -J 5
C or  1  i b r a  i, i o n   i i i   ....... . .....   P
D  L s  a b 1 s   P u = ', - r u n   F: T   u fr d a 1 4   .  .   H 0
oHMF'LE   ft M T   ........... . ......   8
M U L   F A C T Q F:   ..................   i
 •i      EDIT    C H L  IB       2

 1   »  CALIB   PROCEDURE
 £   =  F; E T E N T I Q H   TIME   U 11J D 0 U 5
 S   =  TABLE   ENTRIES
 4   =  PEA K'.   u R 0 U P S
5   =  C A L 1 8   0 F' T I 0 N i

SECTION   TO   BE   EDITED:   'C

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 •t-      EDIT     CALIB       3

 1   =  CALI6   PROCEDURE
 2.   -  R E T E H T I 0 N   TIME   U 1 H D u U S
3   =  TABLE   E H T R I E 'i
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5   =  CHUB   OFT IONS

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 '   EDIT   CALIB   «3

i =  CHLIE PROCEDURE
£ =  RETENTION  TIME  UII4DOU3
3 =  TABLE ENTRIES
4 =  PEAK  OS GUPS
5 *  C A L J 6 OPTIONS

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M U L    F M C T 0 R  =  1  ,  01< t) 8 E  + 0 u
RUN     PARAMETERS
ZERO           =        y
H T  T     2 •"     =     - 2
C H  T     S  F"     =        1.0
H F:     R E J     =        3 Q 0
T H  R  3  H        =        4
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£2444944     .139
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3 4 4 0 06 £     3        £31.929    P R 0P H H E
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RUH  FMR ft ME i Er. 'j
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HTT  Z-  =  -£
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fi R  R E J  =   5 0 3
T H R & H    =   4
F K  W D    =   0.84
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      1 3 . •» 2 13
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              STOP
RUN*        95                 5 £ P  2 4 .    1931     1 6: i 2• 4 £
MflTHV  CONSTRUCTION
          RT  TYPE            rtREft    UIOTH         HEIGHT  CAL#  COHC.             HrtME
    I Q .  5 i 5      B B         162243      .299           1 2 9 3 Q      7               .985    BENZENE
    1 .3 .  -1 2 fj      PB           76654      .304             
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    18,
RUri»
                      SEP 24,  199L   l6:5^:5a
      CONSTRUCT ion

E3TO-HRE*
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13.534
15.58o
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TYPE
PB
66
1 BP
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1 •» S 6 3 £ 3
"£l 15573
UIDfH
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1 .251
HEIGHT  CftLK COHC.
 13355    ?         .934
 2 "633            58,^9-1
 £3234    3       IB.iSfl
                                                                 HAHE
                                                                 BENZENE

                                                                 ETHVLBEHZENE
TOTAL HREM-.-J753986
-------
F. IJ M  F' H P- IT i'l E T E £. C-
:ERO      =    o
HT T  2 '    =  -2
€ h 7  S?    =    1 .  y
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T H F. •;. h     -    4
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£4:51
            TF
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                             SEP  25.-  I'JSl    6 7 s £ •» ! 5 1
f'lw THY  CONSTRUCT ION


,
1 .
2 .
€, .
16.
RT
5 13
649
893
730
3 0 3
3 3 2
T V P E
PB
BB
BB
BB
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1
1
2
(1
HREft
4 6 6"j i36
9 2 fl 9 2 4
353454
880156?
333526
665480
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, 356
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.971
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. 259
.234
                                                    HE1C.HT   CM|-»  CONC.           NnME
                                                    13/645                1 a.£39
                                                    265206                36,119
                                                    315662                5 3. I a £
                                                    £€15339                73.736
                                                    166336                91.717
                                                                  ,'          16.379   BENZENE
TOTAL  AREfi=9.6433E+e6
HUL  FACTGR-l.S680E+0e
RUN  PARAMETERS
ZERO     =    8
HTT  £-'-  =  -i
C H T  S p  =    1.0
Afi   S, E J  =    5SQ
T H R 3 H   =    4
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C H T   b P   =    i . 1
Hp;   P.EJ   ^    5iji
T H R i H    =    4
PR   L.JD    =    0 .
-------
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. ''- 5 :;  rs F-,^  TYPE    UIDTH           ftRErt^
       .515         3 i l J 5 7      f-' 6      . y 5 D    1 0 9 . ^ 1J 0 8 0

TOFrti.  Hf:£«=    3&9S7
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F, U H  PnRA METERS
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ft T T  2''  •  - 2
C H T  S F'  =    1.0
MR  REJ  =    "3ma
T H R S H    =    J
P K  LJ 0    =    3 . 0 4
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C1-C4  14.5 PFHV
   RUN  t  nil
START
                   T ? ClL - i
                            O  e N D -•
       F
         STOP
                     5EP  25.  1991
                                                                                         10. tO iJ
RUN*
        I 31
                       SEP
                                  9 I  87:56:93
NttTHV  CONSTRUCTION
ESTO-rtREn
ftT T
. 52 I
. 000
i . i a 7
2.799
6.328
I 0 . 4 9 S
TOTAL flSEw
MUL FACTOR

Y P E
BB
BB
PS
P6
SB
BB
a .^
= i .
                      AREA
                    4632~5
                   137S8 1 9
                   2269279
                   26Q22 13
                             y IDTH
                               .S57
                               . 959
                               . 871
                               . 149
                               . 281
                               . 225
                S90E+ic
                                         HEI&HT  CftL* COHC.
134379
2*3785
319205
289526
1 38320
192434
18. 170
36.493
53,o49
73.578
89.001
15.371
         BENZENE
RUN  PARAMETERS
ZERO    =  g
flTT  2"  - -2
CHT  SP  =  l.e
ftp. REJ  =
THRSH   =  4
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', ij'sE  BREnK  Or  C C'ti T r, OL -'r   TO
B T E X  '= T li H D K G ,   1   F P 11 V
     R UN  It    1 a 2
S T fl R T
SEP  c 5 .   i '"i '
                                                 0 3 :  1 .7 : 0 1
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                                                                                                                       14,313
                                                                                                                       I 6.£ 18
                                                                                                                       16.3 a a
                                                                                                                      21.437
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f. U 14 I
          I Hi.
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         P T
    i , 2 b o
   I 4 . i l 3
   lo,2I3
   1 e,3*3
   hi R E n  r v P E    u i D r H          AREA:;
2U 3032     66     .225     14,43632
2 0S389     Be     . 1 'j "     14 ,  6 9 U i 3
3 T b 9 S J     66    j . 2 1J 1     i b .  1 3 5 1 4
             B 6     ,-336     2 i .  T 6 9 4 9
             B 6     ,583     2 I .o 6 ' 37
                 3 1911 3
T 0 T H L  H R E A = 1 4 y 1 4 9 4
I1! U L  F ft C T 0 R = l . y C 0 6 E + ij y
RUU  PARAHETERS
ZERO     =   
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- H 0 7 £ P f Cr

.,  U .3 £  S E E ri /.  0 a   C 0 N 7 R 0 L - <   ' 'J   END,'
6 T E   S X    1 , 13  P P i*" 'J    3 T H N D M ft 0
k    RUN*   183         S E P   i 3 >  1 9'? 1    0 3 ! 5 -1 : 4 'j
3 T ft R T
        -	—rr-
                                                                                                                               14.320
                                                                                                                               15.511
                                                                                                                               16.395
                                                                                                                               21.522
               STOP
-------
f "J  C ri L i B  r E H K >  r 0 U H D
           RT
    S 1
                         nftEft   TYPE     WIDTH            riRE*;-,
                      I 9 3 0 r2      E 6       .2 c *      24.49438
                        3 v 7 £ "5      E: B     i  . >i ." 1        4 ,  5 i J J i
                      arS'?2l      FB       . J3?      3=-.£5^-34
T U T H L   H R £ M »   r 9 t  1 i .5
MUL  FriC TG'R= 1 . yuOOE + y-J
RUN
ATT  2'-   =
C H T  S Pa
* P.   R E J   =
T H R S H     =
P K   U D     =
                  4
                  0.04
-------
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—      i r
  •9,256
  14,3Q5


  1 5 . "t 7 1

  16,332
-------
r. IJ H
                i  0 4
                                            '3 £ r'   I 5  -    I 5 '? 1
     T H Y   C 0 H S T R U C T I Q N
HO   C R L  1 S   F E fi K S   F 0IJ H D
H P. t A :•,
             F; T              n r. t H   T V r E     lil  i D T H              n R t h:,
       '5.256          13^,13       PB        ,227        ii.5r-i-3~
     i 5 . 9 71          1 j i 3 3 3       B 6     '?  , -4 U S        I 7 . 7 i» j -t o
     1 Q . o b' c         2^05 -j >S       '/ B        , o 4 5        -i' y . *2 S 4 i '3
    £ 1 . •; i i         c 5 i "J 0 6       V B        . 3 '? £        3 a . 3734 7
T 0 T t, L   rt F. t M =   3 o o 5  1 fl
n U L   F H C 7 0 R = I .  0 0 9 0 E
F; U N   P ft R ft 11 E T £ R 3
2 E F: 0       =     0
C H T   '5 r'   =
hF:   REJ   =
T H R S M     =
P K   bi [j     =
                      1.0
                      506
                      -)
                      0,94
-------
 »NQ7EPb 0 'i e  5 F. E S K >J F.  C 0 N T r 0 L - i'  ~ "j END .•
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S T M R T
    .	  ! F _

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        STOP
RUN*    105           SEP  25,  1991   1 @ : 6 l ;
MATHY  CONSTRUCTION

NO  CALI6 PEAKS  FOUND
M R E H 'r,
       P,T       AREA TYPE   U1DTH
    .•193     130534   PB    .036    42.58165
    .561     293659   BB    .132    5?. 49835
TOTfiL  n
            j . aeeeE + ee
RUN  PARflMETERS
ZERO    =   e
MTT  ~d'"  =  -2
CHT  SP  -   l.Q
AR REJ  -   5051
T H R S H   =   4
PK yo   =   a.64
-------
             L 16
     R T 10 :
y e y    H 014 - R E F  :>,   R T U :
                                                         5 . u y o
LEVEL: i
LEVEL: ;
LEVEL: 5
C A L » R T L V
IF: Q . 7 5 y 1
c
5
c U . '•> 'i i i
3 1,55-! I
£
4 a . r 5 i i
d
5 7 , 46-3 1
6 11.725 1
7 I y , 5 7 6 1
3 13.307 1
9 i 4 . S 1 5 1
C A L It H M M E
1 M E T H H H E
2 E T H ft 14 E
3 P P 0 P A H E
4 B U T H H E
5 P E H T fl N E
6 H E H M H E
7 B E N Z E H E
3 ETHVLBEHZENE
•'i 0-XYLENE
CAL I BRAT 10H Qf'T I OH3
R F of 'j n c « 1 i b r a i e d

D i ~. a b I e BO* i- run R T

MUL FACTOR 	
RECHL1BRHT IONS: l
R E C M L I B F, S T 1 G 1 i i : 1
P. c. 1 n u I c R ri i i u 1 1 i- . i
H M T n V\ T - n F: E
i . 5 0 Q e E -*• 3 L 3 . S 4 s1 3 E
i . -3 2 5 3 E -*• 3 2 '5 . S 5 9 i E
? . 5 » 0 'j E - 0 L 3.4 i 5 0 E
1.4500E*0V c. • 0 1 i 8 E
l.-li80E + Ol 1 . 2 S 6 fl E
1 . e Q4 y E <• 0 2 I.iSSSE
1 . 4 6 W ij E + 6 1 9 . 1 5 6 0 E
9 . 7 3 i y E + 0 1 S . 3 ••> 5 3 E
1 . 4 ii Q <3 E * 0 L 7 . 3 y 3 U E
1.45UGE-OL 6 . 4 'J 7 5 E
1.0Q0eE + 00 6.6'J9aE
1.14QQE + 0Q -4,S38i3E
l.Qs00£ + eO 4 . ••} £ ii 0 E











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DELETE    CMLI6
LIST;   CAL1B
ESTD
R E F :'. 1
LEVEL!
LEVEL:
C H L tt
1 R

2
3

4

5
6
7
3

STU: 5.
1
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ftT
y , 759

0.922
J . 554

3 . 7 5 i

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11.725
10.576
1 6. 307

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1
2
1
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1
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. 4606E+01
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. 1 400E + Q3

RTU: 5.806
I G N 3 i 1
IONS! 1
AMT/ftREA
3 . 3496E-05
3. 359 IE-05
2. 0130E-05
1 .2&e.BE-05
1 . 2553E-95
9. 1560E-06
3. 8953E-06
7.3S30E-66
b. 4675E-96
6. 3390E-06
4.3590E-e6
-------
   ^.      H n K E
   ?   r r -I' F M ri t
   •1   B U T M H E
   5   F E N 7 H N E
   •=   HE A H H E
   r   E.EHZEHE
   "=   ETHVLBEMIENE
   !?   C> - X V L E N E
C fi L L & R ft T I 0 r,  OPTION'-.
r. F  o f j •=. T, - r u n  R T update  •  ,  HO
S n M F L E  ft M T  ..................  0 , 9 9 9 U E T 0 >3
M U L  F H C T 0 F ............ . ......  1 . a 0 M 0 E + 8 u
•-   EDIT   C H L I B    £

1   =  C H L I 6 PROCEDURE
i.  =  R E T E H T 1 0 H  TIME U I H D 0 U S
3  =  T M B L E E H T F, 1 E S
•4   =  P E H K  G R 0 U P 5
5  =  C H L I B 0 P T I 0 H S

S E C T I 0 N  TO  BE  EDITED!  3

C « L « :   I
R T :   .521
H M T :
AMTVSREA:   3 . 2 Z? 5E -05
H A M E :

C M L * :   2
R T i   . 6 b Q
A M T :
H H T . M R E ft :   1 . 5 5 6 6 5 5 IS S $ 6 & 5
I -I ft M E :

CSL* :   2
R T i   .640
M M T :
MMT/AREM:   1.5645E-Q5
NAME!
     !    3
R T ;    1.107
     AREfl:    1.0435E-95
N PI n E i

C H L » s    4
RT:   2.799
NAME:
CflLK:    5
RT:   6.3328120
N H PI F. :
-------
t ^ L » :    ?
PT:   -5, £,6
AWT:   1 . f] 0
"MT.'sREn:    5 . 1 6 -i E - 0 o
H H M E :

>~, M L # :    3
P. T :   1 4 , .3 i :;
M M T :   I . 15 5
f> H T , « S E H !    5.9S56-yb
H A M E :

C n L » :    9
F. T :
HI1T :
H M T ,' f, P E * :
N H M E !    T 0 L IJ £ N E

C ' H L H !    '•>
f:~ '•   16,333
ft M T :   1 . H
A M T / A R E H i    4 . 9 1 1 E - 3 6
NAME:    ETVJSHVLBEN2EHE

C rt L » :    I Q
ft T s   21.43?
ft M T :   1.03
S M T -' fl R E ft f    3.322E-ido
H R 11 C :    o - X V L E N E

CALK:

SECTION  TO  BE   EDITED:

*   DELETE
6 R E H K

*   EDIT   CHL1B  £   BREAK

•c   DELETE    CttLIB   2   S

*   EDIT   CfiLIB  2   O

1  =•  CALIB  PROCEDURE
2  =  RETEKTIGH   TIME UIHDOUS
.3  =  TPBLE  ENTREES
4  =  PEftK  GROUPS
5  =  CftLlB  OPTIONS

SECTION  TO  BE   EDITED:  3
CAL » :    1
RTi
ANT:    .993
flMT/ftREfl!    2.575E-95
H A tn E i
SECTION  TO  BE EDITED:
-------
H u ri - P E f
L E 'ijl E L
LEVEL
•: A L it
I

£
3
4
5
6
v
a
?
1 £1
CALK
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2
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4
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0,521 1
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14.313 1
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H rt M E
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ETHANE
r P 0 F H H E
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F E H T A H E
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Mf'IT
1 . 5 0 y U E -r 3 1
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SAMPLE fl M T
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SAMPLE  H I'l T   [ 3 . 8 j el y E * 0 0   J =
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TOTAL  AR.EM=27y52 t 9
H U i.  F
RUN  PARAMETERS
ZERO »
ATT 2"- =
CHT SP =
AR REJ =
T H R 5 H
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0
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1 . 0
590
4
0,04
-------
1 ij i c D r. E A '• Of
3 M F L £ # i
+   RUM*    1 3 r'
START
SEP  Z'j,  1991   i I : i 5 : 0 f,
                                                                                                I . 5 3
     9. 225
     10.333
          STOP
                                                                                               1 -t . «
                                                                                              ._l5.5Z
-------
»' » ' •* . >j t
M«TKY CONS
E'iTQ-hRcM
F.T T
. 5'3 1
. 5 2 b
, €20
. / O i
1.034
1.536
2 , 3 Q 3
2.566
2.79 2
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6.293
3 Ji c. *"•
1 0 . "j 3 3
i 1 . 2 .J 7
14,284
15,526
16, 555
2. 0 ,961
V r U C T '

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F £
Bk
S 6
0 D
S &
a &
PS
£-5
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F&
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66
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5254
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t>l E T H H H E
BUTAKE

PEH TAME
BENZENE
H E X ft N E

TOLUENE

ETHYLBEN^EHE
o-XVLEHE
TOTAL  A R E H = 893524
NUL F«CTOR=i,aaewE+oi
F: UN  P A R H 14 E T E R S
ZERO
M T T 2 "' =•
C H T S P =
AF: F;EJ =
THR5H
F K bl D =
y
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56 o
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0.34
-------
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> U j c  o R E ri f-  0 r  '1 0 H T R 0 L - >'  T 0  t H D .-
 n M 0 P L t  # -3
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     14.£5 1

     15.112
     13.595
-------
           TIMETHBLE  STOP
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                           -5 E P  2 5 ,   1991    I 1  : 4 * : Z i
M H f H <  C 0!! '9 T F, U C T I u H
E S T D - h R E H
        R T  T Y P E
WIDTH       HEIGHT  C M L It C 0 H C .          H M M E
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1
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TOTML  AREA=  553035
M Ij L  F A C T 0 F: = I . y e B 9 E + M
fiUU PARHMETER.S
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C H T i P  =   1.9
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nrlEn        uitOTH

6274            ,  ij  i7
                                                                                                                 H  £ I  G h T    C M  L i*    C 0 \\  L .
B D
r 5
V B
f ' B
B B
B D
V B
F6
3 o »Ji *J •;«
1 17^42
i94 1 2
f . i v r 4
7 5 ? 0 •?
- jj "^ C "'
1 4 1 '.j I 1
ir~50
, y « 4
. .}*•?
.120
, 24i
.277
.581
. n 1 v
.433
22303
2 i 3 3 5
J L 'j 1
5519
4371
553
3S2*
-• a" ^ -^
                                                                                                                                          i  y
                                                                                                                                                                                            tin HE
                                                                                                                                                                                            M E 7 H H N  E
                                                                                                                                                                          .  i 3 5        HE X M H t
                                                                                                                                                                      £  .  450
                                                                                                                                                                          ,  67 0
                                                                                                                                                                      4  ,  5  j  1
                                                                                                                                                                          .259        o-XYLEUE
T 0  T  »i  L    hi r. E rt =    -j  1  T 2 '? ~
M U L     F H C T i j F: =  1  .  Ci  © 0  0 E * 0
F; UN     ?  A F: h in E 7 E
t E F: 0           =       e
C H T     b  P     =       1  .  0
A R     R E J     =       5 y &
T H F.  S  H       =       A
P K     U D       =       U  . a  4
-------
                                                                                     -M
                                                                                  1 4 . i 3
                                                                                 —1 5• 339
STOP
-------
E



' i 7 D - ^ F, E f
RT
') . i. 4 J,
i 5 . 3 3 '3
1 * . ij 4 i
< ; . r •« '_ . i v n
i
7 Y r E M r! E M
B B 1 '5 3 i o a
SB i j i 3 5
B B i 4 v -3 j i

M \ D T H
, ii'5
. 3 3 1
.531

HEIGHT
i 4 r> 9 4
5 1 3
1 4 3 3 0
                                                                                                            C r^  L «   C 0 H U
                                                                                                                                       I  . Q i 4      o E N Z £ H E
                                                                                                                                         . 3 2 '5
                                                                                                                                       i  . i 4*3      E TriV LBE
T  u T n L   n F, E H =   4 "t  3 3 a. 5
14  U L   F ri C  7 0 F. = 1 .  3 -i 0 U E + 3 0
F- IJ H   r M F, fi M E  i  £ F '.a
i E F, 0         *      9
r. T T   e."    =    - i
C n T   3 r    =      I  . 0
^ K    F. E j    =      5QQ
T H F. s H      =      4
P K    U D      =      8 .  a •»
-------
     R U h   «     ill
                                3 £ F
            i T 0 F
RUN*       1 i i
                                   :stf  z. j :
    T H V   C 0 H S T R lj C T I 0 H
           R T   T Y p £
         505       BB
            WIDTH
3 6 .3 9 5      .056
HEIGHT  C ft L»  C 0H C.             NAME
  10 S 93      L               .9 5 0    METHANE
T 0 T K L   M R E fi "    3 13 o S 5
M U L  F H C T g F: = I . o 6 fj 0 E - y 0
RUM  PARAMETERS
ZERO      =     Q
H T T  a *  =   - 2
C H T  3 F  =     1.0
MR   F:£ J  =     5y Q
THF.SH    =     4
F R   bl 0    =     0.0-1
-------
   L i i
-t-P-
                                                                                       ii.ir a
                                                                                       11.796
                                                                                       12.1d3
                                                                                       ^1 * 3 o 8
                                                                                      1 4. i
                                                                                      id.5i5
                                                                                      24. M 16
-------
R U H *
W H T K f    C 0 rt S T R U C 7  I U K
                                                      -: c, r     ,_ -j
                                                                              -"t J  I
                                                      -i R E H      WIDTH
                                                                     HEIGHT    C H L *   C 0HC.
                                                                                                                                                                 H M PI E

C.


I
\
2
i
4
4
=,
*
-
O
V
1 u
1 l
1 i
1 2
i 2
1 5
1 D
l y
23
24
. D -J c
r5T.T^>

. d (i 5
.325
. "5 *i 5
. 555
,777
. 1 3 9
. 5 5 3
. 2 7 ."5
.274
. 9 5 iS
. o 7 b-
, 1 7ii
, 3 o 2
,172
. 73o
.123
. i' 3 3
. 70 i
, 372
. 57-S
e -i e
.416
PB
SB
BB
S3
6S
BB
F'6
E&
66
ee
6B
PB
BB
P&
SB
VB
BB
BB
65
PB
BB
PB
BB
P6
68
i i33ii
4701
42713
•? 5 4 L 9
? 3 5 -3 5
15S12
s0127
2 1 •> 7 7
1 a i 0 7
1 "5 4 1 6
.' b U 6
74997
24392
7 b -j ^
43433
63203
9 2 2 3 6
7 i 4
4 9 3 4
2 Q J 2 4
3240
9 2 9
1706
1 2 -3 9
1 % 3 9
, '112 5
.317
, U 7 0
, 0 9 I
.875
. 0 9 i
.113
. lib'
,223
.247
. 100
, 234
,194
.14^
. ,320
. 2 3 3
. 2 ,' 9
. 1 65
. 199
,196
,157
,034
, 95 1
. S 9 3
. 830
i a 6 o i i
4545
1017- 2
i 7 "t i 4
2 0 (j 3 4
2 3 5 1
4249
j 093 4
754
9ijii
1 262
4395 5
2093
370
2261 7
4525 6
5504
72
4 1 4
1725
345
461 9
552
229 10
227
.414 .MET'riHME -rtf^
.152* "'
. 6 "i r ET H nflE
j , 176
3 ,019
.501
. ;-.-2
. 1 7 i B U T H H E
.325
. 4 "i 3
, 245
,475 R E H T A H E
,737
, 24b
,224 6EN2EHE
.347 H E X A H E
2.977
.823
.159
. o 56
. 105
.004 ETHYL6EN2EHE
. 85-5
. & Q 5 o - X V L E H E
.035
T 0 T  ri L    AREA-    t> 9 4  3 a 5
M U L    F A  C T rj R = i  . y 9 0 0 E + U 8
RUN    PARAMETERS
ZERO         =      t)
ATT    2~   =    - £
C H T    S F
H R   ft E J
THR3H
PK   UID
1  .  &
500
                           0.84
-------

             STOP-
R U M *
Mn i  KV  CON
E '2 i  D - M r. E ri
           F, T   T V ? E
                                     1 i 4
                                   3 S 6 3
LSIQTH
  .Oil
  .  'Il b u
HEIGHT   C H L *  C 0 K t ,             ri n m c.
    17 o ?                        .937
  i -3 8 I'?       1                . 9 9 9    H £ I H M rl E
 1 0 T PI L  ri ?: E H =    -39327
 IU L  F H C T 0 F- = i . a u v] y E •» 0 0
RUM  P A F; A H E T E R S
Z E "f- 0      =    d
fiTT  2'"   =   -2
CHT  SP   =    1.6
MR  P.EJ   =    58i
T H R S H    =    3
P K  U 0    =    9 , -3 4
-------
    r. !„• f4  «   ; 1 J       S £ r  i 5 •  I • i 1    1 -I : ; ; : 5 1
         STOP
R U H ft    114
                                                      <**""'*'
H ri T H Y  0 0 N 5 T ?. U C 7 I 0
       FT  T V F E
      030    6 B
      526    B B
      r 31.  i B F
  H R E H  WIDTH
  Jo5 4    .316
 5 e60 I    ,056
1 1S r 6 5    ,165
HEIGHT C H L « C, 0 H C .
  '2.7 i-3
 lOS9e    1          .942  MET
 1 t 0 0 5             3 , d 3 3
H U L " F ri C T 0 F. = 1 . 6 Q Q fl t + 8 6
RUM  F- H R A M E T E r. S
ZERO    =   0
H i J  C.  =  — ^
C H 7  S r =   i , 0
H R  R E j =   sea
T H R S H  =   3
F K  U 0  =   0 . 3 -(
-------
  ft U N *   I ! 5
                     v.o(r
                                                           TH=
       STOP
                                                                      11. £ '3
                                                                      14.2 9 3
                                                                      15. -I-M
                                                                      1 6.9 Tl
                                                                      21.39 o
RUN*   115
                  SEP 25. 1991   14:£3«3Q
FlriTHY COH3T RUCTION
-------
                             b £
                             F E
                                                                                                                                          1  . .3 >4

 i  u I h L    H R E M -      1 i ~* i
M  U L    F n C T 0 F = i  ,  0 3 y u E + 0 0
F, U H    F .i F, rt M t  T E r. i
Z E f,  "j         =      U
CHT   SF   =
M R    F: E  J   =
T H F; s H
F V,    lu 0      =
                           1 .  0
                           u  .  CM
-------
 ;-•"'   iri  $rfi!i 1>fl
f.Z
                   ., ; ij -t
                                                              1 i , 2 0 3
                                                              1 £ . 4 i 3
                                                              12.361
                                                              1 j . £ 3 3
                                                             — 15.9 1 7

                                                             .._! 6.451
                                                              i a, 5 ? o
                                                              d u . 5 y
                                                              i£.535
-------
F. U K *
                   E T H 8 i- E
                                                             ! -J4 : 46
 1 H T K .'  C 0 H 'j T ft U C T 1 0 N











1
1
1
1
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F:T 1
504
•3 J 7
332
y j -j
54 1
371
5 o 9
79 1
27,
304
2 j 7
3 9 ~
2uS
4 9 S
3ft 1
283
272
9 17
45 1
57u
590
535
' 'i r> E
F B
56
D D
BB
BB
PB
B3
63
PS
F5
56
FB
SB
BB
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68
BB
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PB
FB
BEf
PB
HfiEh
73553
•i !? 8 5 9
3 9 3 9 4
j 0 y 9 ^
1722s
5453
29641
1330 0
13520
3 8 3 6 9
1043 6
4523 3
6 9 S 6 9
1 9 S 7 6
22795
2126
34557
26 1342
4642
919
63562
1 £34
W1D
. 6
. 5
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47
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. w
. 2
2 , 2
. 6
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. ^
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3 , 4
. 0
. 0
2

H hi I"! E
« 6 METHANE
24 ETHhiKE
0 1
3 j
56
r>i
c- --
42 BUT hi HE
36
43 PEHTrtHE
54 BENZENE
43 HE X HUE
55
-32
33
6 '5
07 TOLUENE
51
1 >i ETHYLBEHZENE
3e
43 o - X Y L E N E
4 1
TuThlL   hlF;ER=   947 y 51.
I'lUL  FACTOR= 1
RUN  PARAMETERS
                 i.  a

                 3
                 6 .  94
ATT   2 "
C NT   S P
H R  R E J
THRSH
P K  U D
-------
    ; U N i   11 T I A/  = E ?  : 5 .  1 ? ? 1    i i : 4
          STOP
                                                                                           U  9.243
                                                                                              13,
                                                                                              14.30
                                                                                              1 5 . 3 5
                                                                                              :L .
R U H «     117
                        iEP  £5,  1991
[1HTHY CONSTRUCTION
-------
  j .  i - a      - a           i 3 ;3 •= 4 -J

i •;. .  i 5 o      5 B           151 j * -J

i i .  -I 5 5      V B           i -H '? 7 •?
                                                    . i ? '3
                                                  6 , i 5 4
                                                    ,355
                                                                                                        .>."-!
                                                                                                       1 . 0 j -(     c T H 't L B E ri (. £;t t
                                                                                                        • '? 3 o     o - X V l_ £ *i E
T u T H L   fi R E ft - 1 ft y 6 ? "5 £1
M'.' L   r ^ C 7 0 R = i . 6 0 0 €' E ^ 0 0
RUM   PARS METERS
ZERO       =    0
H T T   2  '   =   - i
C H T   'i P   =    1 . 6
n K   P- E J   =    -I y f i
T H R S H     =    ^
P K   U D     =   • Q . 0 -1
-------
* N G T E f n C
                                                         C ."
'<• USE  o r. E n X, 0 R  v : J h T ? 0 u - '<""  TO  END y
v I *"" C "3 i 4 , j P ** 1 !'i •• '  • j r r-i H 0 !-i R D
*   fiiJIJ »   115       SE?  25,  1-5-91   ie.'i9-'00
i T ft R T
                                                                                    IZIITII
                                                   2, r j 3
                                                                                              10.332
     1 1 , !
           "OP
RUN*
         1 i 9
                        SEP
                                  1991   16:19!B 0
Pit* THY CONSTRUCTION
ESTD-flREfl
       R T  TYPE
     ,530    BB

1
2
6
1>3
1 1
TOTn
MUL
,669
.113
.793
.317
. 332
. 950
L flfiE
FflCTO
BB
66
BB
PB
PB
PB
M= 1 ,
R= t .
AREfi
518513
1 8 8 -J 2 1 5
1491 I 3 S
2078894
2538529
2970293
1168
y IDTH
. 961
, 862
. B?4
. 154
. 269
. 235
.161
HEIGHT C«L«  COHC.         NAME
133i2£    l         16.584   METHANE
269913    2         15.389   ETHANE
334436    3         15,561   PROPANE
225472    4         1 D. lot   BUTflNE
266261    5         16,496   PENT*HE
210685    6         IS. 294   HEXftNE
    121               .038
RUM  PHRftPlETEHb
ZERO    =   8
-------
-------
CH7  if
n ft  F: E
T H R •'; H
f K  LI D
           y . 04
    L ;•
f; I U
f; £ F  ;
               5.060   HOH-REF
LEVEL
L E V E L
                       REC riL I &F:hT IOHS:  1
                       REC^L I 6RH T I Qtlb :  1
 10
  y
 i u
R 7 L V
•j . ^ I "5 i
c
U , i =j •< 1
1 . i tl 0 I
i . r 3 c i
6 . 3 0 £ 1
1 0 . "j 7 9 1
'3 . £ 3 0 1
1 -1 . £ 9 9 1
1 6 . ? e 3 i
i 0 . '9 £ 8 L
NAME
METHANE
E T H fl H E
PROPANE
BUTANE
F E H T A N E
H E X ft N E
6EHZEHE
T 0 L U E N c
ETHYLBENZENE
0 - X ¥ L E N E
SMT
L . "5 y y 0 E
9 . T* i fl £j E
I . 45iiiE
i . -i 2 e o E
1 . 4 & 0 0 E
L , 4 6 0 G E
L , 4 1 fl u E
I . a US 6 E
1 , 9 5 a y E
i . 1 4 ti a E
i . a 3 -3 e E












+ y i
-01
+ 51
+ 0 1
-y 1
+ U 1
+ 0 l
+ Ci6
+ 90
+ 00
+ 00











                                       " hi R E
                                   3 . £^
                                      5 ii
                                      0-1
                                        o j E
                                        3 5 E
                                     3 3 5 w E -
                                            OS
                                            eb
                                            @ 6
                                   4 .
                                   3.
93
Q L
                                        50E
                                        1 0 E
                                            06
                                            a -i
              OPTIONS
R F  o*'  un calibrated Raaks  .
C a 1 i b r a I i o n  fit
Disabls  POST, -run RT  update
SHMPLE  A ti T  .......... ...,.
MUL  F fl C T 0 ft
                                  3,£275E-05
                                  P
                                  NO
                                  e.oaaeE + i&a
                                  1.60QQE+90
   LIST;  TIME
   £) . a 8 8  1 H 7 C  »  =  2
   6.930  1N T G  H  =  3
   ~.ee9  STOP
-------
   APPENDIX F

ANALYTICAL DATA

 F.I   PM/Metals
 F.2   PMto/CPM
 F.3   Aldehydes
 F.4   PAH
 F.5   Sample Log
-------
APPENDIX F.I




 PM/METALS
-------
Client

Plant .
                              Run  K

                              Date 	
Sampte type
                              Technician

                              Sheet _2
                               -rt/J
                                  of
Run 0
        Sample
Sample
 Vol.
Blank
Corr.
 (ml)
 Tare
Weight
  (g)
 Final
Weight
Sample
Weight
Comments
        33
                                  o-l^flt.
 3
                                         tf,
         17
                                                          y
                                                          c
                                                                                    I
                                                                                    50
                                Method 5 Analysis Data Sheet
-------
Client

Plant .
                                    Run  ft

                                    Date 	
                                    Technician
Sample type
                ( r* i>
                                 of
Run
        Sample
       Sample
        Vol.
        (mil
Blank
Con.
 Tare
Weight
 Rnai
Weight
Sample
Weight
Comments
       , iVf
           r?
                                o.nsa
                                                a.otnD
_li
                                                O.Oo^O
       *?
       jf
                                                d.OO^t
                                               v
                                 0,2 IS"?
        33
                                                        V
                                                                   Q,o£Ha
                                                            >T^ - 0.0 MiS
                                                        y
 iv J *
                                                0.0^ s
                                                                                  EC
                                                                                  (M
                               Method  5 Analysis Data Sheet
-------
Client

Want
                                    Run  *

                                    Data
                                                  / ll'i
Sample
                                    Terfmioan

                                    Sheet     ?__ of - 2-
Run 9
Sample
 10*
Sample
 Vol.
Blank
Con.
 Tara
Weignr
 Rmri
Weight
Sampto
Weight
Comment!
        31
        5-5"
                                o».
                                              0,0111
                                                       /
       LL
                                     'C&Oaafe-
V
       t^. -k'
       A* c-t

       IS
 crc
       CLo?
 ,-C

 3
                                                      /
                                                          O-
 CrC

  1,
                 o.oooz
                          . '? C(«|
                                                      "fe
 < ' t-c

 fS
       LLiO


                                                          Q
                              Method 5 Analysia Data Sheet
-------
HMHT • Asphalt: Front  1/2
Rieulta in ug/L.
| SHI
| Umber
lPMD-010-oi.
IPI-IO oio oj«
(pi-ia-aiD-ah
|F1-10-010-D4>
|PMD ClO-IHo
IPI-ID-OID-D&I
|pi-io-oio-o7«
Ipi-io-oio-asi
1
|pi-ro-oio-09«-i«
|P1- 10-010- tQa-N
1
(Fl-IO-OID-llt-B
1
IPI-10-003-
1
Sonple
Dcicriptfon
K26 - 15,14,17 Ffl
*a
1CU>
< 6,00
N21 - 3!,32,UCul|> 20. 7
M26 - W,35,Mfc*.*|* 29,8
N26 - 47,A8.S»i_-J|- 20,2
H& - 2,3, 4 C6
N6 - 2i,2«,27*~.L
MA • C],44;4SR— I
• 14.2
• 28,0
* 21,4
NA - 40,41, 62 K—l|< 4.00

Mthed Spika
Method spikc-cLp

Method llnnk

LCS


7*5
2«7

< 6. 00

2145

Ba
I UP
180
257
140
119
19.2
14.6
29.9
M.O

9U
910

• I.OQ

1B32

Be
IUP
	
• 1.60
• 2.20
• 1.7D
• 1.10
< 1.00
< 1.00
< 1.00
< i.oo

175
47«

< 1.00

974

W
IUP
	
• I, TO
• 9. DO
12,4
18. 8
• 6.10
11,7
• 3.30
• 5,70

loud
W

< 2.00

20S3

Cr
IUP
• »7.9
403
419
111
• 15.1
• 31.0
• 12.8
• 13.5

W6
994

< 6.00

2007

Cu
IMP
' 10.4
92.0
77.4
148
< t.OO
< 4.00
t ' C,00
< 4.00

en
919

< i.OO

1926

Hn | Hi
ICW | I CAP
	
221 | 11,0
J2B | 551
376 | 399
420 | 5J.I
19,7 ]• 13:2
212 | 180
116 |- 9,70
l« |* 14.0
1
MI | 999
962 | 1302
1
3.10 |« 1,00
I
1«*2 | 2048
1
p
IC»P
*47
* 1261
* 1222
• 1MO
~i MO'
• 300
• 300
« 300

B9Z
921

< 300

1900

Pb
MS CF
32. 5
124
115
147
* i".«>
• 7.67
< 1.00
25.4

978
1020

< 3. DO

50.3

5b | Se
I CAP | 1CAP
1 	
• 37.5 |< 16,0
• 60.1 |< 14. C
• 4T.2 |< 14.0
* IB. 3 |< 16.0
• 54.4 |* 16:0
• 56.2 |c 16. 0
- «B.2 |< 16.0
• 40. 2 |< 16.0
1
loot | 790
1001 | 996
1
< 15.0 |« 16.0
i
2185 | 2121
1
Tl
IMP
« 100
< 100
< 100
< 100
< 100
< 100
< 100
< • 100

1DZJ
1002

' 100

1970

In
iew>
278
997
1073
1265
" B67V
95.2
61.5
140

1014
1014

24.1

2105

Us
MS GF
64.3
93-B
80.6
ioa
<- 4-00-
< 4,00
< 4.00
« 4.00

874
954

< 4. DO

45.7

• less than S  tines  the dercccioi Unit.
-------
Table 2.
MTHT - Atpfialt.  Front  1/2
Btiulla in lolsl  ug.
| SAM | Sao?U
| nutter | Description
I 	 " 	 I 	
|Pl-IO-OIO-01a | N26 - )S, 14,17". ',
1P1-IO 010 02« | «J4 • 31,32,3)1 >
|PI-1D-010-03a | «6 • 14,15,34 '
|PMO-D10-04a | NZ4 * 47,60,49 -j
|P1-lO-010-Oio | M - 2,5,* ", 1-,
JP1-10-OIO-06* | N4 • 25,24.2*. «
|JM-10-OIO-07« J H6 - 41,44,45 •
|PI-lO"Q10-0«a | H6 - 60,41,62 '•
1 1
|P1-10-alO-09«-N| Method ipikt
|P1-IO-010-10a-N| HBihod Spike-dtp
1 1
|P1-10-010-Ha-aj Method 3 look
I I
|P1-10-001- | LCS
1 1
Ag f fl»
ICAP | 1CA>>
	 1 	
< 1,50 | 45.0
• 5.18 | 64.3
• 7.45 | 40.0
• 5.05 | 79.8
• '4.05 | 4.80
• 7.00 | 9.15
• 5.J5 | 7.tB
< 1.50 | 9.50
1
74.5XJ 91.41
24.7XJ 91.01
!
< 0.600 |* 0.100
I
107S| 91.41
i
ICAP

- D.40C
• 0,550
• 0.425
• 0.275
< 0,250
< 0.250
« 0.250
< 0,250

95 -W
«.n

* 0.100

97. 4X

Cd | Cr
1C*P | IMP
I
	
• LIB [• 24-5
• 2.25 |' 101
3.10 | 105
4.70 | 27.8
• 1.58 )• J.7B
2.93 (• 7.75
• 0.83 |- 3.20
• 1.43 |- J.M
i
KMTI| 99.&I
99,n| 99.41
1
< 0.200 |< 0,400
!
104X| 1001
1
Cu
1C«P

• £.40
21.0
19,4
37,0
< 1.00
< '1,00
< 1.00
« 1.00

93.5*
91.91

- o.;oo

W.4X

Nn
ICIP

55, J
42,0
94,0
IDS
4.91
58.0
2V, 0
41,5

96.11
96. a

• o.uo

97. IX

Hi | P
IC*I | ICAP
i ...
	 1 	
15,3 I' 112
133 )• US
W,3 |- 10*
13,1 |- 3M
• 3,30 |< 75.0
45,0 |< 75,0
• J,«J |< 75,0
• 1.50 |« 75.0
1
99,H| B9.21
1COX| 92.11
1
f 0.300 ]• 30,0
1
102*1 99.0X
1
Pb | Sb | Se
MS GF | ICAP | ICAP
...„. 	 j !....'.»-
	 1 	 1 	
8.11 |* 9.38 |- 4.00
31.0 |* 1S.1 |i 4.00
28.3 1* 11.8 |< 4.00
V..8 |* 9.58 |< 4,00
• 1'.7*'|« 13,4 |« 4.00
• 1.92 [• 14.1 |« 4.00
« 0.750 |« 12.1 |« 4.00
4.35 |- 12.1 1< 4.00
1 1
97.8X) 100X| 99. OX
102X| !OOI| W. Kt
\ 1
< 0.300 |< 1.50 \< 1,60
1 1
101X| 109X| 1041
1 i
Tl | Zn
ICAP | ICAP
	 i 	 	 	
	 1
t 25.0 | 49.5
< 25.0 | 249
< 25.0 | 268
< 2S.O | 314
e 25.0 j 21.4
c 25,0 | 23. S
< ,25,0 |- J5.4
< 25,0 | 15.0
1
I02*| 1031
100X| 104»
1
« 10.0 |* 2,41
1
98.5X| I05X
1
As
US CF

14.1
23.5
20.2
27.0
< 1.00
< 1.00
< 1.00
i 1.00

87.4X
95. 4X

< 0.40

91. 4X

Final
Volume
, . . , . —
	

0.250
0,250
0,250
0.250
0.250
0.250
0,250
0.250

0.100
0.100

0,100

54.0

  less than 5 lines cho detection
MLCUIA.TIMIS;
              Sarqile Result (oa/L) I Final Volute (1) « lolol ua
                                                                                                                                                                                                                                    t  b
-------
MIHT - «sphnli:
BHUlie in ug/L.
| Umber
	
|pl-10-010-16a
|p1-10-010-17a
Pl-10-OlO-IBa
Pl-10>010-19a
PI 10 010-12=
Pl-10-010-13a
PMO-010-Ua
P1-10-010-1S«,
PI 10-010 20..M
P1-10-Q10-21B H
P1-10-Q10-22a-B
P1-1Q-QIO-

Baek 1/2
Saiple
Description
	
M - 1
H6 - 24
"*'«
Ha * 59
«26 - It
N26 - 10
M2ft • 37
«6 - «
Marhmd Spike
Method Spike 1*4)
He c hod Blink
LCS


1

•
<
c
«
<
<
*
«


< I



>g
CAP

.30
.00
.00
.00
,00
.90
.00
.00
410
104
.00
145


Ba |
IUP | I
	
9-10 |<
7.BD |<
too |<
13.5 [<
< 1.00 |<
12.5 |<
15.B |«
12. & |<
i
1
882 |
i
1
* 1.00 |«
1832 |
1

Be
CAP

.00
.00
.00
.00
.00
.00
.00
.00

447
.00
974


Cd
(CAP
	
< 2.00
* Z.70
96.0
• 6.66
< 2.00
• 2.40
• 6. BO
• 2.00
985
BBS
< 2.00
20BJ


Cr
[CAP

• 7.30
• 17.9
104
12.2
< 6.00
• 11.9
• 29.2
• 12.4
970
U5
< 6.00
2007


Cu
IMP

< 4.00
59.6
1876
54.3
< 4.00
•^ 10.1
27.5
< 4.90
901
793
< 4.00
1923


m
IUP

n.l
26,9
384
11.8
* 4.00
17.4
216
19.1
940
B49
22.4
1942


Hi
1CAP

- e,w
20.8
290
16.4
• 3.30
24.5
4t.i
17,4
aei
985
• 5.40
2048


P
ICtP

' 698
565
IBIS
• 697
• 449
* 414
495
• 642
782
B6S
< 300
1980


Pb
AAS CF

• 1.34
• B.4S
280
IS.fl
< 3.00
• l.JA
11 -J
• 9.21
886
988
• 7.02
ts.o


Sb
(CAP

< 15.0
< 15.0
< 15.0
< 15-0
4 15. 0
i 15.0
< 15.0
i 15.0
B68
96B
• 15,0
2185


Se
IUP

< 16.0
t 16.0
< 16.0
< 16.0
< 16,0
< 16.0
f 16,0
< 16.0
853
958
< 16.0
2121


U
IC*P

< 100
< 100
< 100
< 100
< 100
< too
i 100
< ' 100
947
975
< 100
1970


Zn
I«P

20,2
154
2326
127
< 15.0
136
231
55.5
907
1010
* 15.0
2105


19
AAS GF

< 4.00
< 4. CO
• 10.4
< .00
< .00
* .00
* .00
< .00
840
978
< 4.00
44.0

* less than 5 dimes the detection limit.
-------
Table Z.
MINT
Resulti In local
Back 1/2
"9-
[ SMI
| Hunter
1 '
|PI-IO-010-16«
|PI-lO-OlC-17a
{PI-ID-OlO'lte
|P1-10-010-19l
|Pl-10-010-12a
|P1 10 010 13»
|Pl-10-D10-Ua
|pi-io-oTo-iSa
1
|pi-to-oio-2o*.M
|PI-IO-010-21«-H
I
|P1 10-010 22« B
1
IPI-IO-OIO-
I
Saople
Description
*• 1 PI
H6 - » K-- »•
HA • 42 *— 1
tt - S9 1., J
N26 - U f^
•26 - JO H— 1
M26 - 17 t-- T-
H26 - 46? -" 5

derliod Spik«
Method Spike-dup

Method Blink

LCS

*g
ICAP
• 0.700
< 0,«7
< 0,413
< 0.631
< 0.671
< 0.614
< 0.631
< 0.631

41.01
JO 41

< 0.616

1071

BB
ICAP
1 01
0.815
10.5
1.42
< 0.112
1.3Z
1.66
1.11

flfl.K
7e.4«

• 0.106

91 .6X

Be
IUP
< 0.111
< 0,104
•< 0,105
< 0.105
< 0.112
< 0.106
< 0.105
« 0.105

83. 41
93. rt

< 0.106

97.41

Cd
ICAP
* a. 222
• 0.202
10.1
• 0,700
< 0 224
' O.Z54
• 0,716
< 0,210

«8,SX
M.5X

« 0.212

104X

Cr
IUP
. .*.....
	
* 0.811
• 1.07
11.0
1.29
< 0.671
* 1.24
• 1.07
• 1 .30

97. n
84.51

< 0.&3A

1001

cu
IUP
* 0.444
6.2}
198
S,«
< O.U7
• 1,07
' 2.8?
< 0,421

90,11
7V.W

< 0.424

96.41

Nn
IUP
1.25
2.B1
40.5
3.14
" 0,447
1.B4
24 .8
2.01

94.01
84.91

Z.17

97.11

Ni j P | Pb
[CAP 1 1C1P | MS GF
II
	 1 	
• 0.955 I* 77.5 |- 0,373
2,17 |* 5».0 |' O.BB6
JO. 8 | 191 [ 29. S
1,72 |* 73.1 | 1.66
• O.JM |" 50.2 |« 0.115
2.5» |* 64.9 |« 0.155
4.M |- 73,1 | 1.50
2,04 |- 67.5 |* 0.969
1 1
aa.itj 7s.2i| M «
9fl.5I| B6.II) 98, Kl
1 1
• O.S7Z )« 31.8 |«. 0.7U
I 1
102I| 99.01) W-01
1 1
Sb
l»p
< 1.67
* 1.57
< 1.58
< 1,58
< ran
« 1.59
< 1.58
< 1.58

B4.BI
M.BI

< 1,59

1091

Se
ICAP
. . . . . 	
< 1.7B
i 1.67
< 1.69
< 1.U
— r.fr
< 1.6V
< 1.68
< 1.&B

85. IX
9S.8X

< 1.70

1061

Tl
ICAP
« 11,1
< 10,4
< 10.5
« 10.5
< 11.2
< 10.6
« 10.5
< 10.5

94.71
97.51

« 10.6

96,51

In
(CAP
I...... 	
|* 2.24
16.1
2(5
13.4
< i:«r
14.4
24.1
• 5.64

DO.Tt
101X

< 1.59

1051

AS
AAS CF
< 0.444
i 0,418
• 1.10
< 0.421
< o:w
< 0.421
< 0.421
< 0.421

B6.0I
97. HI

: 0.424

1071

Finat
valunc
0,100
0.100
0.100
0.100
"0.100
o.ioo
0.100
0.100

0.100
O.IOO

0.100



Initial
Volune
0.5030
1.1615
0.9605
1.0191
•o:i75!"i
0.9246
1.0069
1.0161

O.IOO
0.100

O.BB34



bigesled
Volune
	 . . 	
0.4510
1.1115
0.9105
0.9691
OTtSS
0.8746
0.9569
0.9661

0.100
0.100

0.8114



• less than 5 [(
                    the detection Unit,
CALCULATIONS;
              Soiplt Result  (ug/L)  V  final Volun  (L) X  Initial Voluac / Digested Volune " lotal
-------
APPENDIX F.2




  PM10/CPM
-------
Client

Plant .
                                     Run  #

                                     Date 	

                                     Technician
                                                  T
Sample type
f
       f*
                      V-VW-S  (/? <
                                     Sheet
                                              '
                                                   n.
Run
        Sample
        Sample
         Vol.
         SmU
            Blank
            Corr.
             (ml)
                                   Tare
                                 Weight
 Final
Weight
  tg)
Sample
Weight
  (g)
Comments
                                         0,3591
                                                 .OC10
a-
                                 0,213-?
       /
  3
                          .3
                                                 0,00%
  B
                                 &.3IS3
                                                               M
                                                     \\ /M
                                                                                    i
                                                                                    a
                                Method 5 Analysis Data Sheet
-------
Client

Plant ,

Sample type
                                              Run   *

                                              Date
                        /'.5T
                              Technician

                              Sheet
                                                     Of
Run n
Samole
  100
Sample
 Vol.
 (ml)
                           Blank
                           Corr.
 Tare
Weight
 Final
Weight
  (9)
Sample
Weight
  (g)
Comments
                                                               T>^
                                                                  o.o
                                                 0,0
J
 fS
                                  **$",% "70
                                                               2,<.t,«.n --••3  "   Y
crc
       LLo?
                                  /c '
                          Q.cooi.
                                                  0,
                                                   /
                          0. OOQ 2
                                  1 2 . ^ C»<»
                                                                      O, o 2. » <*
 <-' r r
                            fefiSS:
                             H«
                                                                          -i-rt t\
                                  ti-j, tjji??^
                                                  O.
                                Method 5 Analysis Data Sheet
-------
                                            Run
Client

Warn .
Sample type  ?'W5
                         +
                             Technician

                             Sheat_
Run f
       Sample
         ID*
Sample
 Vol.
Blank
Corr.
 (ml)
 Tare
Weight
 Final
Weight
Sample
Weight
  (g)
Comments
  i
                                                        /
                                                               O-OOMO
H-jO

  1
                                          ,05- JS
                                                                Oi-f'
                                                                  a. oo to
                                                                                 f 0,
         .
        7?
       LLol
                                                       y
                                                                 1^,,-
 3
                                               0.00^5
                                                       J
                                                                                 > a.
  3
        7?
                        0 . 00 (i
                                               5,03^*
                                                                                  4
        p
                                f^.'ffCI
                                    f C~
                                                                   X \0
                                                                  , i^-tL d
                                        l~i
                               Method 5 Analysis Data Sheet
-------
APPENDIX F.3




ALDEHYDES
-------
             Radian Uork Order PI-10-001

                  Analytical Report
                      12/16/91
              EMB
              EHB
              Radian Corporation
              RTP( NC

              Larry Banesburg
Customer Work Identification EHH Asphalt Teat Site 26
   Purchase Order Nuifcer 275-026-48-17
                      Contents:

             1     Analytical Data Surmary
             2     Sample History
             3     Comnents Sinmary
             4     Notes and Definitions
             Radian Analytical Services
             900 Perimeter Park
             Horrisville, NC  27560
             919-481-0212

        Client Services Coordinator; LJROHESBURG
           Certified by.-
-------
                                          Analytical  Data  Suimary
Page:  3

EMB
Radian Work Order: P,1-10-001


-

Met hod: Aldehydes, Mod T011, HPLC (1)
LiscCcnpendiUD Method TO- 11
Sample ID: M26-0922-ALD—
FB (1C, PR)
Factor: 10
Results in: Total ug
OU
Matrix: Stack


K26-WZ3-ALD--
1 (1C, PR)
10
Total us
02A
Slack


N26-092J-ALD--
2 (1C, PS)
10
Total ug
03*
Stack


MZ6-0924-ALD--
3 UC. PR)
10
Total ug
04A
Stack

Ace t aldehyde
Acetone
Acetophenone/o-Tolualdehyde
Acrolein
Beni aldehyde
Butyraldehyde/Isobutyraldehyde
Crotonaldehyde
2,5-Dimethylbenzaldehyde
Formaldehyde
Hexanal
Isophorone
1 sova I era Ldehyde
HIBK/p-Tolualdehyde
Methyl Ethyl Ketone
Propionaldehyde
Quinone
m-Tolualdehyde
Valeraldehyde


Result Det, Limit
'•••'•'••'^••'4'w^y^
ND
396
MD
ND
ND 2T«»|I'
S:iii:;K:«;:»-
ND Kill
ND
:Wft.XWSW
ND
14.5 • Pill
ND iftttt
MD .1*111
ND lillll
ND lill
ND
ND lllll
ND
ND
ND lilll


Result Det. Limit
3530 11B -
2180 148 -
ND 23
107 11
86.4 2,1
464 is :
109 18 -
ND 24 •
2070 m
190 20
ND 11
75.1 • 1ft
ND 25
36,9 • JI
241 14
122 14
NO 23 ••
89.1 • 18' *


Result Det, Limit
1220 ilolll
2280 ilSlli
ND ZJlif
NO lllll
65.3 • iilli
253 1:8111
48.1 • lilil
NO
2100 iilll
136 atflll
5W5SftlW:r:
MD 1B?;;ii
::::«"vft::'-.v:v:
ND mm
ND afiii
NO lllli
105
155 ia?»
«D siiii
62.9 • lilll


Result Det, Limit
5830 ZTOll
2280 JWlll
«D 23|1|
MD llil!
757
633 lllll
561
"°
11800 22Cli
519
ND iia:i|l
138 iail-1
MD alii
BO iaiS
759 l^:!:;ii
Bi a msm
ND ZS|1|
344 lllll

ND Not detected at specified detection limit                    • Ear. result less than 5 times detection limit




(1) For a detailed description of flags end technical terms In this report refer to Appendix A in this report.
-------

im
Kadi an Work Order:
P1-10-Q01

Analytical Data Summary
Page: 9
Method: Aldehydes, Mod T011, HPLC <1J
List Compendium Method TO- 11






Sairple ID: M26-M25-ALD- • METHOD BLANK METHOD SPIKE Calibration
4 (1C
Factor: 10
Results in: Total
05A
Matrix: Stack
, WJ)
.56
ug Total
06A
DNPH
Check OC
1 1
ug X Z
07A 20A
DNPH ACN







Aceta Idehyde
Acetone

Acetophenone/o-Tolua Idehyde
Acrolein
Benzaldehyde
Butyra Idehyde/ 1 sobuty ra Idehyde
Crocona Idehyde
2,5-Dimethylbenialdehyde
Formaldehyde
Hexanal
Isophorone
I sova I era Idehyde
M I BK/p-Tolua Idehyde
Methyl Ethyl Ketone
Propiona Idehyde
Ouinone
Ffl*Tolualdehyde
Va I era Idehyde
Result
2560
2710

ND
134
135
Det. Limit
110
tt«

21
11 •
21
237 1« '
102 18 i
ND
3050
200
ND
85.3 *
ND
ND
181
344
ND
134

24
69
20
18
16
23
1*
14
1B
21
1*
Result
NO
2.74 «

ND
ND
ND
ND
ND
ND
1.24 •
NO
ND
ND
ND
ND
ND
NO
ND
NO

ND Not detected at specified detection limit
Q Outside control limits
NS Not spiked
(1) For a detailed description of flags


and technical terms In
Det. Limit

mmm

.t£2$£$
1111
ifiii
1*111
Still

ifisitSsi?


(JSfSiii
SlaPli
W&m

mm
ilpll
mtim
Result Oet. Limit
90 lllll
83

70 Q '&&£&'????
23 Q
lit lllll
NA
25 0
•85 Hil
87 »§«wHs
117
91
MS
106
«* ill!
107 sftmm
64 Q liifi
93
82 lllll
Result Det
115
NS

NS
NS
NS
103
NS
NS
105
NS
NS
NS
NS
NS
165 Q
NS
NS
NS

* Est. result less than 5 tines detection limit
HA Not analyzed

this report refer to Appendix A in this report.
. Limit
!!:£w®;-:i


SSiJiiBSs:
Illii

lllll!
Hill

'iSS*:>wJ

'•;|!|:|;;J!l
••"•• ;••;».*

'i-'yt'i-i-ry ; •:•;•;•:;


:*;lliti
•>:'y '•'•'&'•$''•$!$'






-------
                                       SanpLe History
Page:15
EMB
Radian Work Orders P1-10-001

Sample Identifications and Date*
Sanple 10 H26-092Z-ALD-- H26-0923-ALD-- H26-0923-ALD-- NZ6-0924-M.D-- H26-0925-ALD-- METHOD BLANK
FB (1C, PR) 1 (1C, PR) 2 (1C, PR) 3 (1C, PR) < (1C, PR)
Date Sanpled 09/22/91 09/23/91 09/23/91 09/24/91 09/25/91
Date Received 10/01/91 10/01/91 10/01/91 10/01/91 10/01/91 10/01/91
Matrix Stack Stack Stack Stack Stack ONPN
01 02 03 04 05 06

Aldehydes, Mod T011, HPLC
Prepared
Analyzed
Analyst
File ID
Blank ID
Instrument
Report as


10/08/91
10/18/91
IKK
OWEN 130
OUEN129
V5000
received


10/08/91
10/19/91
LKK
OWEN131/179
OWEN 129
VSOOO
received


10/08/91
10/19/91
LKK
OUEN132/17B
OWEN 129
VSOOO
received


10/08/91
10/19/91
LKK
OWEN133/177
OWEN 129
VSOOO
received


10/08/91
10/19/91
LKK
OUEN 134/1 76
OWEN 129
VSOOO
received


10/08/91
10/18/91
LKK
OWN 129
OWEN 129
VSOOO
received
-------
           Append IK A





Conmenrs, Notes and D«fInitfons
-------
EMB
Radian Work Order: P1-10-OT1
                                       Report Coronents and Narrative
                                                                                                                   Page: K-2
     General  Comnents
     05-A;   The XAD-2/Filter portion of the sanples was lost during
      preparation.
     NO = Not quantitated.
     PAH sanfjies were diluted because of hiflh hydrocarbon content.
-------
                                       Notes and Definitions                                                       Page: A-3
EMS
Radian Work Order; P1-10-001
J   Indicates an estimated value for GC/MS data.  This flag is used either
    when estimating a concentration for tentatively identified compounds
    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 quantisation 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 the right of
    the < syntool is the method specified detection limit for the sample.

MS  This analyte or surrogate was not added ( spiked) to the sanf>Le for
    this analysis.

D   This quality control standard is outside method or laboratory spec-
    ified control limits.  This flag is applied to matrix spike, analy-
    tical QC spike, and surrogate recoveries; and to RPOCrelative percent
    difference) values for duplicate analyses and matrix spike/matrix
    spike duplicate result.

*   The asterisk(*j 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:  P1-10-001
                                                                                                                  Page: A-4
    TERMS USED IN THIS REPORT:
    Analyte -  A chemical for which B sanple is to be analyzed,
    EPA method and QC specifications,
The analysis uill  meet
    Conpound -  See Analyte.

    Detection Limit - The method specified detection limit,  which is  the lower  limit  of
    quantisation specified by EPA for a method.  Radian staff  regularly assess  their
    laboratories'  method detection limits to verify that they  meet or are lower than  those
    specified by EPA.  Detection limits which are higher than  method  limits  are based
    on experimental values at the 99X confidence level.  The detection limits for  EPA CLP
    (Contract Laboratory Program) methods are CROLs (contract  required quantitat ion
    limits) for organics and CRDLs (contract required detection limits) for  inorganics.
    Mote,  the detection limit may 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 QC tests in eonformance 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 sanple specific detection limits based on alternate
    matrices (soil or water), reporting units, use of cleanup  procedures, or dilution of extracts/
    digestates.  For example, extraction or digestion of 10 grams of  soil in contrast
    to 1 liter of water uill result in a factor of 100.

    Matrix - The sample material.  Generally, it will be soil, uater, air, oil, or solid
    waste.
    Radian Work Order - The unique Radian identification code assigned to the samples reported in
    the analytical  sumary.	
    Units •  ug/L     microgratns per liter (parts per biIIion);liquids/water
            ug/kg    micrograns per kilograa (parts per billion); soils/solids
            ug/H3    microgrsBS per cubic meter; air sonnies
            mg/L     milligrams per liter (parts per mil I ion);liquids/water
            mg/kg    mi 11 i grams per Icilograa (parts per mi U ion);soi Is/solids
            X        percent; usually used for percent recovery of QC standards
            uS/cm    conductance unit,* oicroSiemans/centimeter
            nt/hr    ml Ui liters per hour; rate of settlement of matter in water
            NTU      turbidity unit; nephelometric turbidity unit
            CU       color unit; equal to 1 mg/L of chloroplatlnate salt
-------
EHB
Radian Work Order: P1-10-001
                                      Sanple History
                                                                                Page:17
            ID
     Date Sanpled
   Senile Identification and Dates

Method Spike   Calibration
               Check QC
Date Received 10/01/91 10/01/91
Matrix XAD-2/Fi ACN
19 20

70-Semi -votatil.es
Prepared
Analyzed
Analyst
File 10
Blank 10
Inscrunent
Report as
hydes, Hod T011, HPLC
Prepared
Analyzed
Analyst
File ID
Blank ID
Instrunent
Report as


10/11/91
11/05/91
RK
45B6534.TS
4586533, TI
GC/NS B
received



















10/19/91
UK
OMEN ISO

VSOOO
received




































































-------

Phenol
2-Chlorophenoi
1,4-Dichlorobenzene
N-Nitroso-di-n-propylamine
Aceiophenone
3-Meihylphenol
Indene
Cydohexane
Isophorone
1 ,2,4-TrichIorobenzene
Naphthalene
4-Chloro-3-methyIphenol
2-Meihynaphihalene
l-Meihynaphlhalene
Acetoaphthylene
Aceioaphihene
4-Nilrophenol
2,4-Diniiroioluene
Dieihylphthalate
Fluorene
N-niircrtodiphenylamine
Pentachloropheriol
Phenanthrene
Anihracene
Di-n-butylphthalate
Fluoranthene
Diphenylamine
Pyrene
Butylbenzylphihalate
Bis-(2-cthylhexyl)-phthalate
D i- n -oc typh t ha la I e

34,63



93.5
5.695
420.855



416-255

407.595
249.355
41.765
14.94






9.035
10.24

50

1

47.4






83.405
3.465
387.09



776.14

347.54
212.975
37.745
50


12.245



7.935
8.99

50.

0.625

390,355
0.66

23.97



113-565
2.745
426.24
995.545


1470.645

416.865
262-12
48.13
50


17.875



8.49
9.62

50

1

36,87
1.17
-------
     Dilution Factor
     Final Extract Volume
     Target Compounds
  9  Nitiobenzene-dS (SS)
 10  2 FluofObiphonyl (SS)

 14  Phenol
 17  2 Chlorophonol
 19  M-DtcHofOberuene
 Z5  N-Nltraao-tf-n-fHOpylamine
 32  AcelophenOM
 33
 37  IndMW
 39
 43
 49  1,2,4-TricWofotwnzww
 50  Napftihaian*
 S3  4^hlof^3^n<«hytph«ooJ
 54  2-4fcnfryeo<>
 «3  1 Motfrytnaphthatsne
 73  Aoooaprthytorw
 75  AoKvapMhene
 77  4-NJtnphmeX
 80  2.4-OMtratolMm
 81  Diomylf*tt»tat«>
 83  Fh
 97
100  PwttKhlOfOphenol
101
102
103
104  FtuoniKtam
107
DO  Pynn*
ill
114  Bb-(2-eOTytho*yf) phthalala
131  Dt-n-oety*pWhalalo
1 100 TOO
5 10 10
M-260922FB M 26 923 1 M 26 923 2 M-
304.35
462.095
341.985
NA
NA
NA
NA
NA
NA
NA
NA
2-235
NA
87.39
NA
NA
NA
NA
NA
NA
NA
5685
NA
NA
NA
NA
NA
7.9'
NA
NA
NA
NA
3.125
NA
779
1023
650
NA
NA
NA
NA
NA
NA
NA
16763
NA
NA
NA
NA
3033
2016
NA
NA
MA
HA
911
NA
NA
NA
290
NA
1654
NA
NA
NA
NA
716
NA
777
B34
590
NA
NA
NA
NA
1017
NA
NA
9731
NA
NA
NA
NA
2256
1451
NA
NA
NA
NA
112
120
NA
NA
430
75
2049
73
330
NA
NA
1069
NA
100 1
6 5
26-924-3 M26-Blank
928.2
10524
655. B
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
1502.4
NA
1983
1217.4
NA
54.6
NA
NA
43,8
54
134.4
NA
207.6
NA
1102.Z
NA
134.4
36
NA
590.4
NA
625.085
771.33
773.BB
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
037
NA
NA
NA
NA
NA
NA
NA
12.98
NA
NA
NA
NA
NA
6.34
NA
NA
NA
NA
13.02
NA
< 11111
5 55555
Spike M-6-918-FB M69191 M-6-9192 M-6-919-3 M-6-Blanh
53604
741.09
647.43
940275
941.64
477,905
520,855
NA
NA
NA
NA
NA
5M.90S
53002
999.405
1.285
1.165
NA
546.725
529.995
491. BBS
14.41
NA
NA
2C6.t7
NA
NA
10,77
NA
NA
676.415
NA
8.5
NA
491,05
729,41
566.67
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
751,275
NA
2.36
1,935
NA
NA
NA
NA
7,27
NA
0,72
NA
0.275
NA
0.405
NA
0.72
NA
NA
11,435
NA
573.825
757,145
566,49
34 S3
NA
NA
NA
93,54
5,695
420,855
NA
NA
NA
416.265
NA
407.595
249,355
41.765
1494
NA
MA
NA
MA
NA
NA
9,035
tfl.24
MA
HA
HA
1.265
0,67
47,«
0,66
478,18
642.93
568.265
NA
NA
NA
NA
83.405
3.465
38709
NA.
NA
NA
776.14
NA
34754
212.975
37.745
NA
NA
NA
12.245
NA
NA
NA
7.935
8,99
NA
NA
NA
Q,025
NA
390,359
NA
575765
794.995
614,345
23.97
NA
NA
NA
113.565
2.745
42624
995.545
NA
NA
1470.645
NA
416.865
362.12
4813
NA
NA
NA
17875
NA
NA
NA
8,49
962
NA
NA
NA
0.805
NA
36.87
1.17
445.09
67551
564.045
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
259,75
NA
0.68
0.365
NA
NA
NA
NA
22.26
0.375
NA
NA
NA
NA
11.655
NA
NA
0.605
NA
19.465
NA
-------
APPENDIX F.4



    PAH
-------
             Radian Work  Order  P1>10-001

                  Analytical  Report
                      01/13/92
              EMB
              EHB
              Radian Corporal ion
              RTF,  NC

              Larry Homesburg
Customer Uork Identification EMB Asphalt Test  Site  26
   Purchase Order Nurfaer 275-026-48-17
                      Concents:

             1     Analytical Data Surinary
             2     Sample History
             3     Corments Suimary,
             4     Notes and Definitions
             Radian Analytical Services
             900 Perimeter Park
             NorMsvilte, NC  27560
             919-481-0212

        Client Services Coordinator: UROHESBURG
           Certified
           Previously Reported on 12/16/91.
-------
       RADIAN
       COBPQBBTIOH
EHB
Radian Work  Order;
P1-10-001
                                          Analytical Data Sutnriarv
                                                                                             Page: 2

Method:SU8270-Semi-Volatiles (13
LlSE.-pAHs by SWB46 8270
Sample 10: M26-09Z2-PAH-- MZ6-0923-PAH-1 HZ6-0923-PAH-2 H26-0924-PAH-3
FB
Factor: 5 1000 1000 600
Results in: Total ug Total ug Total ug Total ug
14A ISA 16* 17A
Matrix: Acetone Stack Stack Stack


Acenaphthene
Acenaphthylene
Anthracene
BenzoC a) anthracene
Benlo(a)pyrene
Benzo(b)f Luoranthene
Benzo(g,h, i)perylene
Benzo(k)f luoramhene
Chrysene
D i benz( a, h) anthracene
Dibcnzofuran
7, 12-Dimethylbenz(a)ariihracene
Fluoranthene
Fluorene
I ndenot 1,2,3- cd )pyrene
2 -He thy I naphthalene
Naphthalene
Phenanthrene
Pyrene
1
(See next page for ret
Result Det. Limit
ND 50
ND 50
NO 50
ND 50
MD 50 '
ND 50
ND 50
ND SO •
NO SO
ND 50
ND 50
ND 100 '
ND 50
ND 50
ND 50
ND 50
87.4 • 50
NO 50
ND 50

itatively identified co»
Result Det. Limit
NO 10000
ND 10000
ND 10000
NO 10000
ND 10000
ND 10000
ND 10000
ND 10000
ND 10000
ND 10000
ND 10000
ND 20000
NO 10000
ND 10000
ND 10000
3040 J 10000
1900 J 10000
290 J 10000
ND 10000

npounds.)
Result Det. Limit
ND 10COQ
ND 10000,
75.0 J 10000:
ND 10000
ND 10000 .
ND 1001X1
ND 10COO
HD 10000*
ND 10000.
ND 10000::
ND 1000D:
ND 20000
73.0 J 10000
120 Jf 10000
ND 10000
2260 J 10000
3100 J 10000
430 J« 10000'
ND 10000


Result Det. Limit
54.6 J 6000
ND 6000
NO 6000
ND 6000
ND 6000
NO 6000
ND 6000
ND 6000
ND 6000
ND 6000
ND 6000
ND 12000
ND 6000
54.0 J 6000
ND 6000
1980 J 6000
1500 J 6000
zoa j* MOO
36.0 J 6000


 ND Not detected at specified detection  limit
 J Detected at less than detection  limit
                                            • Est, result less  than 5  times detection limit
 (1) For a detailed description of  flags end technical terms in this report refer to Appendii A in this  report.
 C2) 4-Methylphenol co-elutes with  3-methylphenol,  The
     value reported is the combined total of the 2
     cwnpounds.
-------
           • P O B • T I O I
EH6
Radian uork Order:   P1-10-Q01
                                           Analytical  Data  Summary
                                                                                 Page:  3
 Method:SU8270-Serni-Volatiles (1)
   Ust:PAHs by Syfl46 8270
 Sample ID;
 Factor:
 Results  in;

 Matrix:
M26-Q922-PAH-
FB
5
Total yg
14A
Acetone
«6-0923-PAH-1

1000
Total ug
ISA
Stack
M26-0923-PAH-2

1000
Total ug
16A
Stack
H26-0924-PAM-3

600
Total ug
17*
Stack


Surrogate Recovery(%)
2-Fluorobiphenyl
Control Limits: 30 to 115
Nilrobeniene-d5
Control Limits; 23 to 120
Terphenyl-d14
Control Limits; 18 to 137
CS*e next page for ter
Result Det. Limit

59.4

39.4

44.8

natively identified con
Result Det, Limit

132 0

102

85.1

pounds, >
Result Oet, Limit

107

102

Result Det. Limit

135 0

122 Q

90.3 | 85.8





 Q Outside control  limits
 (1) For a detailed description of flags and technical  terms in this report refer to Appendix A in this report.
 (2) 4-Methylphenol co-eluies with 3-methytphenol.   The
     value reported is the confcined total of the 2
     compounds.
-------
       RADIAN
       COBPOBBTION
                                         Analytical  Data  Summary
                                                                                             Page: u
EHB
Radian Uork Order:
Pl-10-001
HeihodrSUaZTO-Semi-Volanles (1
LiSt:PAHs by SU846 8270
Sample ID:
Factor:
Results in:

Matrix:



Acenaphthene
Acenaphthylene
Anthracene
Senzo(a)anthracene
Benzo(a)pyrene
Benzo(tOf luoranthene
Benzo(g,h, Uperytene
BenzoCk ) f luoranthene
Chrysene
0 ibenzC a, h) anthracene
Dibeniofuran
7, 12-Dimethylbenz(a)anthracene
F luoranthene
Fluorene
!ndeno( 1 ,2,3-ccDpyrene
2 -He thy I naphthalene
Naphthalene
Phenanthrene
Pyrene

)

Hethod Blank
5
Total ug
ISA
Stack

Result Det. Limit

NC 50,]>:>;.;;
ND 5CN&J
ND 5D:X' •
NO 50 \.
NO 50:
NO 50:;v: ;.,.,
ND 5'oi; ;•:,..'
ND SO-f jt.
ND 501*,'
NO 5or;_,v'
ND 50 ?-••;•;•
ND |f»^X
ND 50l::; *
ND SO1?'? ;i
NO so;** !•
NO 50 ;U 1
0.37 J 50 •:!-
ND 50;::f ;:
ND 50:;!> 1



Hethod Spike
5
X
19A
XAD-2/Fi

Result Det. Limit
S^sj:;-; :>.;.

NS . '-f:f|
NS -.'•:.':;•;
NS v:;;-;"':
NS ^'S-f
NS .a;i?
NS '*' i'. '/'•.•,•:•
'x '-:':-"' "•'• -
NS -.iifsl-:-:
NS .I:''--!;?
NS /|%
NS 119M
NS '•|i|:l
NS i;lii
NS iPP
NS |--| 1
NS •%; 1
HS ,;|l 1
NS ;;$! 1
. 135 ''S: s;










.>'•:• "'•.•",-,"
Vi%>:';-.:''-
:p"'V,

' '-:.
















	





























 ND Not detected at  specified detection limit
 NS Not spiked
                                            J Detected at  less than detection limit
 (1) For a detailed  description of flags and technical  terms  in this report refer  to Appendix A in this  report,
 (2) 4-Hethylphenol  co-elutes with 3-me thy I phenol.   The
     value reported  is  the combined total of the 2
     compounds.
-------
        RADIAN
EHB
Radian Uork  Order:  PI-10-001
                                          Analytical Data Summary
                                                                               Page:  5
 Method;SU8270-Setni-Volatiles (1)
   List:PAHs by SUB46 BZ70
 Sample ID;

 Factor:
 Results  in;

 Matrix;
Method Blank
Total ug
ISA
Stack
Method Spike

5
f.
1
-------
       RADIAN
                                          Analytical Data Suimary
EMS
Radian Uork Order;   PI-10-001
Tentatively Identified Compounds
Method; SU6270-$emi-Volatile*  (1)
  List: PAHs by SUS46 8270
Sample ID
M26-0922-PAH-FB
H26-0923-PAH-1
H26-09Z3-PHH-2
ftnalyte



Isophorone

Diechylphthalate

Di-n-butylphthalate
Result    Units  "



2.24  J*  .Total ug

5.68  J"  Total ug

7.9   J«  Total ug
Scan
                              Bis-(2-ethylheKyl)-ptichalate    3.12   J*  Total ug
                              Cyclohexane

                              1 -Mechylnaphthalene

                              Diethylphthalate

                              Df-n-butylphthalace
                              Acecopherwne

                              Cyclohexane

                              1 -Hethylnaptithalene

                              Diethylphthalate

                              Di-n-butylphthalate

                              Diphenylamine
                                16800     Total  ug

                                 2020 J*  Total  ug

                                  911 J*  Total  ug

                                 1650 J*  Total  ug

                                  716 a~  Total,  ug



                                1050   J* Total  ug

                                9730   J' Total  ug

                                U50   J* Total  ug

                                 112   J* Total  ug

                                2050   J* Total  ug

                                 330   J* Total  ug
                              8is-(2"ethylhexyl)-phth8late    1070   J* Total  ug
                                                                                      Page: 6
M26-09Z4-PAH-3
                              1-Methyinaphthatene
                                1220   J* Total ug
-------
       RADIAN
       COBPOBHTIOM
EMB
Radian Work  Order;  PI-10-001
                                          Analytical Data Summary
                                                                                     Page: 7
rentalivtLy Identified Compounds
Method:  sy8E?0-Sefni-volati les (1)
  List:  PAHs  by  Sy84& 8270
Sample ID
Method Blank
Method Spike
Analyte

Diethylphthalate

N-nitrosodiphenylamine

Di-n-butylphthalate

Diphenylamitie

iis-(2-e£hylhexyl)-phthalate



Diethylphthalate

Di-n-butylphthalate
Result    Units     Scan

  43.8 J« Total ug

 134   J* Total ug

1100   a* Total us

 134   J* Total ug

 590   J* Total ug



13.0  J"  Total ug

 6.34 J'  Total us
                              Bis-(2-ethylhe*yt)-phthalate    13.0  J*  Total ug
                             Phenol

                             2-Chlorophenol

                             1,4-Dichlorobenzene

                             M-Nitroso-di-n-propylamine

                             1,2,4-Trichlorobeniene

                             4-Chloro-3-methylphenol

                             4-NitrophenoA

                             2,4-Dinitrotolucne

                             Pentachlorophenol

                             Di-n-butylphthalate
84.8
94.2
95.6
104
109
99,9
53.0
96.4
26.6
2.15
%
X
%
%
X
%
X
X
X
X
-------
       RADIAN
                                         Analytical Data Suimary
                                                        Page: 1C
ENB
Radian Work Order:  PI-10-001
 Melhod:Tuenty TICS to be reported (1)
   List:
 Sample  ID;                         H26-Q922-PAH-
                                   FB
 Factor:                            5
 Results  in:                        Total  ug
                                   14A
 Matrix:                            XAD-2/Fi
H26-0923-PAH-1

1000
Total ug
ISA
Stack
H26-Q923-PM-2

1000
Total ug
16A
Stack
H26-Q921-PAH-3

600
Total ug
17A
Stack

Result Det . Limit
Result Oet. Limit
Result Det, Limit
Result Det. Limit

 (1)  For  a detailed description of flags and technical terms in this report  refer to Appendix A in this  report.
-------
         ommommttom
EMS
Radian Work Order:   PI-10-001
                                           ftnalycical  Data  Sunnary
                                                                                 Page:  11
 Method:Tuenty TICS to be reported (1)
   List:
 Sample ID:                          Method Blank
 Factor:
 Results  in;

 Hatrix:
Total ug
ISA
XAO-2/Fi


Result Det. Limit
Result Dec. Limit
Result Det. limit
Result Det. Limit
 (1) For a detailed description of flags and technical  terms in this report refer to Appendix A in this report.
-------
RADIAN
                           Analytical Data Surinary

EHB
Radian Uork Order: Pl-10-001

Tentatively Identified Compounds
Method: Twenty TICS to be reported CD
List:
Sample ID Analyte Result
*
M26-0922-PAH-FB
Cyclohexene NO 6
Oxygenated hydrocarbons NQ
2-Hexanol NO
Hethy Ipentenone isomers NO 8
unknown alkoxy alcohol NO
2,2,4,4-Tetramethyl-3- NQ
pentanone NQ
2,2'-Oxybis-ethanol diacetate NO B
1,3-Diethylbenzene NO
l-Ethenyl-4-ethylbenzene NO
Unknoun alcohol NO
M26-0923-PAH-1
Cyclohexene NO B
Unknown oxygenated hydrocarbon NO
Unknoun branched alkane NQ
Decane NO
Dime thy lundecanes HO
6-Methyldodecane NO
Trimethyldodecanes NO
Uni ts 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
                                                                                    Page:  1
-------
       RADIAN
                                         Analytical Data Sunroary
                                                                                    Page: 13
EMB
Radian Work Order;  Pl-10-001
Tentatively  Identified Confounds
Method:  Tuenty TICS to be reported (1)
  List:
Sample ID
M26-0923-PAH-2
 K26-OW-PAH-3
Analyte

Dimethylheptadecanes

2-Ethyl-l-Decanol



Cyelohexene

Unknown oxygenated hydrocarbon  NO

Decane

Dimethylundecane isoroers

2,3,7-Trimethyloctane

2,7,10-Trimethyldodecane

2,6,11-Trimethyldodecane

Branched  alkanes



 Cyclohenene

 
-------
       RADIAN
                                         Analytical. Data Sunroary
EMB
Radian Work Order:  P1-10-001
                                                     Page:
Tentatively  Identified Compounds
Method:  Twenty TICS to be reported (1)
  List:
Sample ID                     Analyte
Method Blank
                             Dimethylheptadecane  isomers
Result    Units     Scan

NO        Total ug
                             Cyclohexene                    NQ        Total ug

                             4-Methyl-3-penten-2-one         NO        Total ug

                             Oxygenated hydrocarbons         NQ        Total ug

                             2,2'-Oxybis-erhanol diacetate   NQ        Total ug
-------
          RADIAN
ladian Work Order: PI-10-001
                                Sample History
Page:16
Sample Identifications and Dates
Sample 10 METHOD SPIKE M26- 0922- PAN -• H26-09Z3-PAH-1 M26-Q923-PAH-2 H26-Q924-PAH-3 Method Blank
FB
Date Sampled , , 09/22/91 09/23/91 09/23/91 09/24/91
Date Received 10/01/91 10/01/91 10/01/9! 10/01/91 10/01/91 10/01/91
Matrix DNPH XAD-2/Fj Stack Stack Stack XAD-2/Fi
07 H 15 16 17 18

'0-Setni-Volatiles
Prepared
Analyzed
Analyst
File ID
Blank ID
Instrument
Report as
lydes, Mod T011, HPLC
Prepared
Analyzed
Analyst
File ID
Blank 10
Instrument
Report as
:y TICS to be reported
Prepared
Analyzed
Analyst
File ID
SUnk 10
Instrunent
Report as










09/30/91
10/04/91
LKK
UUA76
LLUA75
V50CO
received










10/11/91
11/05/91
RK
45B6539.TI
4586533. T I
GC/MS B
received









10/11/91
11/05/91
RK
45B6539.TI
45B6533.T1
GC/MS B
rece i ved


10/11/91
11/05/91
RK
45B6540.TI
45B6533.TI
GC/MS 8
received









10/11/91
11/05/91
RK
458639.11
45B633.T1
CC/MS B
received


10/11/91
11/06/91
RK
4586545. T[
4586533. T I
GC/MS 9
received









10/11/91
1^1/06/91
RK
45B6545.TI
45B6533.TI
GC/MS B
received


10/11/91
11/06/91
RK
45S6546.Tr
45B6S33.T1
GC/MS B
received









10/11/91
11/06/91
RK
i5B6546.11
4586533.11
GC/MS B
received


10/11/91
11/05/91
RK
4 586533. T I
4586533. T I
GC/MS 8
received









10/11/91
11/05/91
RK
45B6533.TI
45B6533.TI
GC/HS B
received
-------
           RADIAN
    EHB
    Radian Work Order; P1-10-001
                                          Sample  History
                                                                               Page:17
                                        Identifications and Dates
         Sample  ID

         Date Sanfiled
         Dace Received
         Matrix
Method Spike   Ca librae ion
               Check QC
10/01/91
XAO-2/Fi
10/01/91
ACN
20
SU8270-Semi-VoLatiles
             Prepared
             Analyzed
             Analyse
             File  10
             Blank  ID
             Instrunent
             Report as
Aldehydes,  Mod T011, HPLC
             Prepared
             Analyzed
             Analyst
             File  ID
             Blank  ID
             Instrument
             Report as
10/11/91
11/05/91
RK
45B6534.TI
45S6S33.TI
GC/MS B
received
               10/19/91
               LKK
               OWEN ISO

               V5000
               received
-------
COBPORJKTIOM
                                               Appendix A





                                    Comments, Notes and Definitions
-------
EHB
Radian Work Order; P1-10-001
                                       Report  Comnents  and Narrative
Page:  A-2
     General Garments
     05-A:  The XAD-2/FiIter portion of the samples was lost  during
      preparation,
     NO = Not quantitaced.
     PAH sanples were diluted because of high hydrocarbon content.
-------
       RADIAN
       COBPORATIOH  ,
                                      Motes and Definitions                                                      Page: A-3
EHB
Radian Work  Order:  P1-10-001
J   Indicates  an  estimated  value  for CC/MS data.  This flag is used either
    when estimating  a  concentration for tentatively identified compounds
    where a  response factor of  1  is assumed, or yhen the mass spectral
    data indicate the  presence  of a compound that meets the identification
    criteria but  the result is  less than  the sample quantiration limit.

NA  This analyte  UBS not  analyzed,

ND  This flag  (or <  )  is  used to denote anaLytes uHch 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 sample.

MS  This analyte  or  surrogate yas not  added ( spiked) to the sample for
    this analysis.

Q   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 RPDCrelatwe percent
    difference) values for  duplicate analyses and matrix spike/matrix
    spike duplicate  result.

*   The asteriskC*)  is used to  Mag  results which are  Less  than five  times
    the method specified  detection  Limit. Studies have shown  thai  the
    uncertainty of the analysis will  increase exponentially as the method
    detection  limit  is approached.   These results should be considered
    approximate.
-------
       RADIAM
                                       Notes and Definitions
EM8
Radian Uork Order:  Pi-10-001
    TERMS USED IN THIS REPORT:
    Analyte -  A  chemical  for which  a  sample is  to be analyzed.
    EPA method and DC specifications.
                                                  The analysis will meet
    Compound -  See Analyte.

    Detection Limit -  The method specified detection  limit, which  is  the  lower  limit of
    quantitacion specified by EPA for a method.   Radian  staff  regularly assess  their
    laboratories1  method detection limits to verify that they  meet  or are lower than those
    specified by EPA.   Detection limits uhich are higher than  method  Limits  are based
    on experimental values at the 99% confidence level.   The detection limits  for  EPA  CLP
    (Contract Laboratory Program) methods are CROLs (contract  required quantisation
    limits) for organics and CROLS (contract required detection limits)  for  inorganics.
    Note,  the detection limit may 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 analysts of environmental samples.   Radian uill  perform its
    analyses and accompanying OC tests in conformance with EPA methods unless  otherwise  specified.

    Factor • Default method detection limits are based on analysis of clean  uater  samples.
    A factor is required to calculate sample specific detection limits based on alternate
    matrices (soil or uater), reporting units, use of cleanup procedures, or dilution  of extracts/
    digestates.  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
    waste.
The sample material.  Generally,  it uill  be soil,  water,  air,  oil,  or solid
    Radian Uorlc Order - The unique Radian identification code assigned to the samples reported in
    the analytical summary.	
    Units - ug/L     microgrants per liter (parts per biII ion);Iiquids/water
            ug/kg    micrograms per kilogram (parts per billion); soils/solids
            ug/M3    micrograms per cubic meter; air samples
            mg/L     milligrams per liter (parts per mill ion);liquids/water
            mg/kg    milligrams per kilogram (parts per miLIion);soits/sotids
            X        percent; usually used for percent recovery of QC standards
            us/cm    conductance unit; mieroSiemans/centimeter
            mL/hr    mi Hi liters per hour; rate of settlement of matter in water
            MTU      turbidity unit; nephetometrie turbidity unit
            CU       color unit; equal to 1 mg/L af chloroplatinate salt
-------
 APPENDIX F.5



SAMPLE ID LOG
-------
Project No-
-------
        RADIAN
                     Pro|ect Mft   fr
    torn Pige No—
                                                                               *p—.
                          IMHH
S5

3~)
3 I
                                                                  ^
                                                                      »UM^
                                                       S"7."7	f <5tr-ftcj j^-tei?
                                                      iLLk
                                                      JQQ4.1
                          v
                          us
                                           /  i
                                      L\
                                  XA-P
 Ml
 5-
'Si
' 5z
 55
;sc.
                                                                                * t>g
                                  ^^
                          HI
                                       V
                                                                               C-3
                 io-rc- 1
 i.;
 a
 *5
                                                                             To Pafe No.
    Witnessed & Understood by me.
                                Date
Invented by
                                          Recorded lay
Date
-------
       TITLE.
                          Project No	

                          .  BookNo._252B4
    Ci.
c
I)  tj
     'J
    It,

    11
    7?
    ro
        From Page No—
                                                                                               ToPac
        Witnessed & Understood by me,
Date
Invented by
                                                     Recorded by
Date
-------
      APPENDIX G



CALIBRATION DATA SHEETS
-------
Posi Test - Mai hey
                          Meter  Box Calibration
Dale
10/3/91
Cal Meier
6830284
Pbar
29.9
Box*
 N-30
Cal Meter Yd
 0.9967
Vaccum
 10 " tig
Orifice
Selling
1.1
1.1
1.1
Cal. Meter
Pressure
-0.07
-0.07
-0.07
Gas Volume
Cal. Meier
Final
IniL
Toial
Final
lnii.
Toial
Final
IniL
Toial
41149
39.743
3.406
49.823
43.5 IS
6.308
S7.947
49.823
8.124
Gas Volume
Meier Box
51743
49.400
3.343
-59.250
S3. 100
6.150
67.182
59.250
7.932
Cal. Temp
In Oul
68
68
67
67
Avg. 67.5
66
66
67
67
Avg. 66.5
67
68
67
68
Avg. 67.5
Meier 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
||@
1.92
1.87
1.90
1.90
-------
                          Meter  Box Calibration
Posi Test - Maihey
Dale
10/4/91
Cal Meier
6830284
Pbar
29.88
Box*
 N-32
Cal Meier Yd
 0.9967
Vaccum
  12 "llg
Orifice
Setting
1.0
1.0
1.0
Cal. Meier
Pressure
-0.06
-0.06
-0.06
Gas Volume
Cal. Meter
Final
[nil.
Total
Final
Inii.
Tolal
Final
Init.
Tolal
32.507
21882
9.625
37.323
3Z507
4.816
44.398
37.323
7.075
Gas Volume
Meier Box
47.087
37.450
9.637
51.885
47.087
4.798
58.962
51.885
7.077
Cal. Temp
In Oui
65
66
65
66
Avg^ 6S.5
66
67
66
67
Avg. 66.5
67
67
67
67
Avg. 67.0
Meter Temp
In Out
71
73
69
70
AT 708
73
74
70
71
Avg. 710
73
75
71
71
Avg. 715

Time
18
9
13.25
Average
Yd
1.0028
1.0083
1.0042
1.0051
Delia
M@
1.95
1.95
1.%
1.95
-------
Post Test - Maihey
                          Meter  Box Calibration
Dale
10/15/91
Cal Meier
6830284
Pbar
29.88
           N-33
                Cal Meier Yd
                   0.9967
              Vaccum
            11 "Hg
Orifice
Selling
1.1
1.1
1.1
Cal. Meier
Pressure
-0.07
-0.07
-0,007
Gas Volume
Cal, Meier
Final
[nil.
Total
Final
(nil.
Toial
Final
Ink.
Total
67.375
61.057
6.318
73.116
67.375
5.741
79.410
73.116
6.294
Gas Volume
Meier Box
76.428
70.000
6.428
. 81298
76.428
5.870
88,777
82.298
6.479
Cal. Temp
In Oui
70
72
70
72
Avg. 71.0
73
72
73
72
Avg. 715
73
72
73
72
Avg. 715
Meier Temp
In Out
73
78
70
72
Avg. 73.3
80
77
75
73
Avg. 76.3
82
79
78
75
Avg. 78.5

Time
11
10
11
Average
Yd
0.9810
0.9788
0.9765
0.97.88
Delia
H@
1.89
1.89
1.90
1.89
-------
   APPENDIX H




SAMPLE EQUATIONS
-------
                                                   SAMPLE CALCULATIONS
COMPANY           ;  BORGESS  MEDICAL  CENTER
PLANT SITE        :  KAIAMAZOO. MI           INPUT  PARAMETERS:
SAMPLING LOCATION  :  BAGHCUSE OUTLET
DATE              ;

EXAMPLE II:  PM/Hetals  ,  RUN  02
iHUUbt QUILtl
07/91

RUN 02

F, 29.92 in Hq


As
Cp
On >
Kp
P(std) -
Pb
Pmg(avg)-
gas sampled at standard condi

Y * Vm ' (T(std) • 460) ' Pm
551
0
0.
94
29
29
0
.55
.84
313
.59
.92
,52
45
sc

i n

in
in
in
|. in.



Hq
Hg
HZO
Ps
xcoz
INZ
toz
T(std) -
Tm(avg) •
Vm
29
4
80
15
68
no
91
48 in. Hg
PM COLLECT.- 0.0102 grin* :
69 AVG SORT OEL.P • Q.ZS46 IN HZO;
26
05
00 f
09 F
40 ft"3
MOISTURE • 211.60 grams :
COLLECTED :
SAMPL TIME . 240 rain. :
Ts(avg) - Z94.4Z F -.
Y • 1.0108 :
tlons:




Pm
Pm
• Pmg/13.6 » Pb :
V
29.5530



      Vm(std)
                       P(std) • (Tm(avg) • 460)


      Vm(std) •       (1.011 " 91.40 " (88 * 460)  * 29.55) / (29.92


      Vm(std) •             64.52 dscf



2)  Volume of water vapor at standard conditions:



      vw[gas) • 0.04707 ftj/g • (moisture collected)

      Vw(gas) -       ( 0.04707 ' 211.60 )


      Vw(gas) *              9.95 scf



3)  Percent moisture in stack:

               100 * Vv(gas)


             Vm(std) * Vw(gas)


      XV «   (100 *9.95) / (84.SZ » 9.95)


      XV .      10.53



4)  *c!a fraction of dry stack gas:


              100 - XV
      HFd -   	
                 100


      Wfd •  (100 - 10.53) / 100

      HFd •     O.B9S
                                                                              110.09 * 460))
-------
                      DEFINITION OF TERMS
 SYMBOL                   DEFINITIONS
   As                    AREA  OF  STACK
   Cp                  PITQT COEFFIC1EMT
   Ca            CONCENTRATION OF PARTIOJLATE
   On             DIAMETER OF  SAMPLING NOZZLE
   ER            EMISSION RATE OF PARTICIPATE
   Kp               PITOT TUBE COEFFICIENT
   MFd          HOLE FRACTION  OF  DRY  STACK  HAS
   HWd         MOLECULAR WEIGHT OF DRY STACK GAS
   MW>         MOLECULAR WEIGHT OF WET STACK GAS
                MOISTURE COLLECTED [N IKPINGERS
 P(std)        STANDARD PRESSURE  (29.9Z  in. Hg)
   Pb                 BAROMETRIC  PRESSURE
Pnq(avg)         AVERAGE GAUGE METER  PRESSURE
   Pa               ABSOLUTE STACK PRESSURE
                       PARTtCULATE CATCH
   Old      AVERAGE STACK ORY  VOLUMETRIC FLOW  RATE
  XCOZ             PERCENT COZ IN STACK  GAS
   XNZ              PERCENT NZ IN STACK  GAS
   X02              PERCENT 02 IN STACK  GAS
   XV              PERCENT MOISTURE IN STACK
   US                PERCENT  EXCESS  AIR
                      TOTAL SAMPLING  TIME
 T(std)           STANDARD TEMPERATURE  [68  F)  -
 Tm(avg)       AVERAGE TEMPERATURE OF THE METER
 Ts(avg)       AVERAGE TEMPERATURE OF THE STACK
   Vm                TOTAL HETERED VOLUME
 Vm(std)            STANDAAO METERCD  VOLUME
 V.(gas)         VOLUME OF MTER  IN STACK GAS
   Vs                VELOCITY  OF  STACK GAS
    T         TEST METER CALIBRATION  COEFFICIENT
    UNITS

    In,"2

 gralns/tt'a
      In.
    Ib/hr
  lb/lb-mla
  lb/lb-mla
     gram
    in,  Hg
    In  Hg
    In.  Hg
    in.  Hg
     gratia
 dry ft'3/mtn.
     nitn.
       F
       f
       f
     ft"3
dry jtindard ft'J
 standard  ft"3
-------
10)  £«ces3  air  (X):

                  100  *  «2
   ws •      	     l
             (0,264  '  WZ] - 102

   XXS -      (100  *  15,05) / ((0.26J ' 80,26) - '=.35)

   XXS •        244.53


11)  Concentration  of participate:

   Ca  • (paniculate catch) / Vm(std) / 453,59 * 7000

   Ca  •      0.0102  /  84.52 / 45J.59 * 7000

   Ca  •      0.00186  grains/dscf


12)  Psrttculate Emissions Rate:

   ER  • (concentration)  • (Qsd) * 60 / 7000

   ER  •      0.0019  '  2444,95 • 60 / 7000

   ER  •         0.039  Ib/hr
-------
5)  Average mjlecular weight  of  dry stack gat:

      HWd - (0.4' *  XCOZ)  • (0.32  * MZ) •  (O.ZB ' XN2)

      MWd •  (0,44 ' 4.69)  *  (0,32 • 15.05} •  (O.Z8 • 80.26)

      HWd •     29 35 Ib/lb-mole


5)  Average molecular Might  of  vet stack gas:

       HUM • HWd * KFd • 18,0 '  (1.0 -  HFd)

       rV. - 29.35 " 0.895 *  18.0  ' (1.0  -  0.895)

       MU« -    28,16 Ib/lb-mole


7)  Stack velocity (feet/min) at stack  conditions:

       Vs * Kp'Cp'[SQRT(dPn»»g*(SQRT[(Ts)avg])'[SQRT(l/Ps-MI*)]*60

       Vs -  84.59 • 0,84 ' 0.25 • SQRT[(29«.4Z  *460) /  (29.48  • 28.16)]

   Vs •      17.24665 fpi
             1034.799 fan

8)  Average stack dry volumetric fin rate:

                    Vj • As " HFd  " (T(std)+460) '  Ps
   Qsd •    	
             144 sq.in./cu.ft, * (Ts(avg)  + 460) *  P(std)

   Qad -     17.25 ' 551.55 • 3.395 ' (M.O * 460)  *  Z9.48 /  (144  •  (294.42 * 480) ' 29-92)

   Qsd •      2444.95 dicfn
             69.24236
9) Fsokinetic sailing rate (X):

          1039.S746 • Vm(std) • (Ts(avg) + 460)
   II	-	-	
        Vs * samp, time ' Ps " HFd " (Dn)"2

   XI •      (1039.5746 ' 34.SZ • (294.42 * 460))  / (1034.80 * 240 • 29,48 *  0.895  '  (0.3U)"2!

   11 •        103.24
-------
     APPENDIX I




PROJECT PARTICIPANTS
-------
                        PROJECT PARTICIPANTS
RADIAN CORPORATION

     Rod Brown
     Geoff Johnson
     Jack Johnson
     Vince Laura
     Julie Lopez
     Tom McDonald
     Terry  Medley
     Charlie Parrish
     Kathryn Potter
     Larry  Romesberg
     Tim Skelding
     Judy Smith
ENVIRONMENTAL PROTECTION AGENCY

     Dennis Holzschuh
-------
             APPENDIX J

SAMPLING AND ANALYTICAL PROTOCOLS

          J,l   PM/Metals
          J.2   PM10/CPM
          J,3   Aldehydes
          J,4   PAH
          J.5   CEM and GC
-------
APPENDIX J.I



PM/METALS
-------
                                                         EMB  DRAFT  METHOD  1C,]! =3

            METHODOLOGY FOR THE DETERMINATION OF METALS  EMISSIONS
                  IS gfflAUST GASES FROM INCINERATION PROCESSES

1.   Applicability and Principle
     1.1  Applicability.  This method  is applicable  for  the  determination of
arsenic (Aa),  beryllium (Be), cadmium  (Cd),  total chromium  (Cr),  lead  (Pbj.
asercury (Hg),  nickel (Ni), and sine  (Zn) emissions  from  municipal  waste
incinerators and similar combustion processes.  These  elements  are referred to
hereafter as the primary metals.  This method may also be used  for the
dstermlnation of antimony (Sb). barium (Ba), copper  (Cu). eanganase (Mn),
phosphorus (P). selenium  (Se). silver  (Ag),  and thallium (Tl) emissions  froo
these sources.  These elements are referred  to hereafter as  the secondary
eetals.
     In addition, the eethod eay be used to  determine  partlculate  emissions by
following the additional procedures described.  Modifications to  the sample
recovery and analysis procedures described in this protocol  for the purpose of
determining particulate emissions may  potentially impact the front  hair nercury
determination.*
     1.2  Principle.  The stack sample is withdrawn  isokiAetieally  from  the
source, with partieulate emissions collected la 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  la two (or one)
iBplAgers.  Sampling train components  are recovered  sad  digested  in separate
front and back half fractions.  Materials collected  In the sampling train are
digested with acid solutions to dissolve inorganics  and  to remove  organic
constituents that may create analytical interferences.  Acid digestion  is
performed using conventional Parr' Bomb or microwave digestion  techniques.  The
•Field tests to date have shown  that of the) total aveunt of mercury measured
 by the method, only 0 to <2I was  measured ia the front half.   Therefore,  it  is
 tentatively concluded, baaed on the above data,  that partlculate emissions nay
 be measured by this train, without signlficsntly altering the mercury results.
-------
nitric acid and hydrogen  peroiiide  impinger  solution,  the  acidic  potassium
permanganate impinger solution,  and  the  probe  rinse  and digested filter
solutions are analyzed  for mercury by  cold  vapor atomic absorption  spectroscapy
(CVAAS).  Except  for the  permanganate  solution,  the  remainder of the  sampling
train fractions are analyzed  for Aa. Be.  Cd. Cr. Pb.  Ml,  and Zn  (and  Sb. Ba.
Cu, Mn. P, Se. Ag, and  Tl, if desired) by inductively coupled argon pluaa
emission ipectroacopy (ICAP)  or  atomic absorption spectroacopy {AAS).  Graphite
furnace atoeic absorption ipectroacopy (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 Bay use AAS  for analyses  of all  target metals  if the  resulting  in-
stack eethod detection  Halts (combined  seepling and analytical  detection
limits) meet the  data quality objectives of the) tasting program.  For
convenience, allquota of  tech digested sample  fraction can be combined
proportionally for a single analytical determination.  Thm efficiency of the
analytical procedure is quantified by  the analysis of spiked quality  control
samples containing each of the)  target  metals including actual sample  satrix
effects checks.

2.   Range. Sensitivity,  Precision,  and  Interferences
    2.1  Range.   For the  analyse*  described la this  methodology  and for  siallar
analyses, the ICAP response ia  linear  over several orders of magnitude.  Sam-
ples containing metal concentrations la  the) nanograma per mllllllter  (ng/el) to
aicrograms per mlllllitar (ug/ml)  range  la the analytical finish solution  can
be analyzed using tola  technique.  Samples) containing greater than
approximately 50  ug/ml  of arsenic, chromium, or lead should be diluted to  that
level or lover for final  analysis.  Semples "•*****i*'*«g greater than
approximately 20  ug/al  of cadmium)  should be diluted  to that level before
analysis.
    2.2  Analytical Sensitivity.  ICAP analytical detection limits for the
primary [and secondary] metals  ia  the  sample solutions) (baaed on SH-8»6, Method
6010) arm approximately as follower  As (53 og/ml). fie (0.3 ng/el). Cd (<<
ng/al). Cr (7 ng/ml), Pb  (02  ng/ml). Hi  (15 ng/al),  & (2 ng/ml) [Sb  (32
ng/ml). Ba (2 ng/ml). Cu  (6 ng/al).  P  (75 og/ml). HB (2 ng/ml).  Se (75 ng/il),
Ag (7 ng/ml). Tl  (HO ng/ml)].  The actual method detection limits are sample
dependent and may vary  as the sample matrix may affect the limits.  The
-------
analytical detection Halts  for  the prlaary  [and  secondary] aetals  in  sample
solutions analyzed by direct aspirttion AAS  (baaed  on SH-W6, Method 7000) are
approximately «LS  follows: As (2  ng/al}, Be (5 ng/ml). Cd  (5 nf/il), Cr  (50
ng/al). Pb (100 ng/al). Ni  C*0 ng/al), Zn (5 rig/el)  [Sb (200 ng/«l), 9a  (100
ng/Bi), Cu [20 ng/al). Mn (10 ng/al),  Se (2 ng/il). Ag (10 ng/al). Tl  {100
ng/ml)j,  The detection Halt for aereury by CVAAS  is epproaiaetely 0.2  ng/al.
The use of CFAAS  can give added  senaitivity  compared to the use  of diracc
aspirstion AAS for the following priaary and secondary metals: As  (1 ng/al).  3e
(0.2 ng/al). Cd (0.1 ng/Bl). Cr  (1 n«/Bl), Pb  (1  ng/ml),  Sb  (3 ng/al).  S«  (2
ng/Bl), and Tl (1 ng/al).
    Using (1) the procedures described in this  eethod,  (2) the analytical
detection liaita  described  in the previous paragraph.  (})  a voluae  of  300  al
for the front half and 150 al for the back half saaples.  and  (4) a  stack gaa
laaple volume of  1.2? a3, the corresponding  in-stack eethod detection
are presented in  Table A-l  and calculated aa shown:
    where: A • analytical detection  Halt,  ug/ml.
           9 • volume of sample prior  to  aliquot  for analysis,  al.
           C • stack sample volume,  dsca  (dssP).
           0 * tn-stack detection  limit,  ug/a3.

Values in Table A-l are calculated for the  front  and back half  and/or  the
train.
    To ensure optimum sensitivity  la obtaining the measurements,  the
concentration* of target metals in the solution*  are suggested  to be at least
tan times the analytical detection limit*.   Under certain conditions,  and with
greater care in thm analytical procedure, this concentration can  be a* low as
approximately three time* the analytical  detection limit.   In all cases.
repetitive analyse*, method of standard addition* (0A). serial dilution, or
aatrix spikm addition should be uaed to eatabllah the quality of  the data.
    Actual in-stack method detection limit* will  be  determined  baaed on actual
source sampling parameter* and analytical result* a* described  above.  If
required, the method in-stack detection limit* can be made  more sensitive than
those shown la Table A-l for a specific teat by uaing one or more of the
following option*:
-------
             TABLE A-l. IN-STACK METHOD DETECTION LIMITS fuf/a3)
                    FOR TRAIN FRACTIONS USING 1CA? AUD AAS
Metal
 Front Half
 Fraction 1
Pro ex and Filc*r
 Back Half1
 Fraction 2
laplnfara 1-3
 Bade Half.
 Fraction |
lapiflfara U-5
                                                            Total Train
Primary Matala
Araanie
Baryiliua
Cadaiya
Chroaiua
Laad
Harctiry
Niekal
Zinc
12.7 (0.3)*
0.0? (0.05)*
1.0 (0.02)*
1.7 (0.2)*
10.1 (0.2)*
0.05**
3-6
0.5
6.* (0.1)*
0.04 (Q.QS)*
0.5 (0.01)*
0.8 (0.1)*
5-0 (0,1)*
0.03** 0.03**
1.8
0.3
19- 1 SO. 4)*
O.ll (0.08)B
1.5 (0.03)*
2. 5 '(0,3)'
15-1 (0-3)*
0.11**
5-4
0.8
Secondary Natala
Antimony
Barium
Copper
Mancanaaa
Phoaphorua
Salanlua
Silvtr
Thaliiua
7.7 (0.7)*
0.5
l.l*
0.5 (0.2)*
IS
18 (0.5)»
1.7
9-6 (0.25*
3-8 (0.4)*
0.3
0.7
0.2 (O.D*
9
9 (0.3)*
0.9
4.8 (0.1)*
11.5 (!.!)•
0.8
2.1
0.7 (0.35*
27
27 (0.3>*
2.6
14.4 (0.3)*
    D*t*ction  limit  whan analysad by 3FAAS.
    D*t*cuon  limit  trim analytad by CVAAS.
    Actual MtlMd in-acacfe  d« tact ion llml ta  trill  bm d«tarmin«d baaed
    on  actual  aotiree aampllnc  paraaMtara aad analytical raaulta  aa
    daacnbad  aarliar in tMa  auction.
       A normal  1-bour aaapllnf run collacta a atack faj aaapllnf voluaa of

       atwut  1.25 a*.   If tba aaaplin< eia* ta inerMaad and 5 •*  •«
       collactad.  tha  in-atack aathod dataction lialta  would ba ona fourth of
       th- vmluits ii^^ ^ fabla A-l (tMa aaa&a that with tMa chant*, tha

       aatbod la tour  tim« aor* aanaitiva than aoraal).
       Tha la-atacfc datactlon limlta uaiaw that all of tha •aapla If dl|«at0d
       (vita  a»captlon of t&a aliquot for aarcury)  aad  taa final liquid
       voluaaa for analyaia ara 300 al for tha front Half aftd 150 al for tnc
       back half aaapla.   If tha front half volian li raducad froa 300 ml to
       30  al,  tha front half in-atack da tact ion liaita  would ba ona tanth of
       tha valuaa ahown e.ov* (tan tiaaa aora aanaitiva).  If tha back half
       voluaa la raduead froa 150 al to 25 al. t&a in-atack dataction Halts
-------
        would be one sixth of the above values.  Matrix effects checks are
        necessary on analyses of samples and typically are of greater signifi-
        cance for saaples that have been concentrated to less than the noraal
        aaaple volume.  A voluae leas than 25 ml may not allow resolubtliza-
        :.on of che residue and may increase interference by other compounds.
    o   When both of che above two isproveaents are used on one sample at the
        sue time, che resultant improvements are multiplicative.  For exuple.
        •here stack gas voluae is increased by a factor of five and the total
        liquid saaple 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 acre
        sensitive).
    o   Conversely, reducing stack gas saaple voluae and increasing saaple
        liquid voluae will increase liaits.  The) front half and back halfl
        samples (Fractions 1 and 2) can be combined priorrto analysis.  The
        resultant liquid volume  (excluding Fraction 3. which eust be analyzed
        separately) la recorded.  Combining the asaple as described does not
        allow determination (whether front or back half) of where in the -rain
        the saaple was captured.  The In-stack method detection Halt then
        becomes a single value for all target metals except mercury, for which
        the contribution of Fraction 3 "ust be considered.
    o   The above discussion assuaes no blank correction.  Blank corrections
        are discussed later in this method.
    2.3  Precision.  The) precisions (relative standard deviations) for each of
the primary and secondary metals detected la a method development test at a
sewage sludge incinerator, an as follows: As (13.51). Cd (11.5», Cr (11.21),
Pb (11.6S). Zn (11.81). Sb (12.71). Ba (20.61). Cu (11.51), P U4.6S). Se
(15-31), and Tl (12.39).  The precision for nickel was 7-7J for another test
conducted at a source simulator.  Berylliua, manganese and silver were not
detected in the) tests; however,  based on the analytical sensitivity of the ICAP
for these metals, it is assuaed  that their precisions should be similar to
those for the other metals, whan detected at slallar levels.
    2.4  Interferences.  Iron can b* a spectral interference during the
analysis of anemic, chroalua, and cadalua by ICAP.  Aluainua can be a spectral
interference during the) analysis of arsenic and laad by ICAP.  Generally, these
interferences can be reduced by diluting the asaple. but this increases the
-------
in-stack method dec set ion  Halt.  Refer to  EPA Method 6010 (SM-&46)  for details
on potential interferences  for  chit  method.   For til  GFAAS analyse*,  estrix
modifiers should be used to lialt interferences,  and  standards  should be
aacc.h.ed.

3,   Apparacus
    3-1  Samplinf Train.   A schematic  of th« samplinf train is  shown in
A-l.  Ic is similar to  th* Method 5  train.   The samplinf train  consists of  the
followinf component*.
    3-1.1  Prob* Nosile (Prcae  Tip)  and Boroslllcate  or Quarts  Glass Probe
Liner.  Same as Method  5,  Section* 2.1.1 and 2.1.2.   01 ass nossles art
requiredunless an altcrnata probe tip  prevent* the possibility  of eontaainacion
or interference of the  sample with it* materials of construction. If a probe
tip other than fleet  it used, no correction of the stack ssmpls test results
can be Bade because of  the effect on the result* by the probe tip.
    3.1.2  Pitot Tube and  Differential Pressure Oaufe.  Same at Method 2.
Sections 2.1 and 2.2. respectively.
    3.1.3  Filter Holder.   Olata, same at Method 5. Section 2.1.9, except  that
e. Teflon filter support vuat be uaed to replace the flats frit.
    3.1.4  Filter Heatinf  3ystea.  Same at  Method 9.  Section 2.1.6.
    3.1.5  Oandenaer.   Th* follovinc tyetsti ahmll be  uted for the condensation
                                        *
and collection of fateous  metalt end for determininf the eoisture content of
the stack faa.  The condenainf  eymtem ahould conelat of four to sia impinfen
connected in series with leak-free framd flaea fittin«t or other leak-free.
non-contaminatinf flctinfi. Tbe firtt iapiiift* U optional and it recommended
at s  water toockout trap for ume durlaf teet condition* which require such  a
trap.  The impinfere  to be ueed In th* metalt train arm now described,  vhen
the firtt impinfer it uted at  a water knockout, it shall be appropriately-sited
for an expected larfe. toUture  catch and eonitructad fmnerelly at deeeribed for
the firtt impincer in Method 5. Parafraph 2.1.7'  The second Utpinfer (or the
first HNO,/H,0, iepinfer)  shall alto be at described for th* firtt impiAfer in
Method 5.  Tom third  Upincmr  (or  the impinfer used at th* second RW))/H30,
impinftr) shall be the  same at  the Oreenfrurf Smith impiisfer with the standard
tip described at the  second impinfer in Method 3. Partfrapa 2.1.7.  All other
impinfers uaed in the metals train arm the tarn* am thm second iapinfer (the
first HMOj/RjO, imp infer)  previously deeeribed in this pmrtiraph.  In summary.
-------
a
 2>
i
VI

i
i
 i
•3
 s
   i
-------
che first impinger should be empty, the second and third shall contain kr.owr.
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 '4.2.2)   ./id the last  -apinger shall
 ontain a known quantity of silica  eel or  equivalent deeiccanc.  A  theraoaeter
capable of measuring to within 1°C  (2°F) shall be placed ac  the outlet of  the
last iapinfer.  When che water Imockout lap infer is not needed, it  is  reeoved
from the train and the other ispiiifers resiain the same.  If  mercury analysis ia
not needed, the potassium permanganate tap infers are removed.
    3.1.6  Metering Systee. Barometer, and Qas Density  Detereination
Equipment.  Save ae Method 5. Sections) 2.1   throufh 2.1.10, respectively.
    3.1.7  Teflon Tape.  For capplnf openings and sealinf  connections  on  che
sampling train.
    3.2  Sample Recovery.  Sam*) u  Method  5. Section* 2.2.1  throufh 2.2.8
(Nonmetallic Probe-Liner and Probo-Noiils  Brushes, Wash Bottles, Sample
Storafe Containers). Petrl Oishee, Glass Graduated Cylinder.  Plaetic Storafe
Containers, runnel and Rubber Policeman, and Olaai Funnel),  respectively,  with
the follovtnf exceptions and additions);
    3.2.1  Nonaetallic Probe-Liner  and Probe-Hoatle Bruahea.   For quantitative
recovery of Materials collected Ln  the fr -t half of the saaplinf train.
Description of acceptable all-Teflon eoapvrant brushes  to  be included  in EPA'a
Emission KeasuresMnt Technical Information Center  (BVITC)  filee.
    3.2.2  Saaple 3 tor ace Container*.  Olasie bottles) with  Teflon-lined caps.
1000- and 500-sJ,. ahall be used for KlfeiO,-concal&inf •••pies and blanks.
Polyethylene bottles say be used  for other staple  types.
    3-2.3  Qraduatad Cylinder.  Olass or equivalent.
    3.2.4  Fxmnel.  Olass or equivalent.
    3.2.;  Labels.  For identification of  •••plea.
    3.2.6  Polypropylene Tweeisre aed/or Plastic Qlove«.   For recovery of  the
filter frost the saaplinf  train filter holder.
    3-3  Sample Preparation and Analysis.  For  the analysis, the  followinf
equipment is needed;
    3.3.1  Volumetric Flasks. IX al, 290  ml. end  1000  ml.  For preparation  of
standards and sample dilution.
    3.3.2  Graduated Cylinders.   For preparation of  reagents.
    3.3.3  Parr1 ic«bs or Microwave Pressure Belief  Vessels  with  Capplnf
-------
Station (CO! Corporation lodel or equivalent).
    3.3.4  Beakers and Watchglasses.  250-»1 beakers  for sample digestion with
watchglasses to cover the  tops.
    3.3-5  Ring Stands and Clamps.  For securing equipment such as filtration
apparatus.
    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-d  Disposable Pasteur Pipets  and  Bulbs.
    3.3.9  Volumetric Pipets.
    3.3.10  Analytical Balance.  Accurate to within Q.I sf.
    3.3.11  Microwave, or Conventional Oven.  For heating saaples  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 A*.  C
-------
che metals to b« eeuured.  Analytical results provided by filter
are acceptable.  However, if no such results are available, filter blanks auac
b« analyzed for each tarfet aetal prior to Mission test inf.   Quartz fiber or
gl&aa fiber niter* without orcanie binder* shall b* used.   The filters should
exhibit at least 99-95 percent efficiency  (<0.05 perceri penecretion) on 0.3
aicron dioctyl phthalate saoke particles.  The filter efficiency test shall be
conducted in accordance with ASTM Standard Method 02986-71 (incorporated by
reference).  For particulate determination in sources containinf SO, or SO  ,
the filter aaterial iust be of a type  that is unreactlve  to SO, or S0}, as
described in EPA Method 5-  Quartx  fiber filter* aeetlng  these  requireeencs are
recommended.
    U.i.2  Water.  To conform to ASTM  Specification 01193.77, Type II
(incorporated by reference).  Analyze  the vater for all tartet  aetals prior to
field use.  All tarfet aetals should be le*e than 1 ng/el.
    4.1.3  Nitric Acid.  Concentrated.  Baker Inatra-enalyred or equivalent.
    4.1.4  Hydrochloric Acid.  Concentrated.  Baker Instra-analyzed  or
equivalent.
    4.1.5  Hydrogen Peroxide. 30 Percent (V/V).
    4.1.6  Potaeelusi Permanganate.
    4.1.7  Sulfurlc Acid.  Concentrated.
    4.1.8  Silica 0*1 and Crushed Ice.  Same w Method 5. Sections 3,1.2 and
3.1.4.  respectively.
    4.2  Pretast Preparation for Saaplinf  Reafects.
    4.2.1  Nitric Add (HHO,)/Hydrofec Peroxide (H,0a) Ataerblnff Solution.
5 Percent HNOj/10 Percent 0,0,.  Add 50 ml of concentrated HKO, and  333 •! of
30 percent 11,0, to • LOOO~aU, voluejsjtrlc flaak or fretfuated cylinder  containinf
approxisuitely 500 ml of water.  Dilute to volume with vater.  The reecent shall
contain lace then 2 nf/al of each tarfet eetal.
    4.2.2  Acidic Potassiua Pereanfinate (Ote04) Ataorbiaff Solution. 4 Percent
KMnO, (W/V).  Prepare fresh daily.  DUsolve 40 f of K»aO» la sufficient 10
percent H,SO, to aake 1 liter.  Prepare sad store la flaas bottles to prevent
degradation.  The reagent shall contain lea* than 2 of/al of Bf.
Precaution;  To prevent autocatalytic  decoepoeition of the peraanfmn*t«
solution, filter the solution throufh  Wutman 941 filter paper.  Also, due  to
reaction of the potaMlia permanfaaste vita the add. there aay be pressure
buildup in the ssaple storage bottle;  these bottle* should not  be fully filled
-------
and should be vented both to relieve excess pressure and prevent explosion 
-------
4.4.14  lanthenua Oxide. la,0j
4.4.15  AAS Grid* As Standard,
a. a. 16  AAS Grade Be Standard.
'4. 4.17  AAS Grade Cd Standard.
4.4.1.3  AAS Grid* Cr Standard.
4.4.19  AAS Grade Pb Standard,
4.4,20  AAS Grade Hf Standard.
4,4.21  AAS Grade Ml Standard.
4.4.22  AAS Grade Zn Standard,
4.4.23  AAS Grade Al Standard.
4.4.24  AAS Grad* Fa Standard,
4.4.29  AAS Qrada Sb Standard.
4.4.26  AAS Grade Ba Standard.  1000 uff/al.
4.4.27  AAS Grade Cu Standard,  1000 uff/ml,
4.4.21  AAS Grade to Standard,
4.4.29  AAS Grade P  Standard,
4.4.30  AAS Grade Sa Standard,
4.4.31  AAS Grade A* Standard,
4.4.32
                                   1000 uf/al.
                                   1000 uf/ai.
                                   1000 uf/«l.
                                   LOGO ug/al.
                                   1000 uf/al.
                                   1000 uf/ml.
                                   LOGO uf/al.
                                   1000 uf/ml.
                                   1000 uf/*l.
                                   1000 uf/al.
                                   1000 uf/al.
Optional.
Optional.
Optional,
Optional.
Optional.
Optional.
Optional.
Optional.
                                   1000
                                   1000 uf/*l.
                                   1000 uaVal.
                                   1000 u«/al.
            AAS Grade Tl Standard. 1000 uf/al.
    4.4.33  the aetala •tandarda aay alao be aade froa lelid chaaicali as
deacrib«i in EPA fethod 200.7.  BPA Method 7470 or Standard Method* for the
Analyaii of Water and Waataimtar.  15th*Edition, Method 303? anould be referred
to for additional information on aarcury atandardj.
    4.4.34  Mercury Standard* and Quality Control Saaplw.  Prepare freah
weekly a 10 uf/al intermediate eercury •tandard by addinc 5 al of 1000 yf/ai
•erairy ttock solution to a 500-ml voliaatrle  flaak; dilute to 500 al by first
addinf 20 al of 15 percent UNO, and then adding water.  Prepare a working
aercury •tandard aolution freah daily;  add 5  «1 of taa 10 uf/al intermediate
•tandard to a 250 al volumetric flaak and dilute to 250 al vita 5 al of
4 percent Oto04, 5 al of 15 percent iNO,, and  than watar.  At leaat «i«
separate aliquota of the workinf mercury atandard •olutlon ahould be uaed to
prepare the •tandard curve.  Theae allquota anould contain 0.0. 1.0. 2.0. 3-0.
4.0, and 5.0 al of the working standard aolution.  Quality control laaples
should be prepared by aakinf a Mparata 10 uf/al •tandard and diluting until in
the ranee of the calibration.
    4.4.35  ICAP Standard* and Quality Control SaaplM.  Calibration standard!
-------
for ICAP analysis can be combined  into  four different eixed  standard solutions
as shown below,
                   MIXED STANDARD SOLUTIONS FOR ICAP ANALYSIS
              Solution	ElesMmts (secondary aetals in parantheaea)
                  I                As.  8a. Cd. Pb. Zn (Nn. Se)
                 II                Fa (Ba. Cu)
                III                Al.  Cr. Hi
                 IV                (5b. P. Af. Tl)

Prepare these standard* by coabinlng and  diluting  the appropriate volumes of
che 1000 ug/al solution! with 5 percent nitric acid.  A alniaua) of one  stan-
dard and a blank can be used to fora each calibration curve.  However,  a
separate quality control saiple spiked  with known  aaounts of the target laeais
in quantities in the aidranfe of the calibration curve should be prepared.
Suggested standard levels are 50 uf/al  for Al. 23  uf/el for  Cr and Pb.  15 ug/al
for Fa. and 10 ui/el for the regaining  elements.   Standard*  containing  lass
than 1 u^/al of eetal should be prepared  dally.  Standard* containing ffraaeer
than 1 ug/el of eetal should be stable  for a alnlsus of 1 to 2 we*fcj.
    4.4.36  Graphite Furnace AAS Standarda for Arsenic, Cadmiua, snd Uad (and
Antisony. Selenlua, and Thalliua).  Prepare a  10 uf/al atandard by adding i si
of 1000 ug/el standard to a lOO-el volumetric  flask.  Dilute to 100 el  with 10
percent nitric acid.  For graphite furnace AAS, the standards eust be eatrix
oatched; e.g.. if the saaplee contain 6 percent nitric acid  and 4 percent
hydrofluoric acid, the standarda should'also be esda up with 6 percent  nitric
acid and 4 percent hydrofluoric acid.   Prepare a 100 afl/al standard by  adding
1 al of the 10 uf/el staodard to a 100-el volumetric flask and dilute to 100 nl
with the appropriate aatrln solution.   Other standarda should be prepared by
dilution of the 100 nc/el standarda.  At  leaat five standards should be used ca
aake up the standard curve.  Suffeated  levels  are  0. 10. 50. 75. and 100 ng/al.
Quality control samples should be  prepared by  aaMlnf a separate 10 uc/sd
standard and diluting until it if  in  the  range of  th* saaple*.  Standarda
containing leM than 1 ug/al of eetal should be prepared dally.  Standarda
containing greater than 1 ug/el of eetel  should be stable  for a ainiaue. of  1 to
2 week*.
    4.4.37  Matrix Modifiers-
    4,4.37.1  Nickel Nitrate, l Percent (V/V).  OUaolve 4.996 g of
Mi(N03)a 6H,0 ia approxlMtely 50  el  of rater  in a 100-al volusMtrlc flask.
-------
Dilute to 100 •! with water.
    U.U.37.2  Nickel Nitrate, One-tenth  Percent  (V/V).   Dilute  10  el  of  1  per-
cent nickel nitrate solution  to  100  mi with water.   Inject  an equal  aacunc of
       and this modifier  into the  graphite  furnace  during AAS analysis  for AS.
     .^.37.3  Lanthanum.   Dlsaolve 0.5864 g of L^Qj  in 10  mi of concentrated
     and dilute to 100  mi  with water.  Inject an equal  amount of saaple  and
this eodifler into the  graphite  furnace  during AAS  analysis for Pb.

5.  Procedure
    5.1  Sampling.  The complexity of this  method is such chat, to obtain  reli-
able resultsv testers should  be  trained  and experienced with the test procedures
    5.1.1  Pretest Preparation.   Follow  the saae general procedure given in
Method 5. Section 4.1.1.  except  that,  unless partlculate emission* arc to  be
determined, the filter  need not  ba> desiccated or weighed.  All  sampling train
glassware should first  be rinsed with hot  tap water and then washed in hat
soapy water.  Next, glassware should be  rinsed three times  with tap vster,
followed by three additional  rinses  with water.   All glassware  should then be
soaked in a 10 percent  (V/V)  nitric  acid solution for a minimum or U hours,
rinsed three times with  water,  rinsed a 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.   Seme as Method 3, Section 4,1.2.
    ?.!.}  Preparation  of Sampling Train.   Follow the same  general procedure*
given iA Method 3. Section 1.1.3.  except place 100 el of the nitric
acid/hydrogen peroxide  solution  (Section 4.2.1)  la the two  HNOj/H,Oa  ispingers
{normally the second and  third  impingers).  place 100 al of  the  acidic potassiua
permanganate solution  (Section 4.2.2)  in the fourth and fifth impinger.  and
transfer approximately  200 to 300 g  of preweighed silica gel from its container
to the last imp lager.   Alternatively,  the  silica gel say be weighed directly in
the ispinger Just prior to train assembly.
    Several options ere available to the tester based on the sampling
conditions.  The use of an empty first implnger can be eliminated if the
moisture to be collected  in  the  implngers  is calculated or determined to be
less than 150 al.  The  tester shall  Include two impingers containing the
acidic potassium permanganate solution for the first test run.  unless past
testing experience at  the same or similar  sources ham shown that only one  is
-------
necessary.  The last pereanganete  ispinger  aay  be  discarded  if both
peraanganate iapingers have retained  their  origin*!  deep  purple pereangana:e
color.  A aaxiBua of 200 el in  aach pereanganate ispinger (and a aaxiaua  of
three peraanganate  iepingers) aay  be  used,  if necessary,  to  maintain  the
desired color in the l»st peraanganate  iapinger,
    Retain for reagent blanks,  100 al of  tha  nitric  acid/hydrogen peronide
solution and 100 >1 of tha acidic  potass iua permanganate  solution.  These
solutions should be labeled and treated as  described in Section 7.  Sec up  the
sasplinf train aa shown In Pifur*  A-l.  If  rveceaaary to anjure leak-fr«e
saapling train connection*, Teflon tape should  be  uaed instead of silicon*
gr«asa to prevent contaeination.
    Precaution;  Extreee care should  be taken to prevent  contaainacion within
the train.  Prevent the eercury collection  reagent (acidic potaaaiue
pereanganate) froe  contacting any  glassware of  the train  which is washed  and
analyzed for Nn.  Prevent hydrogen peroxide free) aixlng with the acidic
potasaiue pereanganate.
    5.1.4  Leak-Check Procedures.  Follow the leak-check  procedures given in
Method 3. Section lngera  into  the filter.
    Before eovins; the sampling  train  to the cleanup site, reeove the  probe
the saapling treia  and cap the  open outlet.  Be careful not to lose any
condensats that aight be present.  Cap  the filter inlet where the probe was
fastened.  Remove the uabllical cord  froe the last ispinger and cap the
-------
ispingar.  Cap off  the  filter holder outlet »nd  tapinger inlet.   Use non-
contaainating cape, whether ground-glass  stoppers,  plastic capa,  serum cap*.
or Teflon cap« to close that* openings.
    Alternatively,  the  train can be disajseablad before the probe and filter
holder/ovan ara completely coolad.  if thia  procedure la followed:  Initially
disconnect the filter holder outlet/impinger ialat and looaaly cap the op«n
end*'  Then disconnect  the probe  from tha filter holder or cyclone inlet and
looialy cap the open end*.  Cap the probe tip and remove the umbilical cord  as
previously described.
    Transfer the probe  and filter-impinger assembly to a cleanup area that is
claan and protected from the wind and other potential causaa of contamination
or losa 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 Fifure A-2). Assure that all items necesaary for recovery of the
sample do not contaminate it.
    5.2.1  Container Ho. I  (Filter).  Carefully remove the filter from tha
filter holder and place it  in  its identified petri dish container.  Acid-
washed polypropylene or Teflon  coated tweezer* or clean, disposable surjical
gloves rinsed with  water should be used to handle tarn filters.  If it is
necessary to fold  the  filter,  make certain the particulata cake is inside the
fold.  Carefully  transfer the  filter and- any particulate matter or filter
fibers that adhere  to  the filter bolder gasket to the petrl dish by using a  dry
(acid-cleaned) ayloa bristle brush.  Do not use any metal-containing materials
when recovmrinf this  train.  Seal the labeled petri dish.
    5.2.2  **-**ittlittr Ho. 2  (Acetone Rinse).  Taking care) to see that dust on
the outside) of tha)  probe or other exterior surfaces tees not get into the
sample, quantitatively recover particulata) Batter and any condensata  from the
probe noxile, proem fitting, proem liner, and front half of the filter holder
by washina* tbmmm components vita, 100 ml of acetone and placing the wash i_n a
glass container.  Hotat  The use of emsetly 100 ml Is necessary for the
subsequent blank correction procedures.  Distilled water may be used  instead of
acetone wham approved  by tarn Administrator aad shall be used wHaa specified  by
the Administrator;  la  rhmss esses, save a water blank aad folio* tarn
Administrator's directions  on  analysis.  Perform tarn acmtonm rinses as follows:
Carefully remove  the probe nossla and clean the inside surface by rinsing with
acetone  from a wash bottle and brushing with a nonmmtallic brush.  Brush until
-------
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-------
the acetone rinse shows no visible  particles,  after which aake  a final  rinse  z:
the inside surface with acetone.
    Brush and rinse  the inside  parts  of  Che  Swegelok fittinf with acetone  in  a
giailar way until no visible  particles remain.
    Rinse che p'-obe  liner with  acetone by  tilting and rotating  the prob« while
squirting acetone into its upper  and  so  that all  inside surfaces will be wetted
with acetone.  Allow the acetone  to drain  from the lover end into the staple
container.  A funnel eay be used  to aid  in transferring liquid  washings to the
container.  Follow the acetone  rinse  with  a  nonmetallic 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  lover  end of  the probe, and catch any acetone
and partlculete eattar which  Is brushed  through the probe three times or acre
until no visible paniculate  asttar 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 la the staple container.
After the brushing,  make a final  acetone rinse of the probe as  described above.
    It  is recommended  that two  people clean the probe to minimize sample
losses.  Between sampling  runs, keep  brushes clean and protected from
contamination.
    Clean the inside of  the  front half of  the filter holder by rubbing •
surfaces with a nonaetalllc nylon bristle  brush and rinsing with ace tor,
Rinse each surface  three  tlaee  or more If  needed to remove visible partlculate.
Make a  final  rinse of  the  brush and filter holder.  After all acetone washings
and partlculate eat tar have been  collected ta tbm sample container, tighten the
lid on  the saaple container so  that acetone) will net leak out whan it is
shipped to the laboratory.  Mark  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 el of 0.1 N nitric acid
and place the wash  into  a  temple  storage container.  Note: The use of exactly
100 el  is necessary  for  the subsequent clank correction procedures.  Perfora
th* rinses as described  In Method 12. Section 9.2.2.  Record the) volume of the
combined rinse.  Nark  torn  height  of the fluid level on tarn outside of the
storage container and  use  this  aark to determine If leakage occurs during
-------
transport.  Seal  th*  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  Mo.  H  (lapingers 1 through 3.  Contents and Rinses).   Due
tc the Large quantity of  liquid involved,  the  tetter Bay place  the iapir.ger
solutions in «ore than one  container.  Measure the  liquid in the first three
iapingers voluaetricelly  to within 0.5 al  using a graduated cylinder.  Record
the volume of liquid  present.   This information is  required to  calculate  the
aoisture content  of the sastpled flue fas-   Clean each of the first three
iapingers. the filter support,  the back Half of the filter housing,  and
connecting f lass ware  by thoroughly rinsing with 100 ml of 0.1 N nitric acid as
described in Method 12. Section 5.2.1.  Note);  The use of exactly 100 si of 0.1
N nitric acid rinse is necessary for the) subsequent blank correction
procedures.  Combine  the  rinses end impinger 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 occur* during transport.   Seal the) container and clearly label the
contents.
    5.2.5  Container  No.  5  (Acidified Potassium Permanganate Solution and
Rinses, lap Inge rs No. *t fc 5).   Pour all the liquid  fros) the permanganate
iapinger* (fourth and fifth, if two permanganate iapinger* are  used) into a
graduated cylinder and measure the volume  to within 0.5 ml.  This information
is required to calculate  the) moiaturs) content  of the sampled flue gas. Using
100 al total of the acldlfiad potassium permanganate solution,  rinse the
permanganate iapingmr(a)  and connecting glama  pieces a minimum  of three tiaes.
Combine the rinse* vita tarn permanganate impingmr solution.  Finally, rinse the
permanganate iapingar(s)  and connecting glamsvmre vita 50 mi of fl N HC1 to
remove any reaidu*.   Ngta:  The) ua* of exactly 100 al and 50 ml  for the two
rinse* is omcasaary for the) subsequent blank correction procedure*.  Place the
combined rinsaa and iapingar eontanta in a labeled  glass storage bottle.   Nark
the height of the fluid level on the outside) of to* bottle to determine if
leakage occur* during transport.  Sa*j the)  following nota and the) Precaution in
Paragraph U.2.2 and properly seal the bottla sad clearly label  the ce«tents.
    Nota:  Due to thai potantlal reaction of th* potassium permanganate with the
acid, there aay be pressure buildup la tat) sample s to rag* bottle*.  These
bottle* should not be filled full and should be vented to relieve axeass
-------
pressure.  Venting, is highly recommended.   A No.  70-72  hole  drilled  in  the
container cap and Teflon  liner has  been  found to  allow  adequate  venting wichou:
loss of sample.
    5.2.6  Container Mo.  6  (Silica  Oei).   Note the  color  of  the  indicating
silica gel to determine whether  it  haj been completely  spent and oake a
notation of its condition.  Transfer the silica gel from  its iapinger co  its
original container and seal.  The teeter may use  a  funnel co pour the silica
gel and a rubber policeman  co remove the silica gel from  the ispinger.  The
small amount of particles chat may  adhere to the  impinger wall need  not be
removed.  Do not use water  or other liquids to transfer the  silica gel  since
weigr   rained in the silica gel  impinger is used  for moisture 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.; g,
    5.2.7  Container No.  7  (Acetone Blank).  Once during  each field  test, place
LOO ml of the acetone used  in the sample recovery process into a labeled
container for use in the  front half field reagent blank.   Seal the container.
    5,2.8  Container No.  8  (0.1  N Nitric Acid Blank).   Once  during each field
test, place 200 ml of the 0.1 N  nitric acid solution used in the sample
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  (5* Mitrie Acid/lOS Hydrogen Peroxide Blank).  Once
during each field test, place 200 ml of  the) 5* nitric acid/101 hydrogen
peroxide solution used as the nitric acid impinfmr  reagent into  a labeled
container for use in the)  beck half  field reagent  blank.  Seal the container.
    5.2.10  Container No. 10  (Acidified  Potassium Permanganate Blank).  Once
during each field teat, place) 300 ml of  the acidified potassium  permanganate
solution used as the impinger solution and in the sample  recovery process inco
» labeled container for use In  the)  back  half field  reagent blank for mercury
analysis.  Semi  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).  Ones) during each  field test,
place 50 ml of the 8 N hydrochloric acid used to  rinse the acidified potassiua
permanganate ispinger* 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 dish.  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 lost  during shipment.   If •
noticeable amount of leakage has occurred, either  void the sample  or use
nethods, 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 in  Figure A-3.
    5-3-1  Container No. 1  (Filter).   If  partieulata  emissions are being
determined, then desiccate  the filter and filter catch without heat  and weigh  ::
a constant weight as described in Section 4.3 of Method  5-   For analysis of
•etals, 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  Parr1 Bombs.   Add  6  ml of
concentrated nitric acid and * ml of  concentrated  hydrofluoric acid  to each
vessel.  For microwave heating, microwave the ssmpls  vessels for  approximately
12-15 minutes in intervals of 1 to 2  minutes at  600 watts.   For conventional
heating, heat the Parr Bombs at l40"C (28**F) for  6 hours.   Than cool  the
samples to room temperature and combine with the acid digested probe rinse as
required in Section 5-3-3. below.
Motes:  1. Suggested microwave heating times are approximate and are dependent
           upon the number of samples Heine  digested.  Twelve  to  15  minute
           heating times have bean found  to  be acceptable for  simultaneous
           digestion of up to 12 individual  samples.  Sufficient heating is
           evidenced by sorbent reflux within the  vessel.
    '•   2.  If the sampling train uses aa  optional  cyclone, the cyclone catch
           should be prepared and digested using tarn  same procedures described
           for the filters and combined vita tarn digested filter  samples.
    5-3-2  Container No. 2  (Acetone Rinse).   Mot*  tarn level  of liquid  in the
container sad confirm oa tarn analysis sheet  whether or not leakage occurred
during transport.  If a noticeable amount of leakage  ham occurred, either void
the sample or use methods,  subject to the approval of tarn Administrator, to
correct the final results.  Meaaure thai liquid in  this container  either
voluaetricslly to •! ml or  gravimetrically to ±0,5 •• Transfer the  contents to
an acid-cleaned tared 250-ml beaker sad evaporate  to  dryness at ambient Figure
-------
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                                                                                      Fractional
                                                                                            Mltk
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-------
temperature and pressure.   (IF participate emissions  are being  determined.
desiccate For 2
-------
 ..          -3-'4-2, b«low.
    5. 3.U.i  Convention*! Difettion  Procedure.   Add  30  ml  of  50  percent nitric
acid and heat for 30 ainutti on * not  plat*  to  Juat  below  boilinf.  Add 10 al 3f
3 percent hydrofen peroxid* and heat for  10  more ainutaa.   Add 50 al  or hoc
water and heat the sample for an additional  20  ai iutee.  Cool, filter the
staple,  and dilute to  150 ml (or the appropriate volua* for the  expected setais
concentration*) with water.
    5.3.U.2  Microwave Digeation Procedure.   Add 10  el  of  50  percent  nitric
acid and heat for 6 alnutaa in intervale  of  1 co 2 ainutee at 600 Watts.   Allow
the iaarpl* to cool.  Add 10 al of 3  Percent  hydrogen peroxide and heat for 2
no re ainutea.  Add 50  al of hoe water  and heat  for an additional 5  minutes.
Cool, filter th* aaapla, and dilute  to 150 eJ. (or the appropriate volume  for  the
expected aatals concentration*) with water.
    Note: All alcrowave heating CiM*  given  are approjilaate and  are dependant
upon the number of saaple* being digeated at a tlae.  Heating tlaea a* given
above have been found  acceptable for simultaneous di feet ion of up to 12
individual aaiplca.  Sufficient heating la evidenced by solvent  reflux within
the veaael.
    5.3>3  Container No. 5  (I«pinger«  445)-  Haaaure and record the total
voluae  of this saaple  to within 0.5  al.  Thia aaflple ia referred to aa Fraction
3.  Follow the anal/eia procedure* deccribed ia Section 5.U.3.
    5-3-6  Container No. 6  (Silica del).   Weigh the  spent silica fel (or  silica
gel plua iapingef)  to  the neareat 0.5  g uaiag a balance.  (IMa  step
may be  conducted  ia tha fiald.)
    5.U Saaple Analyaie.  For aach  sampling train,  five individual samples  are
generated for analyaia. A achamatic identifying; each eaapla aad the prescribed
saajple  preparation  and aaalyaia ache»a ia above in  Figure A-3.   Tbe first two
saaplea. laba>lad  Fraction*  IA  and  IS,  conaiat of taa digeated saapla* froa tha
front half of tba train.  Fraction  1A  ia for ICAP or MS analysis aa daacribed
in Section*  5.4.1 and/or M-2-  Praction IS i* for datersUnation of front half
aareury aa deecribed ia Section 3.4.3,
    The back half of th* train waa uaad to prepara  tte third through fifth
saapla*.  The third aad fourth saapla*, labeled Fraction* 2A and 28. contain
tha digeated saaplas froa th*  H,0 and  HN03/H,0, lapingera 1 througa 3-  Fractior
2A it for ICAP or AAS  aaalyaia.  Fraction 2S will be analyaad for mercury.
    The fifth sample,  labeled  Fraction 3. coaaiau  of th* impLnger contents  snd
-------
rinses froa the paraanfanata  Ispinfwrs U and 9.  This sasple u analyzed for
Mrcury u described In Section 5.*».3.  Tha total back hair Mrcury cacch i$
determined froa the sua of Fraction 2fi and Fraction 3.
    5.4.1  ICAP Analysis.  Fraction 1A and Fraction 2A are analyzed by ICAP
using EPA Method 200.7 (<*Q CFR 136. Append!* C).  Calibrate the ICAP, and set -p
an analysis profraa as described in Method 200.7.  The quality control proce-
dure* described in Section 7-3-1 of this Mthod ihall ba followed.  Recooaended
wavelenrth* for UM in the analysis of the prioary. secondary, and incerferring
oetals are listed below.
                        ElesMmt            Wavelenfth  (ra)
Arsenic
Beryl liua
CadaluB
ChrosM.ua
Ued
Nlckal
Zinc
Aneiaony
Bariua
Ccpp«r
Nanfanes*
Stlanlua
Silver
Tlxalliusi
Alumlnua
Iron
193.696
313-042
226.902
267.716
220.333
231.604
213. 356
206.833
*55.<*03
324.75*
257.610
196.026
328.066
190.864
308.215
259-940
Tha wavelenfthsj lisjtsjd SJT«  rernamaniled because of  thslr sensitivity and overall
acceptance.  Otter wavmleoftlui My b« subatlcutad  if  ttey eta provide the
needs*! sensitivity and are  traatad with  tte  saasj corrective  techniques for
spectral int«rfareac«.
    Initially, analyis) all  saaplesj for tte tarfat  astala plus iron and
alualnua.  If iron sad aluaimai  are present  la tte saaple, tte saaple aay have
to be dilutsjd so ttet each  of ttess) eleaants Is at •  concentration of less than
50 ppa to redue* tteir spectral  latarfarencsa on arseelc and lead.
    Note:  When anslyilnc saaplas la a hydrofluoric acid ntrla, an aluaina
torch should be usad; sines all  front half saaples will contain hydrofluoric
acid, usa an aluaiaa torch.
-------
    5.U.2  AAS by Direct Aspiration Mid/or Graphite Furnace.   If analysis of
oetals 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 aethods should be applied  for each  target  a«tal.  Table A-2
should also be consulted to determine posaible interferences and techniques :c
be followed far chair minimization.  Calibrate the instrument  according  to
Section 6.3 and follow the quality control procedures specified in  Section
7.3-2.
    5.U.3  Cold Vapor AAS Mercury Analysis.   Fraction IB. Fraction  2B, and
Fraction 3 should be analyzed for eercury using  cold  vapor atomic absorption
spectroscopy following the eethod outlined in EPA  Method  7**70  or in Standard
Method* for Water and Was tracer Analysis. 15th  Edition,  Method 30 3F.  See up
the calibration curve aa described in Section 7.3  of  Method 303F.   Add
approximately 5 el of each saatple to BOD  bottlee.  Record the  amount of  saeple
added.  The aeount used is dependent upon the expected levels  of mercury.
Dilute to approximately 120 si with eercury-free water.   Add approxlaately  15
ol of 5 percent potassium permanganate  solution  to the Fraction 2B  and Fraction
3 samples.  Add 5 percent potaesium permanganate solution to the Fraction IB
sample as needed to produce a purple solution lasting at  least 15 alnutes,  A
ainiaum of 2? el is suggested.  Add 5 ml  of  90 percent nitric  acid.  5 el of
concentrated sulfurlc add, and 9 •! of'5 percent  potassium persulfate to each
sample and each standard.  Oisjeet the solution in  the capped BOD bottle  at 95s'
(205*F) in a convectloo oven or water bath for 2 hours.   Cool. Add 3 ml of
hydroxylamine hydrochlorlde solution and  aix the) sample.   Than add  7 el  of
stannou* chloride to each saaple and analyie Ijsmedlately.

6.  Calibration
    Maintain a laboratory lot of all calibrations).
    6.1  Sampling Train Calibration.  Calibrate  the  taavlinf train  components
according to the indicated sections) of  Method 5i  Probe  Mossle (Section  9.1):
Pitot Tube  (Section 5-2); Metering System (Section 3.3);  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 as outlined  in Section 4.4.   Profile  and calibrate the  instrument
according to the instrument manufacturer's  recommended procedures using  :he
-------
              TABLE A-2.  APPLICABLE TECHNIQUES.  METHODS.  AND MINIMIZATION OF  INTtKLHthCK Km AAS ANALYSIS
Metal
Sb
Sb
Aa
Ba
Ba
Ba
Cd
Cd
Cr
Cr
Technique
Aspiration
Purnaca
Purnaca
Aspiration
Aspiration
ftu.sc*
Aapiratlca
Puroaca
Aspiration
Purnaca
Method
Mo.
70*0
70*1
7060
7060
7090
7091
7130
7D1
7190
7191
Wavelength
(M)
217.6
217.6
193-7
553-6
23*-9
23*.9
226.6
226.6
357-9
357 9
Interfei
Cause
1000 ag/al Pb
Ni. Cu, or acid
High Pb
Arsenic vulati -
zation
Aluainiua
Calciua
Bar iua ioni zation
500 ftm Al
High Me & Si
Ba in optical path
Absorption & light
acat taring
Aa abova
bceaa chloride
Plpet tipa
Alkali Metal
Absorption I acatt
2OO ag/L calciua
4 phosphate
*ence.
Miniaiztttioi)
Use secondary wavelengla ol ^Ji , | am.
Natch aaaple 1 standards m id concentration
or uae nitrous OMide/aceiylene riaaw
Secondary wawnlpnirih rtr /<•<••»» mmu-t im
Spiked saaplea i add nickel nitrate solution
to dlgeetatea prior to analyses
Use Zeeann background correction
High hollow cathode current 1 narrow band set
2 aL of KC1 per 1OO aL of saapla
Add 0.1| TLduride
Uae •etltod of atandard additions
Optiaiaa paraawtara to aJainlza effect a
Background correction ia required
Aa above
Aaaonlua) ohaaphate uaed aa a aatrla aodifler
Uae cadaiua-frae tlpa
KC1 i on J zation suppreaaant in aaaple i stand
Consult Manufacturer's literature
All calciuM nitrate Tor a know conatant effect
and to elJainale eTfect of phosphate
(continued)
-------
TABLE A-2 (CONTINUED)
Metal
Cu
Fe
Pb
Pb
Nn
Ni
Se
A«
Tl
Tl
Zn
Technique
Aspiration
Aspiration
Aspiration
Furnace
Aspiration
Aspiration
Furnace
Aspiration
Aspiration
Furnace
Aspiration
Method
No-
7210
7300
7420
7*21
7460
7520
77*0
7760
7MO
7Ml
7950
Wavelength
( — >
324.7
248 1
28J.1
20-3-3
279-5
2J2.0
196.0
326.1
276.8
276.8
211-9
Interfe
Cause
Absorpi t scalier
Contaaination
217.0 nm alternal
Poor recoveries
403.1 na alternat
352-'l nm aliernai
Fe. Co. 1 Cr
Nonlinear reopons
Vulltallty
Adaorpt 4 scatter
Abaorpt I scatter
AgCl insoluble
Viscosity

Hydrochloric acid
or chloride
High Si . Cu 1 P
Con 1 a* j nm mil
'ente
Nmiaizalion
Consult manufacturer's nauii.il
Greul care taken lu avuxJ cuniaBiinal ion
liuckground correction required
Main a aodirier. add JU ul. ui (ihusphorus acid
to 1-mL of prepared saaple in soapier cup
backg round correc 1 1 on requ 1 1 CM!
hut: kg round correction requn-cd
MairiH matching or a nilruu^-uxide/acety Tlaae
Sa^tle dilution or uae 352. .jked saapleij or atandad addl
Palladium is a suitable aairim audifler
jii I'tini ILM reaovea Cu an
-------
above standard*,  'ihe instrument calibration  should  be  checked  once  per  hour.
If the instrument do*s not reproduce  th*  concentration* of th*  standard  within
10 percent, the coaplet* calibration  procedures should  be  performed.
    6,3  Atoalc Absorption Spectrometer - Direct Aspiration. Graphite  Furnace
and Cold Vapor Mercury Analyses.  Prepare the standards a* outlined  in Section
k.k.   Calibrate the apectroaeter using these  prepared standards.   Calibration
procedures are also outlined  in the EPA aethods referred to in  Table A-2 and in
Standard Method* for Mater and Maatewater.  ijth Edition,  Nathod 303F (for
aercury).  Each standard curve should be  run  in duplicate and  the  Bean values
used to calculate th* calibration line.   Th*  instrument should  be  recalibrated
approximately once every 10 to 12 saaples.

7.  Quality Control
    7.1  Sampling.  Field Raagant Blank*.   Th* blank sample* in Container
Numbers 7 through 12 produced previously  in Section* 5.2.7 through 5.2.11.
respectively, shall be processed, digested, and analyied a* follow*.  Digest
and process Container No. 12  content* par Saction  5-3.1.  Container No. 7 per
Section 5-3.2. and half of Container  No.  8  per Section  5-3-3.   Thla  produces
Fraction Blank 1A and Fraction Blank  IB froa  Fraction Blank 1.   Coabine  the
remaining half of Container No. 8 with th*  content*  of  Container No. 9 and
digest and proce** th* raaultant voluaw par Section  5-3-1*-  Thla produces
Fraction Blank 2A and Fraction Blank  2B froa  Fraction Blank 2.   Container No. 10
and Container No. 11 content* are Fraction  Blank 3.  Analyse Fraction  Blank IA
and Fraction Blank 2A par Section 5.4.1 and/or 5.*-2.   Analy**  Fraction  Blank
IB. Fraction Blank 21. and Fraction Blank 3 par Section 5.4.3.   The  analysis of
Fraction Blank LA produca* th* front  half r a agent  blank correction value* for
th* aatal* except aarcuryi th* analysl* of  Fraction  Blank IB produces  the front
half reagent blank correct valu* for  aarcury. Th* analyvla of  Fraction  Blank 2A
produca* th* back half reagent blank  correction valu**  for th*  **tala  except
aereury. valla aeparat* analyai* of   Fraction Blank* 2B and 3 produca  th* back
half reagent blank correction valua for aarcury.
    7.2  An ettaapt aay be aada to detarala*  if th*  laboratory  reagent*  used in
Section 5.3 -aiirtil contamination.  They ahould b*  aaalyiad by  th*  procedure* in
Section 5-1.  Th* Adainiatrator will  dat*rala* afMthar  or not  th*  laboratory
blank reagent valua* can be uaed la th* calculation  of  th* stationary  source
teat result*.
-------
    7.3  Quality Control Staples.  Th*  following quality control samples should
be analyzed.
    7.3.1  ^CAF Analyeia.  Follow  the quality control ihown in Section 8 of
Method 6010.  For the purpoee* of  a  thre«  run teat  aeriea. theae requirements
hav* been modified to Includ* the  following;  two inatrument  check  standard
runs, two calibration blank run*,  one interference  ch*ck sample at  the
beginning -f the analyau  (must  be within  251 or analyze by standard  addition).
on* quality control tuple to check  the accuracy of the calibration standards
(must be within 25% of  calibration), and one duplicate!  analysis  (Bust be within
51 of average or repeat all analyaii).
    7.3.2  Direct Aapiration and/or  Graphite Furnace AAS Analysis  for Arsenic.
Beryllium. Cadmium. Chromium, Lead.  Mercury, Nickel, and Zinc (and Antimony,
Barium, Copper, Mangane«e. Phoiphorua.  Selenium, Silver, and  Thalliua.  if
aeaaured),  All sawplea should be  analysed In duplicate.   Perform  a aatrix spika
on one front half eaaple  and one) back half aeaple or one combined  sample.   If
recoveriea of leas than 73 percent or greater than  125  percent are obtained for
the  aatrix ipike. aoalyie each aacple by the) method of  addition*.   A  quality
control sample should be  analysed  to check the  accuracy of the calibration
standard*.  The reeult* muat be  within  101 or the calibration repeated.
     7.3.3  Cold Vapor AAS Analyai* for  Hercury.  All samplea  should be analyi«d
in duplicate.  A quality  control aamplfahould  be analysed to check the accuracy
of the calibration standard*  (within 10% or repeat  calibration).   Perform  a
matrix apike on on*  aampl* from  the nitric i*jpiiif*r portion (au*t  be  within 251
or samplea muat be aaalyied by  the) method of ataadard addition*}.    Additional
information on quality  control on be obtained  from ffA Method 7470 or in
Standard Kethod*  for Hater and Waatewater. 15th Bdltion,  Method 303F-

3.   Calculation*
     8.1  Dry OM  Voliaw.   Uaia§  che data from thla cave,  calculate v.(iia, . the
dry  faa sample volum* at  •taadard  eonditlona  aa outlinmd in Section 6.3 of
Method 5-
     8.2  Volum* of Water  Vapor and Noiaeurm Content.  Uaiac the d* a obtained
tvm thl* tmat. calculat* the) volume of watar vapor Vv<0li)  and the moiatura
content BVI of the ataek  fma.  U«e Equation*  5-2 and 5-3 of Method 5.
     8.3  Stack Oaa Velocity.  Uainf the data from  thla  taat and Equation 2-9 of
Method 2, calculate)  the average  atack  fa* velocity.
-------
    3.1*  (totals  (Eacept Mercury)  In Source Saeple.

    3.1.1  Fraction 1A. Front  Half,  Metals (except  Hf).   Calculate the  aaounc

of each aetal collected in  Fraction 1  of the •ampling train using the following

equation:

                                «rB  '  C.  F,  V..,.^                      a,.  L-


where:

    Mril • total eass of *ach eetal  (except Hf)  collected la the
          front half of  the laepllng train (Fraction i),  ug.
     Ct * concentration  of eetal  In saaple Fraction LA ae reed fro* the
          standard curve (uf/ml).
     Fc • dilution factor (?t   •  the inverse of the fractional portion of the
          concentrated laeple  in  the solution actually used in the instrument to
          produce the reading  C,.   For example, when the dilution of Fraction LA
          1* froe 2 to 10 el.  F<  -5).
                volume of digested saaple aolution (fraction 1),  el.
    8.4.2  Fraction 2A.  Back Half.  Natals (except Hg).  Calculate the amount of
each Beta! collected  in  fraction 2  of the sampling train using the following

equation.


                          **» '  c» p»  v.                                   B«- 2*

where:

    MH, • total mesa  of  each metal  (except Hg) collected in the back half
          of  the  sampling train (Fraction 2), ug.
     Ct • concentration  of metal in sample fraction 2A. as read from the
          standard curve (ug/ml).
     Ft • aliquot factor, volume) of fraction 2 divided by volume of aliquot
          fraction 2A.
     V  • volume  of digeeted sample analysed (concentrated fraction 2A). al.
    8.4.3  Total Train,  totals (except Hg).   Calculate the total amount of «ach
of  the quantified  metals collected in the sampling train as follc


                     "t  " <"f.  - «W *
•If Fractions  1A and 2A are comhlned. proportional aliquots must be used.
 Appropriate changes must be aade in Equations 1*3 to reflect this approach.
-------
where:
    M.  •  total  aaaa  of  each  seta!  (separately stated for each aetal)  collected
          in  the saapling train,  ug.
  Mfn9  •  blank  correction value  for  aaia of aetal detected in front half
          field  reagent  blank,  ug.
  *»„<,*  olank  correction value  for  aa*a of aetal detected in back half
          field  reagent  blank,  ug.

Nbte:   If the Manured  blank value for the front half (•,„,)  ia in the range  C.;
to A ug [wham  A ug  equal* tha value determined by aultiplylng l.U ug par iquar<
inch (l.U ug/ln.]) times the actual  area in aquare inches (in.1)  of the filter
used In the ealsaion saaple],  efh, aay be) vuad to correct the ealasion sample
valua («,„): If •rht  exceed* A ug, the greater of cha two following value*
(either I. or II.) eay  ba uaad:
    I-   A ug,  or
    II.   the leaaer  of  (a) arht. or  (b)  5 percent of mrit,
If the aaaaurad blank valua  for  tha  back half (•khk) it in tha rang* 0.0 to 1
ug, athB aay ba uaad to correct  tha  emiaiion saaple valua («^J;  if a^^ exceeds
1 ug,  tha greater of tha two following valuaa aay ba uaad:  1 ug  or 5 percent a
"Hh-
    8.5   Mercury In  Source Sample.
    d.5.1  Fraction  IB.  Front  Half,  Hg.   Calculate tha aaount of  aarcury
collected in tha front  half. Fraction U of tha aaapllng train uaing tha
following aquation:

                                       a
                               »tf. •—^-'
                                      Vfli
where:
    Hgfh • total aua of  aarcury collected in tha front half of tha aaapling
           train (Fraction  1),  ug.
     0,,, • quantity of  aarcury  in anal/tad staple.  ug.
 vieln t • total volume of  dlgvatad aaaple aolutloa (fraction 1).  al.
    vril • voluaa of Fraction IB analyzed, al.   Sea tha following Note.
      vri| la tha actual  aaount  of Fraction IB analy»«d.  For axaapla,  if 1  al
of Fraction IB wara dllutad  to 100 al to brine it Into tha proper analytical
range, and 1 al of tha  100-al  dilution waa analysed, Vfll would ba 0.01.
    6.3.2  Fraction 2B  and Fraction 3. Back Half. Hg.  Calculate tha aaount  or
aarcury col lee tad in Fractiona 2 and 3 uaing Equation* 5 and 6. reapectively.
-------
CilcuJ.it* th« total Mount of Mrcury colltcttd  In  tin back half of th« sai

train uiinf Equation 7-
                                               * V.8li, ,               Eq,  5
                                         v 4
                                          rn
where:
           J  • total **•• of Mrcury colltctad in Fraction 2.
           a  • quantity of Mreury in analytad taipl*. u§.
        vfli  • voluB* of Fraction 2B analytad. •!  (MM Mow  in
               Section 8.5-1).
             ' total voluM of Fraction 2,  al.
what*:

              total aaaa of a«rcury coll«et*d la  Fraction 3. uf.
         ,
       Q,h. • quantity of avreury 1ft analyiad  vaapl*. uf.
        VM • voluM of Fraction 3 aaalyiad, al  (MM Hota in
              Sw:tlon 3. 5-1).
     . «i n. 3 " total voluaa of  Fraction 3.  al.
                                                                        -  7
           K • tot«l MUMI of •arcury colltcta4 ia  U» back half of th«
               train, uf.


    6.3-3  Total Train lareyiy Catca.  Calculat* tha total aaouRt of Mrcury
coll«cta4 la thft MBpllng train uaiaff Bquation A.
                       •, . (Bf,. - HiV,,.)  * (i^k  •  iaV.J                Eq. 8


wharv:

      Nt • total aaaa of Mrcury collaetad la taa taapllnc train, uff.
   Hffllk • blank correction valu* for aa*a of Mrcury wtactad  In front half
           flald raafnt blank, uf.
-------
                 correction value  for aass of aercury detected  in back
           half field reagent blank, ug.

No_ce;  If the total of the measured blank values  (Hgfmft  • Hg,fta) is in the r
of 0 co 3 ug. then Che total aay be used to correct  the  eaission saaple value
(Hgrn - Hg,n); if it exceeds 3 ug. the  greater of the following two values say
be used: 3 ug or 5 percent of the  eaission saaple value  (Hgfh  • Hgbpi).
    8.6  Metal Concentration of Stack Gas.  Calculate the concentrations of
arsenic, berylliua. cadalua, total chroeiua.  lead, aercury,  nickel, and zinc
(and antiaony, bariua, copper, eanganeae. phoaphorua, •eleniua, silver, and
thalliua. if aeaaured) in the stack gaa (dry  baala.  adjusted to standard
conditions) &a follows:

                               c.  ' K*  (Nt/v»<.i«) )                      Eq-9
where;
        Ct • concentration of each aetal  in  the  stack gaa. ag/daca.
        K, • 10*1 eg/ug.
        Nt • total «a»s of aach aetal collected  in the  saapllng train, ug.
   v.did) • volu«* of f*» saaple  aa eeaaured by the dry gaa eater, correczed
             to dry standard conditiona, dacsj.
    3.7  Isokinetic Variation  and  Acceptable Reault*.   Saa« aa Method  5,
Sectioru 6.11  and 6.12.  respectively.

9•   Bibliography
    9-1  Method 3037  la  Standard Methods for the Eaamination of Mater
waatewater. 15th Edition,  1980.  Available froa the Aaerican Public  Health
Association. 1015 18th Street  H.W.,  Washington. D.C.  20036.
    9-2  EPA Hethoda  6010,  7000. 7041,  7060. 7131,  7421.  7470. 77<*0, and
Teat Method* for IValuatiflg Solid  Waate; Ptiyaieal/Chemical Methods.  S
Third Edition.  Septeaber  1968.  Office of Solid Waate and Eeergency Response.
U.  S. TTni li ijiaeiiiil Protection Agency,  Waahingtoe.  O.C. 20460.
    9.3  EPA Hethod 200.7.  Code of Federal Regulation*. Title 40,  Part 136.
Appendix C.  July 1.  1987-
    9-4  EPA Method*  1 through 5.  Code of Federal Regulations. Title 40,  Part
60. Appendix A, July  1.  198?.
-------
APPENDIX J.2




  PM10/CPM
-------
Federal  Register  / Vol. 55,  No.  74 /  Tuesduv. AD.-;! -.".  1WU
                                                                                                 and  Reauiauons
Sun;;///if* flo/c, for directions in the UPC of
ihn equation tor 0 in (he setup caiculaunrs.
  •V4   C«---«d« Impactor. The purpnir ni
rjhliralmc a Cascade impactor u In
Oi-.lermme the empirical consent (SIX,),
which  is specific to the impador and which
ptrmiti ihe accurate determination ol ihe eul
>i7.e of ihe impaclur napes a! Held  condition*.
ll la nm necessary 10 calibrate each
individual impaeior, Onn* iifi impuctoThan
linen calibrated, the calibration dug can be
applied to other tmpacion o( identical demgn.
  5-'.l   Wind Tunnel Same ai in  Section
5.11 ot thii method.
  S,4.r   Puriiclf Generation System. Same as
in Section 5.3.2 of Ihii method.
  H.3   Hardware Configuration (or
Calibrations. An impacnon nape Constrains
un nerobul to (ofm circular or rectangular jots.
which  urc directed toward a suitable
substrate where the larger aerosol  particles
arc collected. Far calibration purpone*. three
stages  of the caacude impHClnr thull lie
discussed and designated culibrulion  itupes
1. Z. and  3. The tint calibration maae consists
of the cullcction substrate of an impuction
mane and all upstream surface* up to  and
including the nozzle. Thii mny mcludf other
urevcdinR imoactor Hugos. The second and
third cnlibrmion ilagei consul of each
respective collection substrate and all
upMrewm surfaces up lo but excluding (he
collection substrate of the preceding
culihruuon tinge Thii may include
intervening impaclor napes which  are not
designated ae calibration itayet- The cut size,
or D»-  of the adjacent calibration iinget aholl
differ by a factor ol not lest than l.J and not
more than :.0, For example, if the fir*i
calibration flag* h«i • DH of 12 nm. then tho
DM of the downitream itagc ahaii be between
6 and 8 nm.
  5.4.3.1  It it expected, but not necessary.
that the complete hardware assembly will be
used in each of ihe templing rum of ihe
calibration  and performance deiermjnadoni.
Only the first calibriiiion itage must be tesicd
under isokinetic lampling conditions.  The
second and third calibration itagua mull be
calibrated with Una collectnsn-Jubiiraie of lha
preceding calibration ita?e in place. 10 lha'
gus (low  patterns ousting in field operation
will be simulated,
  5.4.3.2  Each of the PM» singes should be
calibrated with the type of collection
substrate, viscid material (such a* gn«M) or
flust Hbcr. uied in PM» measurements. Note
that moil nutenali uied at •ubimiet at
elevated temperature! are not viicid at
normal laboratory condition*. Tho  eubtuvie
mbtena! used for calibration* ihould
mini mile particle bounc*. yet t>« VIKOIU
enoup+i to withstand ermien or deformation
by ;he  impactor jell and not interfere  *nh
the procedure for meaiuring (he collected
PM.
  5.4.4   Calibration Procedure, Establish tail
panicle generaior operiuan and verify
panicle size microscopically If
monodUpenity ii to be verified by
nvensurcmenii at the beginning and the end
of the run rather than by an integrated
sample, these measurements shall b*  mode  at
this lime. Measure in triplicate the  PM
collected by the calibration uage (m)  and ih«
PM on all surfaces downitream of  the
                                        r;nlil>ra\ion n.ipi- |m"i lor .ii ol thr
                              flaw m:cs  md pnnicle IIZP cnmbinHMuiw
                              shown in T«bte i ol this melKud  Trchmqucs
                              ol nialb mtiijuremenl tn«v inriudr 'hi- usi- ol
                              d dye and jpecirophuiomcter. PMTlirlf s an th<-
                              upstream side of a jet plaie ahull bt- includea
                              wi;h (he substrate downstream- enccpi
                              «a«lumfnj(et of particle!', which thai! be
                              included with the preceding or upmream
                              substrate-  Us* the following formula to
                              calculate the collection efficiency 1E1 tot euch
                              stupe,
                                544.1  Use the lormula in Suction B^JJ
                              of this mrlhod lo calculate thn iLaqdard
                              di viation \r\ lor the replicate measurements.
                              II if exceeds C.10, repeat ihe replicate runs
                                S.4.4.2  U>* the following formula to
                              calculate the averape collection efTicieBcy
                              (E.^) fur each sei ol replicate mennurctncnts
                                £...-(£,* EC-- E=]/J
                              when; Ei, Ee. and EJ are rt-pllcole
                              measurements of E.
                                i.4.4.3  Upe the followmp formnU Hi
                                     - S(k r'ir nar.h
                                            Sik.
                                                      Ad,
                              whrrc:
                              D = Afrwlynamic diameti.-r gf the Itsi
                                  particlu. cm (g/cn1)^.
                              Q = Cat flow rate through the culibmion
                                  mage at inlet condition!. cm'/»*c.
                              u."Cat viscoiity, micrapoiie-
                              A •Total cross-icctionni area ot iht juts of
                                  the calibmtion itafiv. cm1
                              d. = Diameier of one jet of ihe calibrulion
                                  Huge, cm.
                                5 4.4 4  Dvtermme Sik« (or each
                              calibrntion sufie by plotting £„ vrrsuc Sik
                              on log-log paper, Slkl, ii  the Sik number el SO
                              percent efficiency. Note that nonicie bounce
                              can cause  efficiency to decreoM at hlph
                              valuei of Stk. Thus. SO percent efficiency can
                              occur at multiple value* of Sik. The
                              calibration data should dearly indicate the
                              value of Slku (or minimum panicle bounce.
                              Impaclor efficiency versus Sik with minimal
                              panicle bounce ii characterized by a
                              monuiotucatly increasing (unction with
                              constant or increasing slope with increiisinp
                              Sik.
                                J.4.4J  The Sth» of the flrel cnlibration
                              stage can potentially decrease tvith
                              decreaiing nouia sue. Therefore,
                              calibraliona should be performed with
                              enough rural* aizca to provide • measured
                              value within IS percent of any nonle site
                              uMfd in PMt. meaaurvmcnu-
                                5.4.1  Criteria For Acceptanca Plot EM for
                              tha first calibration stage v«raui the square
                              root of the ratio of Sik to Slk» on Figure 9 of
                              this method Draw a imooth curve through ill
                              of the polnn. The curve shall be within tha
                              banded region.

                              6. Calculation*
                              a.I Nomenclature.
                                B_- Moisture (mcuoo of stack, by volume,
                                  dlnjentionlcts.
                               , Ci -Viscosity constant. 31.11 mioropoise
                                  for *K (51-05 mtcropoiM for *R|.
                                C, - ViKoiity conitanL OJ7Z micmpouw/
                                  'K (IL207 micro|xjise/*R).
  Ci i Ymconn conmuni. 1,oS •: l(t~'
   (nn.Ttipoi»WK:f3.24 • 10'1 rmcrupaisi-,'

  C. a Viscnaity eonsia^l. S3.147 micrnpinut;/
   frkcnun Oi.
  C>- Visco.iiiy constant, 74.143 micmpoise/
   fraction K-0.
  LU m Diameter ol particle* hnviru: a SU
   percent nnibuhiliiy of prneimiiun. >jm_
  I, =• Slack gut fraction Oi, by volume. dr>
   Lam
  k, .O.HlM'K/mm llgjlMM "(I/in. I IB).
  M,«alVel molecular weight of mixKii pan
   through Ihu PWi« cyclone, p/g-mulu |ll./
   !l*-niDlr).
  M.«iDry mnli-ciilar wrighl »'*luck piiii. p/
   p-mole (Ib/lb-rr.olc).

   mm lip (in. HK>
  P." AUiidlulc slack presnurc. mm UK (In.

  Q.wTuhil cyclon* flow rale at wet r.j'cltmc
   conduioni. m'/min [ft',mini.
  Q.iu«<"Total ryclone flow rale nl it.iftdai J
   condiiions. dacm/min (ilacf/miiij.
  TB- Average absolute iempHrniurb of rfry
   mi:!cr, 'K ('RJ.
  T.o Averttpe alisuliilv stuck gin
    tcmpiTBlur*. 'K (*R).
  V.4Mt» Volume of WSILT vapor in fas
   lumi'ie (sluniiard conditional, son Iscf).
  OiToUl  wmpling bmc. min.
  ti^," ViBcosiiy of mixed cyclone gHS.
   micropaitc.
  M,M- VUeojiiy of Jiandurd uir. ina.l
   micro poiM.
  0-2  Analynii of Cflsoido Impaclor Diilu.
Use (he nanulaclurcf s mt
procedure* to rtn«lyT.« diiiK  from i
impuciort.
  6.3  An.ilysi* of Cyclnne  Oula. Use the
following procedures to analyze dntu from a
sinfiln sinpe cydone-
  8J.1  PMu'WeighL Dci«tmine the PM
catch In the PM» range from the iitm of lhe>
tvcijhti obtained from Contninrr Numbers 1
and 3 IUM the acetone blank.
  6 3J  Tctal PM Weight (oplionall
Determine the PM catch (or greater than PM..
from the wui'pht otitained from Container
Numl.er z Ion ihe acetone bUink. anil add  it
lo the PMi* H'eighL
  8JJ  PM» Fraction. Determine the PM..
fraction of the iota) paniculate wciphi by
dividing the PMn piirticulBfB weigh! bj' ihe
toial paniculate weight.
  8.3.*  Aerodynamic Cut Size. Calculate  the
s:ack gui viscosity ai follows:
  OJ.4,1  The PM» (low rate, at aciuul
cyclone condition*, ia enleuloied ai follows:
    Q,-
     I4  Cnlculale the molecular weiehl un
a wot t*a»ia of the Hack gas ai CoKowi:
  M.- MJl-8») + iaJMB«J
  OJ.4J  Calculate the aciiwl D> ot tha
cydn-ne (of the given conditions ni follows:
-------
14272	Federal  Register  / VQ|.  55. No. 74  / Tuesday, Apr:! I", 199O /  Rul»s  and  Regulations
                                           D» = 5,
             T.
            M,r.
                                                                          Q.
where 3, =0,Q;"S-i for metric uir,!S i
for English uni'.i).
  fl.3.5  Acceptable Rriuiu. The rcsahi arf
BCCCplsU* if l*u toi-.damns urc r.'.i;! The
first is iha: »U cm •, 0« c ll 0 u~- T!ie
iccor.d is !hn! no sarspbnfi poinis i.'e ouliide
A3»,n  and 4P,U, or thai 83 pcrccni •; I  < 120
perceni and nc more than one sampling poini
i.<> ou'sid: lpKII, and 
Mccsurement with Csfisaa.it Ssmp.'imi .t
EPA/000/3-68-057.
BILUKO COOt flM-M-M
-------
              Federal Re^ifier  / Vol.  55, No. 74  /  Tuesday, Apnl 17.  199U  /  Ruit:s  and Repuiulions
                                                                                14269
HRii-nilil}' inch lh«t flow dinlurlmncti an-
•  'nmiznd.
  41.:.;  The n-iup calculnlivni- c*n be
r>i-rlnrnif J by using ihu foliuwmn prvccuuntk.
  i I.C.. i  In order 10 maintain « cut n:xe of
in un: in i:,- gizmg device, the Huw rjif
(hrnuEri (he niing dri'ict mull b*- rnaim
dosiyn spccificalions in Fipure 3 of thin
method. use ihr equetieni in Fipur* 4 of lhi»
mtlhoil lo calculate it:ret orifice he«dj lilll
UIH ;n  ihe average nucL lemperimu-e. And ihe
ulhcr Iwu ot lempffnilurss —2H "C [.= 5)1 "Kl
uf tin- average jinck lernpcrMture. Uir all
calculated al lhe ui'eruer Black temprniiur*
*s Ihc \itLiSurc htmil Inr Ihs iambic flow rain
ii* Ion? as iht stuck lemperniurx during lite
run in within ;g 'C ISO  'KJ of the •vcrunt
*lac» temperature. If the IIHCJC lemnerwlurv
vaues by more than :a LC (So T). ihun une
Ihe appropriate AH.
  4.1.2.2.2  IF the  iizinji duvici: in H cyclone
lhai'dijes not meet the design sptrifiCJliuni
in Fipure 3 of ihi!  method, us' the equuliimi
in Figure 4 of this  m*thtid, cicppi use ihn
procedures in Section  5.3 of this  nielhuJ in
dpic'rmin* Q., the  corrrc: cyr!oni« flnw run-
fn: ;. 10 j.m size.
  4.1.2.1.3  To ittiew b nuzzle, uie lliv
.•yum Kirn inFicunrSofihifcmttliod lu uilculnir
ip,,™ and &pM for each nozzle til M three
inmpurHiurei. If she suing device ii a cydonn
thai dam noi meet ihe dctiiin sprcificBli&rui
in Fipun; 3 of ihn  method, ihp exumple
worksheets can br used.
  4.1,2.2,4  Correct the Method ".' pliui
n-wding". to Method 201A pilot reading] by
multiplying the Method 2 pilot readings by
Ihe i-u  --e of a ratio of the Afethod 201A pilot
Cf.cfficu-ni to the Method 2 pilol coefficient.
Select the nozzle for which ip,,. bnd ^p,..
lirnckel nil of the corrected Method 2 pilol
readings. If more than  one nuzzle meed thia
nrquirenienl. uleci Ihe no tile giving the
grcaitjl jvmmetry. Note ihul if the expected
pilol reading for one or more points is near a
limit for a chosen  nozzle, ii may be cu;side
the limili al the time of the run.
  4-1,».S  Vary Ihe dwell lima, or aiunplioj;
time. At each uavenc poini proportioflaleiy
wilh lh« point velocity. UM ihe aqualian* in
figure 8 of ihjt method to cdlcuLala  lh« dwall
nmc al the firit point and al each lubaequaril
point. It i* recommended ;h«l Ihe number of
-•mnutei mingled Ht each paint Uc rounded to
the ntaresi 13 jeconds.
  4-1.3   Preparation of Collection Train.
Same at in Method S. Section 4.1J.  excepl
nmii direc'.ioni about • glai* eye!one.
  4.1.4   Leak-Check Procedure. The fixing
device ik removed before the peit-leat leak-
check (o prevent arj- ditturOance of the
collected sample prior to inalyeil.
  4,1,4.1  Prijiesi  L'lk-Chacki A prelect l«ak-
uheck of the entire sampling train, including
the sizing device,  u required U»e the leak-
check procedure in Method 3. S*etion 4.1.4.1
to conduct a preiesi leak-check,
  4.1.4.1  Leak-Check* During Sample Run.
Same ai in Method 5, Section 4.1.4,1.
  4.1.4.3   Poit-Tsil Leak-Cheek. A Isuk-
check ii required  at the concluiion of each
jamplmg run. Ramava the ci'done befora the
leak-check to prevent the vacuum cnaied by
the cooling of ihe  probe fro- diiiurfaing the
cullocunJ um|Hc und u*c ine proccciure in
Mrlhod S. Seciion 4.1.4.3 ir cunauri t puai-
  4.1.S  Method 3J1A Train Opermiun.
us in Method 1  Svction 4.1 J. encepl UM th«
procedure* to thu nectiun lor iiokmelic
sampling *nd flow rate  uriiufunt!nl. Maintain
(he Haw rate uicututed in Section 4.1J.2.1 of
(his meihud througiinui the run provided the
j'.ack temperature n wuhin 2£ 'C (SO T) of
the iemu*rsiure u»td lu calculair iH. If tiuci
tcrnpeniiu/ei van b>* more than 28 'C (50 'Kl.
usr the appropriate AH vaiue O'tcuiatMi in
Suction 4.1X2-1 of thii method. Calculnle Iht
dwell lime »i each iruvcrw point ai in Figure
fi of Ihit method-
  4.I.B  Calculation of  Percanl UukmelJt
Ratr und Aerodynamic Cut Siza (Owl.
Cdjrultir percent inokinetic rate and UM laer
Caiculmiank. Sc-rtion 6  uf thii mtUind) to
dotcrmiue whether the ten ci*dun^ in
 Section S.3 of ifiii method lu tudbrale (he
 cyclone. The purpoae of the  PS Ie6» arr in
 cnnform Ihut the uyclunt and naizlc
 rombuiunon hai the dcairecJ ihurpnm nf cul.
 Conduct the  PS teiti in a wind i urine I
 detcrUwd in Section J.Z.1 of ihia method und
 particle  generation lyilem deioibed in
 S«-ctior 9-L2 of Ihii malhod. Uie live parlidu
 sizci and three  wind velocities HI Hi ted in
 Tdble 2 uf Ihi* mclhod A minimum of three
 rrplicuir nmuiuremcntj afcolluclinn
 tfficicncj- thatl  tit pertonmtd lor e«ch of tlie
 IS condilioni luted, for a minimum uf 45
 mcaauremanta.
   S.2-i   Wind Tunnel Perform ihr
 caUbmtion and PS lean in a wind tunnel (ur
 equivalent tail apparatui) Capubl* o(
 BSublijMing  and maintaining the required gai
 stream velocities within 10 percenL
   5.Z2  Panicle CHneretion Syiiem. The
 panicle generation lyilem liiuU he cnpuble uf
 prutiucmg iolid monodUoennd dye pnrtictea
 H-iih ihr :rus» median aerodynamic
 di.irnclrn  ipecified in Tiible 2 of thii meihud.
 Perform the panicle liie diUhbttiun
 venficatmn on an integrated aampie aliiuined
 during thr lampling period of each tell. An
 acceptable alternative ii to  verify the- uze
 distribution of jamplei obtained before and
" after each tetL  with both lamplei required  tu
 rntrtti the dinmeler and nionodilpcrsiiy
 rcquiremenia for an •ceaplable ie»i run.
   Siil   Eaiublieh the aize of the aolid dye
 parti del delivered to Ihe leit teciion of the
 wind tunnel  by uiing the opcnting
 parameter! of the particle generation iy,ilem,
 and verify them durinq tha leiis by
 mierotcopic  examination of tjmpiei or the
 parliclea collected on a membrane filter. The
 particle me. ai ntablUhed by the opening
 parameten of the gcneratian jystem. shall be
 within the tolerance ipecified in Tublo 2 a!  •
 ihia method. The preciiion of tiic particle size
 verifiejlion leehnjque ihall be al leeii ±
-------
14270       Federal  Register /  Vol. 55.  No.  74  /  Tuesday. April 1". 1990 /  Rulea and  Regulations
opersung parameters oTlhc particle
generation system.
  5,2.2.1  Certify ihe monoJispe-'sify of the
panicles for each test either by microscopic
inspection of collected particle* on fillers or
by olher suitable monitoring techniques such
us an opiical particle counter followed by a
multichannel pulse height analyzer. If the
proportion of multiple!* and satellites in an
aerntol exceeds 10 percent by mass, the
particle aeneialion ivilcm n unar.repliiliip
lor the purpose of lhi» icsl. Multiplies nrt
partielei that are HRslomrrdlrd, and satellites
are psniclei thai are imalter than the
sp*cjfied size range.
  5.2.3  Schematic Drawings,  Schematic
drawings of ihe wind tunnel end blower
system and other information ihowing
complete procedural deiailt of the ten
atmosphere generation, verification, and
            dehven' techniques shall be furnished with
            calibration data lo the reviewing apenry.
              S.Z.I  Flow Measurements. Measure ttir
            ci'done air now raiei kith a dn> gas meter
            and a nonwaich. or a calibrated orifice
            system capable of measuring flow rates 10
            wiihin 2 perceni,
              S.2,5  Performance Specification
            Procedure, Eatabli'h  (eat panicle gencraiar
            operation and verify  panicle size
            rnir.ioscipically If monoduperry is to be
            verified by measurements at the beginning
            and the end of the run rather than by <>n
            integrated sample, these mpnujremrn'j may
            be made ai ihis lime.
              5.2.5.1  The cyclone cut sire, or DM, of a
            cyclone ia defined hen aa the panicle sue
            having • SO perceni probability of
            penetration. Determine ihe cyclone flow rale
            al which DM ii 10 Mm. A augg-3iud procedure
            is 10 vary the cyclone flow rule while  keeping
e constant rm'ucle sin of '.0 fc.-n. Measure 'he
PM collected in ihe cydun: 1m,). inc eml hific
|m(j. and the filter |m,l. Calculate cyclone
efficiency (E,) for each How rale as follows:
                   m,
                     ,-f m,)
                               100
  i.:.5.2.  Do three replicates ind calculate
ine overage cyclone eflicicncy ;£...„,] as
follows;
When F.I. Em. and Ea are replicate
mcdsurtmenis of £..
  1253  Calculute the standard deviation
If) lor the replir.iiie meuflurumentii 01 E, as
follows:
         (£,'+£,•+£.•)--
If im. Sample
lung enough lo obtain r5 percent precision
on  total collected moss  aa determined by the
precision and the sensitivity of measuring
technique. Determine separately the nozzle
catch f m.]. cyclone catch (m,), cyclone axil
lube (M,l. and collection filler catch (m,] for
each panicle size and nominal gas velocity in
Tab!* 2 of this method.  Calculate overall
efficiency (E,) *s follows:
            following the procedures described in (his
            section far determining efTiciency-
                 (m,+m.J
                              X100
             (m,-f m,-t-m,+m«)
  5 r.5.6  Do three replicates for each
 combination of gas velocity and particle size
 in Table 2 of this method. Us* the equation
 below le calculate the iveng* overall
 efficiency [EV«,il lor ouch combination
            Where E,. E>. and E> are replicate
            measurements of E..
              SJ.3.7  Uaa (he formula in Section SJ.3J
            lo calculate 
            shall be 50^0-9 pamni at 10 pm.      .
              3J  Cyclone Calibration Procedure.  The
            purpose of this procedure ia to develop the
            relationship between Dow rala. gaa viscosity,
            gas denaily. and Dt*.
              SJ.l  CalcuUt* Cyclone Flow Rale.
            Determine flow rein and D»"i for lima
            difTenni porticl* tan between 5 >»m and 19
            jim. one of which shall be 10 MID. All liiea
            mual be determined within OJ fuo. For each
            sue. use a dtflsrenl lemperaiurt) wiihin 80 *C
            (10e *F] of the tampermtura at  which Lhe
            cyclone ia to be u»ed and conduct triplicate
            nino. A luggeited procedura is lo keep the
            panicle ii» constant and vary the Dow rate.
  5.3,1.1.  On log-lftfl graph paper, plot the
Reynold* number (Re) on the abscissa, and
i he a qua re root of Ihe Stokes SO number
|{SiW)r*| on the ordinate for each
temperature. Use the following equations lo
compute both values:
             Re -
                       » M™.
                       q.,
 where:
  Qj,,-Cyclone flow rate. cmVsec.
  p«Cas density, g/cm1.
  d^-Diameter of cyclono inlet, cm.
  H^ -Viscosity of gai through the cyclone.
    micm poise.
  0«- Aerod>-n*mic diameter of a panicle
    having a SO perceni probability of
    penetration, cm.
  5.3.1.2.  UM • linear regression analysis lo
 determine the alope (n) and the Y-mtercepi
 (b). Us* the following formula to dutermine
 Q. the cyclone flow rate required for a cut
 size of 10 (*m-
                                                                     T.   ,-/'—
     w »*«• f              1        f   T-   1
a—r[(»«*)-bj        [—]
"where:
   m = Slope of the calibration line.
   b-y-iniererpl of the calibration line.
   Q.-Cyclone flow rate for a cut siu af 10
               d • Diameter af nozzle, an.
               T.-Suck git temperature, R.
               P. • Abaolule stack pressure, in. Hg.
               M.~ Molecular weight of Ihe alack gas. lb/
                 Ib-mole.
   K,-4.077X10".
   5J.1.3  Refer to (he Method 201A
 operator! manual entitled Application Guide
 for Source PM,m Measurement wiifi Consiar.:
-------
          Fed«ra! Register / Vol. 55. No, 74 / Tuesday. Apr;! 17. 19SO / Rules and Regulations
     93
     90

>   80
o
LU
u
c
yj
70
60
SO
40
30
20

10
                               1       1
17 < v < 27 m/s
              9 < v < 17 m/s
                  v < 9 m/i
                               I      III
                                           a  10
                           AERODYNAMIC DIAMETER
                                                      20
                                                         40
                                                                      • IU-49
          Figure  13.   Efficiency  envelope  for the PM10 cyclone.
•1UJMO COM IMtMO-C
-------
1426B        Federal  Regime* /  Vol.  55.  No. 74  J Tuesday. April 17.  1990  / Rules  and Regulations
Emikwun G«» Rvcvclr. Dull R«dur.iu.n.
V«mnnS.*  MA IT IB*)*
  Te*t ID. Cude: Chupcl Hill :
  Teat Locution  Baghouiu- Ouili-t.
  Teal Site' Chapel Hill.
  Test Ome WtZQtBd.
              : )U RH MIL

                      un Pan:
    TsKCi.'...,..... ............... _ ............... ;>il t
    T.lfC: ........ ....... _______ ...... ___  "I M f
    TiUOMI .............. _________ .......... _  rs.U V
   lem Prniun><
    DHionii— ....... __ .................... _.- -..in !Nwt:
    DHTOT] ____ ...... _______________ ..... i PI IN we;
    I»!NLI__ __________ ............ ... :;.:.'> i.wvc
    DP'KCL] _____ ................................  Z.;i IMVf.
            ......... ____________ ..... _ .....  ti.ra is w::
    DHSTV] _________________ ............. (j.10 1NWC
    V'(i>CMi _____ .......... ____ ....... .... 13. TM IT3
                             bO.tfc MIN
              ..... _ ....... _______ ..... _. g.ou
           __________ ..... ------ ........... SJ.QH
                                                                          r.l: M!.
                                                                          li.ii CM
    I'iltrr ...... — ........... __ ........... ____ 11.7 MC
    Inipmypr P.ikiduiT ...... - ............... O.n MC  •
rili.nl Vilun;
    HfC Km.» .-•„,,... ...... ------- ........ . 0-0 MC.
    filler llulUrf Kin*- ................... u.li Ml',
    Hiii-r niiiiik ............ ______ .......... . on ML,
         fi-p Rin*r,~ --- ........... ____ u.n MC
    OTI1TCT1		-	  u ivu.
    t)Hf«»DRIl	_	_	_  uuwii
    M: rot LH:I _		  u.--2^>.
    BlTOT LK>:i			-	  -  ('I.™
    MIKCI. i»:i	„	_	  (MUM*
    D- HC1, Iff,}	_	  - .00""
    IK At CAMMA—	-		[l !«•<«
                                                            ,'trrluccd Untn

                                             Sv,.k X <-h.:, :ii  (I T,' SIX)..— ........... ___ .............. !.'!••:-
                                             •*!,,i> {;«» Mumiuif p."i _______ ............ ----- ....... ••:.«
                                             Sufli|iii< Fmw R«ic IACCM) ...... - ....................... (UHK
HucvL-lf Kl(>» Ri.lu I ACFMI ..............................  0,1TIHI
Jvrceni hvcynlt- _________ ........................................ -Itt.f
l»i.i>ni"H Rr.ijci [' I ................ _ ............... _ .......... .1.1.1
    P'DARU ..... ____ .......... .............. ;«.!»; IN we
                                                  :   (UMi
                                                                  <)
                                                                         (MG/DNCMI
                                             ,Gn/ACF|
               (Gfl/OCF)
> 1 '
Cycum* l ' 10 'S ' 356 ! KB
f)ickup Pi"tfr , M . 	 i, ' : M5

i , ;
0 OlTSf* ! 0 3J470
000368 1 C 0*332
COI76Z ' 0 03bO:

3 53701
1 907
S "'

                                             EG" f»
Maihod Z01A— Datern:n*tion of PM,.
Emiuuim (Contiuit Sampling Ralr
Procodurv)

Ji. Applicability and Principle
  1.1   Appliciibilily. This T.cihuJ a;t()iie) to
111* in-tlack measuremenr of pa.-.ie-jlale
mailer (PS') eminioni equdl (o nr leu Ui«n
an Rcradycamic diameter of narainully 10
(HM..1 from lialionary sgunres. Ttie EPA
rccujnues Lhn condcniible cmiuianx not
collected by an in. Hack method ire also
PM.i. and tKai emunonj that coninbuie to
ambient PM,, levelt sr* ihe  sum of
condensible emmionj und emujioni
nea.iu.-ed by  an m-nack PM,. melhotl. lucti
m thii method or Method ZUl. Therefore, lot
establishing tource coniribuliont 10 nmliienl
!*velj of PM,fc such ai for emission invcniory
?urpoiei. EPA luggesti thai  source PM,.
nieaiurement includa both In-siack P?.l,. and
CDndensible emiuiong, Condennble
emission! may be measured  by an impinger
jnalvsu in combination with ihn method.
  1^   Principle. A gas sample it axtincied »(
u coni'.ani flow rcte irirough an in-iut;!
siziog device, which separeiei PM greater
than PMi. Vanatign.t from iiokinelic
sampling condiiioni are maintained within
ivell-defi.ied limiti. The paniculate ma*a ii
dtlermmed gravimeiriuilly ii.'ier renoval Of
uncomfaincd we
r. .\ppamuM
  Sole: Melhodi ciled in ihii mrthud ,irt PHPI
nf 40 CFH pan M. app«ndi* A,
  -1   Sampling Traia A schrnatic i-f the
Method 2B1A sampling train ii shown in
Kigure l of this method With thi exception of
(he PM,.  sizing doyico end in-siack niter, thit
train is the ume as an ETA Method 17 train.
  2.1.1  Nozzle. Siainlesa neel <3ic or
^r.ivilent) with • iharp lapennl lending
  ..T Llvven niculuf thai imet the
api-caficaikm in figure 2 of thii method are
recommended A larger number of nonles
with small noatie increments increase the
likelihood that I Sir.pla no^J* Un be Jled fur
thu er.tin travei-se. If the i-.o-iiu do not mcci
the dflbign spcci'iralion* in Figure Zol ihn
ice l hod. (hen the nonlc* must meet lha
cnienn in Sectiun S 2 of thia meihud,
  Z.1.2  PM,. Sixer. Stainleai neel (316 or
equivulcnll. eap-ble of determining tha PNf<.
(ruction. The tiling device shall be eittior •
cyclone that me«U iht  ipeciricaiiooj In
S«ctifin SJ of th;i method or a ca««ada .
impactor that hai been caltbraietl using the
procedure in Section S,4 of thii method.
  2.1 J  Filter Holder. B3-mrn. iujnlM* iteoL
An Andanen filter, part number SE2*4, baa
been found to ba acceptable for the m-nack
filler. Kotr, Mannon of lr«de name* ur
specific product* doei not constitute
aadone;nenl  by 'he Environmental Protection
Agency,
  2.1.4  IHtol Tube. Same as in Method 3.
Sectiun 2.1.3. The pilot linen shall b? made of
heal militant tubing «nd attached lo ihe
probe H-ith itainlvia neel filling!.
  2.1.9  Probe Liner. Optional, seme as in
Method V Section 1.1.2.
  2.1.0  Differential PrMaure C«UB«.
Condenser. Metering System, ftaromcler. and
Cat Density Determination Equipmtml. Same
at in Method S, Section* 2.1.4. and 2.1 7
threuj-n 2.1.10. re'pectively.
  2.2   Samnle Recovery.
  2.L.1   Nowlt, Sizing Device. I'roKe, and
Kilter Hbider Brushes, Nylun bnjtl* bfmho*
with stainless steel wire shafts and handles.
properly aizeii and shaped (or cleaning the
notzie. siting dedvics, prubn or probe line;.
and filler holders.
  Z-L3.  Wuah Bottlei. Ciuaa Sumple S!oru|ia
Container*, Petri Diahoi. Crudualed Cylinder
lind Jtuldrce. Pliislic ~  :• : • Containers.
Funnel and Rubber .!s..;_ r, j.-., and Kunncl.
5
in Mi-thru] 5. Sucliun 4.1.1. except use ;hc
direction) on nozile size selection and
sampl'nt cnie  in this miiiKud. Ulf of any
norjl* ^c(r,pr than 0.16 in. in diameter
require a sampling port di'r-^cr of 6 inchuj,
Alio, the required ma i -  -   -bar of
trnvenr points at ar .             1 be 12.
  4.:il   The iizing ; .    .  : .   ^e in-ilack
or RiHintuined  a', slack leir.prraiLro durinp
iumpi:ag. Tha  blockage effect of the C5R
sampling assembly will be m:nirniil if the
cross-sectional ire« of the san-.pling
aaacmblx* ia 3 percent or less of the cru.s*-
sc-ctiujinl urea  of Ihe duct. If (he LTOSI-
K-c'.iur.iil urea  of the assembly is preulcr Ih.m
1 uercent of ihe crosj-secnonal area of ihu
ducL then either deiermina the pilul
coefficient at mimpling conditions or use a
standard pilot with a known cuefficivnl in »
             with the CSR sampling
-------
               Federal Reister  ' Vui. 55. No. "4 / Tuesdav.  Aj.-.i
            ?;;:ivs ard Reflations
                                                                                                I-S2M
                                 Cyclone  Inte-ior D'!-Tigrisir
                0.10 in.  :-
                                                             Z
                                                L
                                           •Deuo
   I
   :i
_L
                                                          Heup


cm
inches
Dimensions (iQ.OZ cm, ±0.01 in.)
Om
1.27
o.sa
0
4.47
1.76
Oe
i.sa
0.53
B
1.£3
0.74
H
6J5
2.74
b
2.24
0.83
I
4.71
US
S
t.S7
0.62
Hcvp
US
0.89
Ocup
4.45
1,75-
o;
1.02
0.44
D0
124
0.43
                      Figure 12.   Cyclone design specifications.
B1LLIMQ COQC I»«-W-C
-------
14266       Federal  Register / Vol. S5. No.  74 / Tuesday.  April 17.  1990 / Rules  and  Regulations
      SOURCE  PW,o Cyclones and Noz-
  zle ComDinanons
                            eolMcion
                            bl-CK!" l.T.S
                            |nd Figmc
                            13.
2. C*oon* cul  I urn
 TABLE 2. PARTICLE SIZES AND NOMINAL
    GAS VELOCITIES FOR EFFICIENCY

Panic*)  i     Twgei gat *«iociiiai (m/ieel
       i   7-1.0   1   tSsi.l  1   Z1-2.S

  (X Hau moflian Htoornirmc diaff.tii*

•O.UHO COM I
-------
1
Run
Code
Swnplti
ID
FIIHl
ID
fi*mpl*f
Oiltnlillon
S»mpllng
Location
NonU
Diimtlti ID (In}
Optraloi (1}
Due
Slul
Tlmt
End
Time
Sampling
Ounllon (mlnl
OGM
(Initial)
DGM
(llntl)
Snnplt
tfolum, t'l'l
Dull Manantt Iff Leieltd ind 2aro«d>
Mign*h«llc» Z*fotdT
Run
Tlmt










Pail No
TI«>|.










f>f
Pllol










AH
S«npl>



.






DGM
Volumi










AP
loMl










SUcN
TcmpciilufB " (CT)
Sl.ifk Si » lie
Trcssure '"' ^*jO|
Annhlcnl
f etnperalni* i'*}
Amblrnt
PiMiurr <'' "91
G»l
Velocity
Syilvni, tt«l Chfcii
{ » IS In. Hg)



P
Inlfl











fi P
Dec pell










T,
Sl.ck










G» Compo«lllon
%CO, %0, %CO
Molllur* Conlrnl
Pllei Ltik Ch*ch
(Poi) |N«9»
fiolei
Tl
Hf cycle










Tl
Piob*










T«
irE










T»
DGM










                                                                                                                                                   If
                                                                                                                                                   I
                                                                                                                                                   «
                                                                                                                                                   en

                                                                                                                                                    *
                                                                                                                                                   ui
                                                                                                                                                   O.
                                                                                                                                                   n:
                                                                                                                                                   T3

                                                                                                                                                   J.
                                                                                                                                                   (V
                                                                                                                                                   (A

                                                                                                                                                   Ol


                                                                                                                                                   CL

                                                                                                                                                   ja

                                                                                                                                                   03
                                                                                                                                                   C

                                                                                                                                                   £U~


                                                                                                                                                   O

                                                                                                                                                   5
                                                      Flguro 10,  Example EGO Procedure claia sheet,
                                                                                                                                                   10
                                                                                                                                                   cn
                                                                                                                                                   C-J
-------
14264       Federal  Register / Vol.  55. No. 74 / Tuesday.  April IT.  1990 /  Rules and Regulations
Run no. •
Fiilrr no.
                                          Comain*r
                          'art
Amount liquid lost during
Acelone blank volume, ml _
Acelone wash volume, ml
  ( = 1 - (3) -
Aceionp blank cone,, ntp/m£ [Equalion
  5-1. Mnlhnd 5) _
Acetone wash blank, mg (Fqunlton 5-5,
  Methods] _
3....
 Tom	;..
                 i
 L*M «e«or*« Win*....!..
      I of PM*	!..
                                         Container rnjmo
                  Vi«iq.ni o' pincuiaic
                     "man»i, mg

                  inW  i  Tar*  ,
 i»M action* Wink.

                                                                                 Tom oan
-------
             FwiaraJ  RegMler / Vol. 55- No- 74 / Tuesdcy, April 17, 1990  /  Rules  and  Regulations
	
• lack fat. *»t basm,
M. Ib/lb mole.
rVtmuT u|)iln>«m a! °- 0,6
U"E. in. Jig,
Cat inslyaii:
VO. 	

comem. B,..
Calibration dau.
in.
Pilot ^••"'fncicnl C. =
T dial LFE calibration ' Viscosity of dry narJt
constant. X,. a ;ui;
Tulsl LFC cslibral.tin ^« 152.418-^ 023.11
eotuuni. T.. = T.*J.^53 <10"'
Ahjolui* pressure T,;t-0.i31'l7 l"*Oi). - _ 	
upsiream of LFT1
ViicotHj-ofgaiuTiol-I Con.iann;
LFE
^•i-2"^1,?^,

                                    Kiol.STSIxlO'1-
     It,-01139
               Mi«T. D.'C.  f_l] ,,,
                             T.
[i -o.aMtf (i , -
                                                                     (i -
Figure S. CxampI* »orkjh»ct Z. total LTT,
       head.
         X,   180.1 K,



             K. K.

       Bl ° SM.J^X,='
Tola! LFE pretiurc head;
^^Ji^ni —pi t«*pj "™          tn  H^fl
Daromeiric pressure, PB^ in. Hg«i 	,
Absolute slack pressure. P. in.

Average stack temperature, T..

Meier temperature, T_ 'B =
Molecular weight of stack gas. dry basis,
  Me. Ib/lb mole -	
Viscosity of LFE gas. pm. poise=	
Viscosity of dry stack gas, p*   „
                                                                       Abiolulu pressure upjircam 01 LTJ

                                                                         Calibration data:
                                                                       Nozzle diameter, Dn, m. =	
                                                                       Pilot coeffidenL C, =	
                                                                       Recycle LFE calibration conatunt.

                                                                       Recycle LFE calibration constant,
                                      K, - IJ732X10"1-
                                                           T, P.*— m.
                                                    M^T. D.'C.   , P.
                                         K. - 0.1339	  — -  H
                                     1C.  -
                                                                   B,J
_£.    l^n  ,

  X,    180.1 X,
                                                   B,-
                                                        .K,
                                          Pressure head for recycle LFE:
                                                        "	in,H,O
-------
14262      Federal Register / Vol. 55, N'o. "4 / Tuesday. April 17. 1990 /  Rules and  Regulations
  Figure 9, Example workshee
recycle LFE pressure head-
BILLING COOI IUO-W-M
                          t *
-------
                    ORIFICE METER
DRY GAS METER
THERMOCOUPLE
  TOTAL FLOW
THERMOCOUPLE
 DRY GAS METER
  MANOMETER
   SOLENOID
RECYCLE FLOW
OUICKCONNECT
  TOTAL FLOW
OUICKCONNECT
                                                                                                n
                                                                                                a.
                                                                                                ?o
                                                                                                Q
                                                                                                CM
                                                                                                 -
                                                                              HEPA FILTER
                                                                               TOTAL LFE
                                                                               nECYCLE LFE
                                          RECYCLE FLOW
                                            SOLENOID
                                         TOTAL FLOW
                                          SOLENOID
                                                                                                V.
                                                                                                o
                                                                                                Ul
                                                                                                n.
                                                                                                (u
                                                           s
                                                                                                pa
                                                                                                c
                                                           O)

                                                           b.


                                                           10

                                                           5T

                                                           o

                                                           Ul
                         Figure 5,  Example EGR control module (rear view)
                                  showing principle componenls.
-------
142SO
Federal Register /  Vol. 55.  No.  74 / Tuesday.  April  17,  TWO / Rule* and Regulations
                                EXAMPLE EMISSION GAS RECYCLE SETUP SHEET

                                               VERSION m MAY Iflflfi
     TEST 1.D-: SAMPLE SFTUI'
     RUN DATE; 11/24,'se
     LOCATION: SOURCE SIM
     OPERATOR(S): RH |B
     NOZZLE DIAMETER (IN'J: .-5
     AVERAGE TEMI1IKATTHK (If. 2tii4),.
     AVERAGE VELOCITY invsRO: u.n..
     AMBIENT PRESSirKE (IN HGJ: 29-92-
     STACK PRESSUTU, [IN Hai|: .10 ________
                                           	_, r.AscdMi'OSiiii
                                           	   11:0=10.0%	
                                           	   02 = 20.9%..,	
                                                                                       	 MU-2C.H4
                                                                                       	 Mw=:-.rs
                                                                                       	   (LD/U
Dl'(HTO)	
O.D2C	
.rai	
.035..,.
       iso
  SAMPLE
   TOTAJ.
  RECYCLE
     %RCL
        .58
       1.HD
                    i.aa
                    1ST
                    54*
                     .78
                    1.87
                    2.44
101
 .40
1,90
UP
C1%
 .M
1,19
174
57%
 GS
1.88
100
sss
 .71
1.86
-4?
53%
                                            TARGET PRESSURE OUCH'S

                                                 TEMPERATURE (F)
   ir:
   .«w
  1.M)
  :.9:
  ins
   .55
  I.8P
  2.77
  58*
   .M
  1.R8
  2-93
  SS%
                                                            t.m
                                                            2.94
1.9O
2.80
iflt
 .S3
1.89
ran
50%
 .47
1.92
2.37
(CH
 5T.
1-ffl
:.K
59%
 .B2
l.W
:.ta
   .72            .71
  1,8»           1-89
  2.50           2.S3           i!
  SZX           53%           53
Kgur* 6 Example EGR wiup aheel.
 .40
1.92
3.no
Q:I%
 .M
1J1
2-35
59%
 .61
1.90

57*
 69
1.90
2.59
 .45
1.9:
302
«3'.t
 .53
1.91
:.o«
60%
 .00
1.91
                                                                                          .87
                                                                                         1.90
'..U
 AS
1,93
3.05
03%
 ,a:
1.9:
190
ecH-
 -59
1.91
2.74
Sn;
 .(f,
1.91
2.S."
5S':.
Barameinc
Slack italic
  pressure, P,. in.
  H;0.
Ai'entit Hick
  lernperaltrs. (^ "F,
Meier lemperaiurt
  U. T.
GUI anclysii:
  «-COi _____________
  Fraction moitmr*  —
    conicni. B.T
                           Calibrsiion data:
                             Nozzic diameier,
                               D, in.
                             Pi I o( uclficieni.
                               O-
                             &H«. in. 11:0.
                             Molecular »«iphi
                             of itack  gii. dry
                                            (%CO,)-rOJ2
                                                Molecular weight of
                                                 •tack gal, wet
                                                 bain:
                                                Absolute slack
                                                 preiture
                                                                             j/lb
                                                                            in. Hp
                                 K-M&72 D»« 4H» C.1  (1 -8.) "  Hi (t,-t-4aO) l>
                                                               M, ((.4-480) P
Dcf ir«d mtinr onHce rirv->5ufe (iHJ for
    velocity head of itarJt pat |ip|:
4H-Kip-	in. H;O
                           Figum 7, t.iampie wurlshr-tl 1, nit ler urifio;
                           prciRura heiid calculMtion.
                                                  pmtum.
                                          P«v In- Hg.
                                                Absolute Hack
                                                 prvttun. P_ in. Hg.
                                                Ai'flraga alack
                                                 (empersturt, T, *fL
                                                                T_ "R-
-------
           Federal Register / Voi  55. No. ~* I Tuesday. Aorii :7, 1990 / Rules and Regulations        14237
PM 10 CYCLONE
                             i- .-I
          FILTER HOLDER
             (63-mm)
                            i       r
         EGR NOZZLE

  TYPE-S  PITOT

         RECYCLE LINE

rSTACK THERMOCOUPLE
                                                                 RECYCLE THERMOCOUPLE
                     Rgure 3.  EGB PM10 cyclone sampling device.
-------
re
            FINE TOTAL
              VALVE
         COARSE TOTAL
             VALVE
         VACUUM GAUGE
                                            FLOW
                                         MAGNEHELICS
   DUAL
MANOMETER
                                                        7
                                                   TEMPERATURE
                                                  SELECT SWITCH
       TEMPERATURE
         INDICATOR
                                                                                      DRY GAS METER
                                                                                        SAMPLE BACK
                                                                                      PRESSURE VALVE
                         FINE RECYCLE
                            VALVE
                                                                                      COARSE RECYCLE
                                                                                           VALVE
                                                                                                             • i

                                                                                                            I
                                                

                                                                                                              0.
2.
Ol
5"
M
                                  Figure 4,  Example EGR control module (Ironl view)
                                          showing principle components.
-------
             PITOT TUBE
                                         EGR PROBE ASSEMBLY
RECYCLE
  LINE
  10
                                                                           HEATED
                                                                           FILTER
                                                                           HOLDER
              NOZZLE  FILTER
                       HOLDER
                                  METHOD 5  '
                                  IMPINGERS  |
                                             I
	,  METER AMD FLOW
   1 CONTROL CONSOLE
                                                                                                            EXHAUST
                          H
                          n
                          m
                          O.
                          (B
                                                                                                                                 TJ
                                                                                                                                 a
                                              SEALED PUMP
                                 Figure I. Schematic ol tha eihaual gat recycle Iraln.
                          CL.
                          JO
                          i
                                                                                                                                 CT.
                                                                                                                                 o
-------
14256
             Federal Register / Vol. 55. No. 74 f Tuesday. April17. 1990 / Rules and Regulations




Vi
/ r
~T- (H
0^
-xU
*\ ^~
r> /
./
m"*^ tJ

A --
u

              S3
              39
                                                    o

                                                    cr
                                                    u
                                                    o
                                                    jj

                                                    75
                                                    E


                                                    u
t
(3
j"^*
i
F
if
S| Sw
/ 4 o3
b
«
3
&
u.
                       40
-------
              J^deral Register  /VQ|.  55.  JS'Q.  TJ  /  Tuesday. Apnl_17.  1990  /  Rules  and  Regulations        14253
         E.-
              (m, i.mr-* m, -f mr)
                                 X 100
  5.7.5.7  Do Ihret replicaici lor each
 combination of fas velocities and panicle
 rzei In Table : of lhi» melhod,  Calculate E.
 fur each panicle nit following  the
 procedural described in ihii itclion lor
 deiermining efficiency. Calculate the
 itandard deviation |cr) for th« replicate
 meaiurementa. If '« for three
different particle lizes between S u,m and 15
M.m, one of which shall be 10 urn. All tizei
mull be within 0.5 |im. For each stxe. UM •
different temperature within SO'C (106T] of
the temperature at which ihe cyclone u to b*
used and conduct triplicate runs. A suggested
procedure it to keep the particle sue constant
and vary ihe flow rate. Some of ihevataet
obtained in the PS lean in Section 5,7.3 may
tie u»d.
  5,8.11  On log-log graph paper, plot the
Reynolds number (Re) on the abvciiM. and
the square root of the Stoke* SO number '
[(STKn)" 1 on  the ordinaie for each
temperature. Use the following equations:
                                                                                                    Re  -
                                          where:
                                            Q^. • Cyclone flow rale cm-'/icc.
                                            p • Gas density, a/cm'.
                                            d^. •> Diameter of cyclone inlet, cm.
                                            pLo. « Viicoiiiy of gai through the cycionc.
                                              pulse,
                                            Dw - Cyclone cut sue. cm.
                                            3.0.1.2 Use a linear regrestion analysis to
                                          determine the ilop« (m). and the y-iniercepi
                                          [b). UM the following formula to determine
                                          Q. the cycloM flow  rate required-far a cut
                                          sice of 10 fin.
                              Q •
    J  (MOOHK,)*  J -|n.s-m)
                                                                               T.
                                                                             M.P.
                                                                                        m/lm-O.Si
  Q « Cyclone (low rate for a cut sue of 10
    Mm. cmj/sec
  T,  = Stack gai lemptrature. K.
  d • Diameter of nozzle, cm.
  K,  - 4.077 X  10-'.
  3,6-2.   Dircc;iorui Tor Using Q. Refer to
Section S of the ECR opera ion manual Tor
directions in using ihii expression for Q in
the letup calculations.

0. Cotculauo-j
  B.I  The ECR data reduction calculation*
are performed by (he  ECR reduction
computer program, which it written in IBM
BASIC computer language and is available
through NT1S. Accession number PB90-
500000. 5283 Ron Royal Road. Springfield,
Virginia 22161. Examples at proanm inputt
and outputs are ihown in Figure 14 of lhi«
meihod-
  6.1.1   Calculaiioni  can alto be done
manually, as ipecified in Method 3. Scciiona
6.3 through 9.7. ind 6.9 through 8.11 with ihe
addition of the fallowing1.
  8.1.2  Nomenclature.
  B, n Moisture fraction of mixed cyclone
   ga*. by volume, dimensionleu.
  C,  - Viscosity constant 31.12 BliempoiM
   for *K (SI ,05 micropoia* for *R).
  Ci  • Viscosiiy connani.
    *K (0.207 rnicrapoise/'R).
Ci - Viscoiity conatanL i.OS X 10"
  micropoise/'K1 (3,24 X 10~*mlCTOpoiie/

C • Viacoilty conatanl. U.I 47
  micropaiM/fraciion O|.
C, - Vitcosity constant. 74 143
  miercpoise/fraclion H,O.
Du B Diameter of panicle* having a SO
  percent probability of penetration, p.it.
lai «• Stack gaJ fraction ft. by volume, dry
  basis.
K, m 0.3853 'K/mm Hg (17.64 'R/in. Hg).
M. » Wei molecular weight of mixed ga*
  through the PMn cyclone, g/g-tnale (Ib/
  Ib-male).
W, - Dry molecular weighv of atacV gai, gl
  g-mol« (Ib/lb-mole).
PM • Barometer pruMurtt st umpflng site.
  mm Hg [in. Hg).
PI.I - Gauge pressure at inlet lo total LFE.
  mm HiO (in- HaO).
Pi - Abaolut* JUck prMsure, mm Hg (in.

Qi - Total cyclone flow rale at wel
  cyclone conditions, m'/roin (ft'/tnin).
Qt^ft • Total cyclone flow rait at
  standard condilons. dicm/min (d*e//
  mb).
Ta • Avcragji temperature of dry gat
  meler. 'K\"R}.
T, — Average stack gin temperature. "K
  CRl-
V^i^j •  Volume of water vapor in gaa
  lanrple (iiindard candjliona). sen (icf).
                                              XT - Total LFE linear calibration coniianu
                                                m'/Kmrnllmm htO'J (ft'/I(iBin)(ifi.
                                                rM3)]).
                                              YT - Toul LFE liaur colibraijon COWIODL
                                                dian/min (dsef/min).
                                              APT • Pretaun dilTcrennal acrosj total
                                                LFE. nm HiO, [En. K.O)
                                              0 B Total Mmpling lime. min.
                                              !!„ v Vlicomj of nixed cyclone gns.
                                                micro poiM.
                                              u^, a Viscosity of gaa laminar flow
                                                elevrenii. micropoiie.
                                              H^ m Viscosity of standard air. 180.1
                                                micro poise.
                                              U  PMi* Panieulnie WeigiU- Determine
                                            the weight of PMM by summing ihe weights
                                            obtained from Contniner Nurntwn ] and 3.
                                            leu ihe acetone blank.
                                              8.3  Total Paniculate Weight, Determine
                                            Uie paniculate ca:=h for PM greater than
                                            PMn froen the weight obtained from
                                            Conuiner Number 2 ICM iha acetone blank.
                                            and add it to Ihe PM,. paniculate  weight.
                                              8.4  PM,, Fraction. Determine the PM,.
                                            fraction of the total paniculate weight by
                                            dividing the PMw paniculate weight by the
                                            tola) paniculate weight,
                                              64  Total Cyclone Flow Ral«. The average
                                            flow rate at itandard conditions ia
                                            determined from the average pressure drop
                                            icma the total LFE and ii calculated aa
                                            follow*:

                                                     XTAP
-------
1-1S54        Federal Register  /  Vol.  55.  No-  74  /Tuesday,  April 17. 1990 /  Rules and Regulations
  The fioo. rate, gi actual Cyclone conditions.
ii culcuiaiud 19 (o!lo*i-
     Q'  =
            T,
                6.6.1  Determine the «mer fraction of Ihe
              mixed yas through the cyclone by using ihc
              equation
                                                           Q.i.MiO * V.
                                              6.B.2  Calculate Ihe cyclone gai viscosity
                                            as follows:
                                            >W- C, -t- C, T. + CiT.1 + C. U - C.  B,
                             B.G.3  Calculate (he molecular weigh) on a
                           *el basis of the cyclone gas «» follow*:
                           M, •= M.d  - e.) * ia.o(D.s
                             C.B.4  I! the cyclone mecii the design
                           •peciricaiicm in Figure 12 of ihm meihod.
                           calculate the actual D» of Ihe cyclone (or ihe
                           run B9 follow*:
                                                                                                     T.

                                                                                                    M.P.
                                                                                      Q.
                                                         wh*re jj, a 0.1502.
                                                           6.0.5  K the cyclone do«s not meet the
                                                         design tpecificatmnt in Figure 12 of ihi»
                                                         meihod. then uie the following equation to
                                                         culcuiute DM.
DM -
  6,6  Aerodynamic Cut Size. Use the
following procedure to determine the
aerodynamic cut size (D»).
where:
  m a Slope of the eslibraiion curve
obtained in Section S.B.I.
  b - y-imercepi of (he calibroiion curve
obtained in Section 5.8.2.
  6.*  Acceptable Reiuld, Accepiabih'ty of
eniiokinetic variation is the lame as Method
S. Section 8.12.
  6.7.;  If 9.0 nm < DM <11 jwn Bnd90< 1 <;
110. the reiulu are acceptable. If DM it
greater than 11 pro. the Administrator may
                                           (7.378 X 1CT T
M.P.
 T,
                                                                                   d--
              accept Ihe results. If Dm  it lest than BO pm.
              reiect the results and repeal the teat.

              7. Bibliography
               1. Same at Biblioprapby in Method 5.
               2. McCain. 1-D-.! W. (Upland Hnd A.D.
              Williamion. Recommended Methodology for
              Ihe DeierminaUon ofPartidoi Site
              Distribution* in Dueled Source*, Final Report.
              Prepared for the California Air Resource*
              Board by Southern Research Iiutilute. May
              1986.
                             3. Fanning. WE- S S Dawei. A.D.
                           Williamson. | D. McCain. R.S Martin, and
                           J,W, Rsglnnd, Development of Sampling
                           Methods tot Source PM-10 Emissions.
                           Southern Research Institute for ihe
                           Environmental Protection Agency, A prill 389.
                             4. Application Guide for ihe Scarce PMa
                           EfheuU Cat Recycle Sampling System EPA/
                           GOO/3-BS-C2&
-------
              Federal  Register  /' Vol. 55.  No.  74 / Tuesday.  April  17.  1930  / Rule?  and Resdancns
                                                                              14251
  4.1.4.3   Poil-Tei; Leak-Check. A leak-
check is required a! the conclusion of each
sampling mn. Remove the cyclone before ihc
leak-check to prevent ihi> vacuum created by
Irir cooling of ihe probe from disturbing the
cnllecicd sample and use the following
procedure Id conduct a post-test leak-check.
  1,1.4.2.1  The sample.nd* leak-cheek 11
performed ai follows: After removing the
cyclone, seal the probe with a leak-light
Hopper. Before starting pump, close the
coarse total valv« and both recycle values
and open completely the sample back
pressure valve and the fine total valve. After
turning the pump on. partially open the
coarse total valve slowly lo prevent a surge
in the manometer, Adjust the vacuum to ai
iean 3Q1  mm Hg (1S.D in. Hg) with the fine
total valve. If the deiired vacuum ii
exceeded, either leak-check  at this higher
vacuum or end the leak-check as shown
below and start over.
Caution: Do not decrease the vacuum with
any of the valvej. This may cause a rupture
of the filter.
Note: A lower vacuum may be used, provided
that i: is not exceeded during the ten.
  4.1.4.3.Z  Leak rate* in exceaa of 0-00057
m'/min (O.OCO ft'/mm) are unacceptable. If
the leek rate is toe high, void the sampling
run.
  4.1 4 3J To complete the leak-check.
slowly remove the (topper from the nozzle
until the vacuum ii near zero, then
immediately turn aft the pump. Thii
procedure sequence prevents a pressure
surge in the manometer f.uid and rupture of
the filler.
  4.1.4.3.1 The recycle-side leak-check is
performed at follows: Clow  the coane and
fine total  valves and sample back pressure
valve. Plug the sample .inlet at the meter box.
Turn on the power and ihe pump, close the
recycle vaivej, end open the total flow
valves. Adjtut the total flow Tine adjust valve
until t vacuum of 23 inches of marcury it
achieved. If the desired vacuum is exceeded.
either leak-check at this higher vacuum, or
end the leak-check and stan aver. Minimum
acceptable leak rates are the same as for the
sample-side. If th« leak rale is too hiah, void
the sampling run,
  4.1,3 ECU Train Operation. Sane a* in
Method 5, Section 4.1.3, except omit
references to nomographs and
recorr.mendationa about changing the filter
assembly during a run.
  4,1.5.1  Retard the date required on a data
sheet such at the one shown in Figure 10 of
this method- Moie periodic chtcka of the
(nanometer level and lero to ensure comet
iH and ip valuer An acceptable procedure
for checking the tero ia to equalize the
pressure at both ends of the  manometer by
pulling off ihe tubing, allowing the fluid to
equilibrate and, if necaasary. lo re-xero.
Mai-.:ain the probe temperature to within
II 'C (ZTJ T) of stack  temperature.
  4.1.3-2  The procedure for using the
example ECR setup sheet ia  as follows:
Obtain a  stack velocity reading from the pilot
manometer (4p), and find this value on lha
ordinal* axia of ihe setup sheet. Find the
stack temperature on the sbsciiia. Whore
the** two values Lnteneci an the differential
pressure* necessary  to achieve isokinetlciry
and 10 pm eui siw (interpolation may be
necessary),
  4.1,3,3  The top three number* are
differential pressures (in. H,O], and  the
bonum number is the percent recycle at these
flow settings. Adjust the total How rate
valves, coane and Pine, to the sample value
I AH) on the letup sheet, and ihe recycle How
rait valves, coarse and fine, to [ha recycle
flow on the setup sheet.
  4.1.3.4  For startup of Ihe ECR (ample
train. Ihe fallowing procedure is
recommended. Preheat the cyclone in the
slack lor 30 minutes. Close both the  sample
and recycle coarse valves. Open the fine
total, fine recycle, and  sample back pressure
valves hallway. Ensure that the nozzle is
properly aligned with the sample stream.
After rnl:ng the dp and stack temperature.
select the appropriate AH and recycle  from
the ECR setup sheet. Start the pump and
timing device simultaneously- Immediately
open both the wane total and the coarse
recycle valves slowly lo obtain Ihe
approximate deiired values. Adjust  both the
fine total and the Tine recycle valve* to
achieve more precisely (he desired values. ID
the ECR flow system, adjustment of either
valve will result in a change in both tola! and
recycle flow rates, and a slight iteration
between  the total and recycle valves may be
necessary, Became the sample back pressure
valve controls the total flow me through the
system, it may be necessary to adjust this
valve in order 10  obtain the correci flow rate.
  Note; Isokmeiic sampling and proper
operation of the cyclone an not achieved
unless the correct aH and recycle flow rate*
are maintained
  4,1,3.5  During Ihe lest run. monitor the
probe and filter temperatures periodically,
and make adjustments aj necsnary lo
maintain lha desired temperature*. If the
aample loading is high, the filter may begin lo
blind or the cyclone may clog, Tha filter or
the cydona may be replaced during the
sample run. Before changing the filler or
cyclone, conduct a leak-chock (Section 4.1  4.2
of this method). The total portlculaia miss
shall be the sum of all  cyclone and Ihe filter
catch during the run. Monitor stack
temperaturt and  Ap periodically, and make
the necessary kdjustmonti in sampling and
recycle Row ratal to maintain isakinelic
sampling and the prepw (low rale through the
cyclone. At the end of  the run. turn off the)
pump, close the coane tolsil valve, and
record the final dry gas meter reading.
Remove the probe from the stack, and
conduct a post-test leak-check as outlined in
Section i.l ,4J of this method.
  4.1.0  Calculation of Percent Lsokinelic
Rate and Aerodynamic Cut Siia, Calculate
percent isokineuc rale and the aerodynamic
cut size (Oa\ (see Calculations. Section a of
this method) lo determine whether the test
wag valid or another test run should be made.
If there wai difficult in maintaining isokinetic
rates or a On of 10 inn bccnus* of source
conditions, lha Administrator nay b«
corumlied for possible  variance.
  4.2 Sample Recovery. Allow the probe to
cooL When lha probe can be ufely handled.
wipe off all external PM adhering to the
outside of the noizle. cyclone, and nozzle
attachment and  place a cap over the* nonle
10 prevent losinji or painmg PM. Do not cap
the noMle lip tightly while the sampling lmin
is cooling, as this action would create a
vacuum in the Filter holder, Disconnect thr
prolte from the umbilical connector, and take
the probe to thr cleanup site. Sample
recovery should be conducted in t dry irinuor
area  nr, if outside, in an area protected from
wind and free of dust. Cap ihe ends of Ihe
imptngen and carry them to the cleanup site.
Inspect llir components of the train prior to
and during disassembly (o note any abnormal
conditions. Disconnect Ihe pitol from the
cyclone. Remove the cyclone from the probe.
Recover the sample ai (ollcwj:
  4.2.1  Container Number 1 (Filler). The
recovery shall be the same as that for
Container Number 1 in Method 5. Section 41
  4.2.2  Container Number 2 (Cyclune or
Large PM Catch). The cyclone must be
disassembled and the nouie removed in
order to recover the large PM catch.
Quantitatively recover ihc PM.from the
interior surfaces of the noiil* and the
cyclone, excluding the "turn around" cup jnU
the interior surfaces of the exit tube- The
rceuvery shall be ihe same as that for
Container Number Z in Method J, Section 4.:,
  4,2,3  Container Number 3 |PM,.).
Quantitatively recover ihe PM from all of the
surfaces from cyclone exit lo the front half of
the in-slack filler holder, including the "turn
around" cup and the interior of the exit lube.
The  recovery shall be the same as thai lor
Container Number 2 in Method 5, Section 4.:.
  4.2.4  Container Number * (Silica Gel],
Same as thai for Container Number 3 in
Method 3. Section 4.2.
  4.1.5  Impinger Water, Same as in Method
5. Section 42. under "Impinger Water,"
  4-3  Analysis. Same as un Method i.
Section 4.3. except handle ECR Container
Numbers 1 and 2 like Container Number l  in
Method 3, ECR Container Numbers 3, t. and 5
like  Container Number 3 in Method S, and
ECR Container Number 6 like Container
Number 3 in Method  S. Use Figure 11 ef this
method to record the weights of PM collected.
  4,4  Quality Contra! Procedures. Same as
in Method 3. Section 4.4.

i Calibration
  Maintain en accurate laboratory ing of all
calibrations.
  3-1  Probe No=le. Sarr.a as in Method i
Section 5.1.
  5.2  Pilot Tube. Same as in Method S,
Section 3.2.
  3,3  Meter and Flow Control Console.
  5.3 1  Dry Gas Meter. Same as in Method
5. Section 5,3-
  3,3J LFE Gauges. Calibrate the recycle.
total, and inlet  total LFE gauges with a
manometer. Read and record flow rales at 10.
SO, and 90 percent of full scale on the total
and recycle pressure gauges. Read and record
flow rales at 10. 20. and 30 percent of full
scale on the inlet total LFE pressure gauge.
Record the toial and recycle readings la the
nearest OJ nun (OBI in.). Record the inlet
total LFE readings lo the neareil 3 mm (0.1
in.). Make thne separata measurements at
each telling end calculate (he average. The
maximum difference between the average
pressure reading and the average manometer
-------
14252
Fudcval  Register I Vol. 5S. No.  74 f Tueidav.  April  17.  1990 / Rules  and Regulations
        hall not eacewd I nun IM3 in.). U the
d»flerwic» exceed we limit specified, adjust
or replace tbe precaure fausW- Afla* etiicfc
field use. check the calibration of the
preMure f eufe*.
  5-3-3  Total LFE. Same »t ihe metennj,
system in Method 5. Section 5.3.
  53.4  Recyck IFL Sane M the  melering
jyjiero in Method i. Section Si woe-Dl
completely dot* boih (he coarse aad fbf
recycle valve*,
  5.f Probe Heater. Conned she proiie -.c
the meier anJ (law control console wi-J» Lhe
umbilical connector. Insert • ihernocoupie
into the probe sample lint approximate:)}  balf
ihe length of ihe probe lample line. Calibrate
the probe heater at 68 "C (ISO T). in *C
(250 "F], and 177 "C I3SO "FJ. Turn on Iht
power, and let the probe heater to  ihe
i pec; Tied temperature. Allow me heater to
equilibrate, and record Ihe thermocouple
temperature and the mete.* and How control
console temperature 10 the nearest OJS "C
(1 '>"]- The two temperatures ihmild agree
within 5-5 "C (10 T). If this agreement ii not
me), adjust or replace the probe healer
controller.
  S.S Temperature Gauge*. Coonect all
thermocouples, and let the meter ana flow
cental coniole equilibrate 10 ambient
temperature- All thermocouple* ihall acree to
within i.t "C (2.0 T] with a nsnoard
nereury-in-glats thermometer, Replace
defective thermocouples.
  S.B Barometer. Calibrate agiinat a
standard tmrcury-m-glai* barometer.
  5,7 Probe. Cyclone and Nozzie
Combiiu lions. The probe cyclomend Mtzie)
combinations need not be calibrated if the
cyclone necta fb* design sncciBcatiotis in
Figure 12 of ihit method and the nosie meets
ihe design specifications in appendix S of the
Application Guide far the Source PM *
EjJiauii Cat Rgeyele Sampling System. EPA/
flOQ/J-as-OAa Thia document may be
obtained from Roy Humley at (919) 441-1060.
If the nozzle* do not meet ihe design
jpeaficaiiona. then lest the cyclone eud
no ale combination Tor conformity wrlh ihe
performance ipecificaliana (PS's) In Table 1
of thii method. The purpose of the  PS lasu Is
to detemme if ihe cyclona'i iharp~eu of oil
meet! minimum performance criteria. If the
evcione doei not meet deiipi ipeoficatieaa.
then, in addition to the cyclone and oosle
combination conforming 10 the PS'a, calibrate
the cyclone and determine ihe relationship
                              between flaw raic, c»i viaco«ity. ard gai
                              denti'.y. Use iht procedures in Scctmn 1.7 J of
                              ihn method.to eondw.i PS teiti and the
                              procedural in Secuon SJ of thii method to
                              ceJibraM the cycioiw. Conduct the PS lent In
                              i winj tunnel deicrtbed rn Secnon S.7.1 of
                              •-  - nwthod and u«m« a  pe,n>de gcnerarion
                                   m detcribed in Seciton 5.7.2 of thii
                                 .-.od. UH live partide litet and three
                                ,nd velocitiei ai liiled In Table 2 of thii
                              method. PeKorm a miniirwai of three replicate
                              meaiurementi of collection rffiriency for
                              each of the 13 cunditioni lined,  for a
                              minimum of 15 meaaurninetita.
                                S.7.1 Wind Tunnel. Perform calibration
                              and PS leiui in a wind tunnel (or equivalent
                              left apparatus) capable of eilabJiching and
                              maintaining the  required gai iirvaa
                              volocitiet within 10 percent.
                                SJ2 Partida Genera tion Syiteui- The
                              particle generation fvatein thai! be capable of
                              producing iclid  monodispenwd dye partlclfl*
                              with the maM rm>diin aerodynamic
                              diameten speciried in 1 able 2 ef ihii method.
                              The panicle tize dMtribution verificntion
                              ihauld be performed an  an integrated sample
                              obtained during the umpJ:ng period of each
                              leit. An acceptable aliematrve ia to verify Ihe
                              liu distribution of iamplea obtained before
                              and after each lea;, with  boih Mir.plee
                              required to meet Ihe  diameter and
                              monodiiaeniry  requirementi for an
                              acceptable test run.
                                SJJLl   Ettabliih the aizaof thcioliddye
                              particiei delivered to the tnt section of the
                              wind lunneJ uiiAg the operating pamrmen
                              of the pa,rucle generaUon ryitem. ami Tenfy
                              (he aite during the leita  by microscopic
                              examination of iairiples of she p*rridea
                              collected oa a membrene filler, Tha particle
                              site, aa eatabliahed by the operating
                              parametert of the generation tyiiean, tiaLl be)
                              wrJ-.m iha lolenaei  f peaCed in Table 2 of
                              thia method. The precwion of the perude ita
                              venntauon lecJsnjque ihall be) ai lean rOJ
                              fiat, and the) pa/ticlt  aiza determiaed by the
                              venficanon ucfaoique ihall not differ by more
                              than to percent  from thai eiuMUhed by the
                              operating paiamMen of ihe particle '
                              generation lyitea.
                                1.7i2   Certify the Bwaodiipenily of the
                              particle* (or each let! either by microscopic
                              inspection of collected pauticiea on filian or
                              by other luilable aoniioriag technique* such
                              ea an optical pautick counter followed by a
                              nuiiichaimei pulaa height aoaiyiv. tl the
                              proportion of multiple!* and aatcUites in a-
ncrosol e«ee*dl tO pereetil by masi, the
particle jenerewow IJPSNMI n unacevriiitbl*
for purpote* of thia tnt Mallipi««9 gre
panic!*! ihet ere atgilomeTiied. and » range-
  S.7.3  Schematic Dniwingi. Sdicmitie
drawing! of the wind lunnel and blower
jVBiern end other information ihowinj
complete procedural detaili ef the test
itmotphere generalinn. verificatron. and
delivery teehr.HHieii ihall be furnished with
calibration data to tne reviewing nfiency.
  S.7.4  Flaw Rate Measuriment. Determine
the cyclone flow ratet  wilb a dry gaa meter
and a stopwatch, or a calibrated orifice
•ysiem capable of measaring flow rates in
within 2 percent.
  J.7 s  Performance Specification
Procedure. Establish the test panicle
pencrator  operation and verify the panicle
lize microicopicully. If mondisparsily is robe
verified by nteeturemerm at the beginning
and the end of the run ruher thin by an
integruted iumplc. these measurements may
be made at this time.
  5.7.3.1   The cyclone cut me (DM) is
defined ai the aerodynamic diameter of a
panicle having a SO percent probability of
penetration. Dei ermine ihe required cyclone
flaw rule nl which Dv> is 10 |tm. A suggested
procedure ia to vary ihe cyclone flow rate
while keeping  a constant particle site of 10
fim. Measure the PM collected in the cyclone
|nU eiil tube (m,), and filler (mr). Compute
the cyclone efficiency (E.) aa fallows:
                    m.
              (m, + m, + m,J
                                    X ICO
  5.7 52Perform ikrree nrpiiatei and
calcuiaic) the arverage cycioae eJQaenr,1 *t
follow.
 where Ea. E«. and Ei ar« replicaie
 Qeasummenta of E^
   5.7.3.3 Dilculala ite itaadard deviation (4f  Cskalstc  ma overall efTicienei' (E,)
 as follows;
-------
             Federal Register /  Vol.  55.  No. ?4  /  Tuesday. April  17.  1990 /  Rules and Regulations       14249
them to be erroneously measured as
PM,..
  Drying and shrinking is not thought to
be a problem. Should it be considered a
problem, the letter could choose Method
201A in which there i» no recycle gas.
  Another commenter laid that the use
of recycle gas increases velocity in the
cyclone which could cause friable
particlei to break yp. becoming PM|0.
  Prior to size classification  by a PM,a
cyclone, there is no known or suspected
mechanism by which friable panicles,
should they exist, may break up. When
particles greater than 10 jim
aerodynamic size reach the cyclone wall
due to  their inertia, (hey are  collected.
  One  commenter said that no
consideration is made in either method
of the gai density, gai viscosity, or of
the denaity of the participate matter
being measured.
  Gas density and viscosity  are
compensated for in the calculations for
both PMio methods. Because the
aerodynamic diameter of PMu
emissions is used in both PMio methods,
determination of particle densities,
volumes, or shapes is not necessary and
would be redundant.
  Another commenter said if the PM,«
measurement is 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 affected.
  The effect of an ESP on par tide sizing
when using Method 201 or 201A is
considered to be negligible.
  There was concern by the  commenters
that the particuiate matter may settle
out inside the sample train.
  The trains have been calibrated with
test aerosols and the relative accuracies
to each other have been established,,
These tests results and Lhe operation
principles of both methods have shown
that "settling" is not 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 all the information
considered by EPA In the development
of this rulemaking. The docket ii a
dynamic file since malarial is added
throughout the rulemaking development.
The docketing system is intended to
allow members of the public and
industries involved to 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 and
promulgated test method revisions and
EPA responses to significant comments,
the contents of the docket, except for
interagency review materials, will serve
as the record in case of judicial review
(section 307{d)[7J(A)J.
  Under Executive Order 12291. EPA is
required to judge whether a regulation is
a "major rule" and. therefore, subject to
the requirements of a regulatory impact
analysis. The Agency bas determined
(hat this regulation would result in none
of the advene economic effects set forth
in section \ of the Order aa grounds for
finding a regulation to be a "major rale."
The Agency has, therefore, concluded
that this regulation is not a "major rule"
under Executive Order 12291.
  The Regulatory Flexibility Act (RFAJ
of 1960 requires the identification of
potentially advene impacts of Federal
regulations upon email business entities.
The Act specifically requires the
completion of • RFA analysis in those
instances where small business impacts
are possible. Oecauie this rulemaking
imposes no adverse economic impacts.
an analysis has not been conducted.

Lial of Subject* in 40 CFR Part 51

  Administrative practice  and
procedure, Air pollution control. Carbon
monoxide. Intergovernmental relations,
Lead, Nitrogen dioxide. Ozone,
Particuiate matter. Reporting and
recordkeeping requirements. Sulfur
oxides. Volatile organic compounds.
  Dated; March 22. 1B90-
William K. RtUIy,
  The EPA amends title 40, chapter L
part 51 of the Code of Federal
Regulations as follows:

PART 51— [AMENDED]

  l. The authority citation for part 51 ii
revised to read ai follows;
  Authority: 12 U.5.C 74O1fb)(1). 7410, 7470-
7479. 7SQ1-7U8. and TtOl(a), unlwi
otherwise noted.

  2. Subpart K. 1 91-212 Ii amended by
adding paragraph [c] to read as follow*:

f 3 1.211  Testing, Impacted, enforcement.
and complaints.
  (c) Enforceable test methods for each
emission limit specified in lha plan. Aj
an enforceable method. Slates may use:
  (1) Any of Uii appropriate methods In
appendix M to this part Recommended
Test Methods for Stale 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 GO.
  3. Appendix M is added to part 31 io
read as follows:
Appendix M—Recommended Test
Meihodi for State Implementation Flans

  Method an—Determmaiion of PM,,
Emuiioni (Exhausi C«i Recycle Procedure).
  Method HttA—Determination of PM,»
Emission! (Constant Sampling Rale
Procedure).
  Presented herein art recommended test
methods for meaiuring air polluisnii
emanating from an emission source. They are
provided for Slates Io uie in their plan io
meel the requirements of Subpart K—Source
Surveillance.
  The Siala may also  chooee lo adopt other
methods to meet the requirememi of Subpari
1C of ihil part, subject  to iho normal plan
review process.
  The Slate may also  meet the requirements
of Subpan K of this part by adopting, again
subject lo Ihe normal  plan review process.
any of lh« relevant methods in appendix A to
40 CFR pan 80.

Melhod Ml—Oetormuniion of PM,,
Emiuioiu

(Exhaust Caj Recycle Procedure)

2.  Applicability and Principla
  1.1  Applicability. This method applies lo
the in.ilHck measurement of paniculate
mailer (PM) emissions equal lo or lesi than
an aerodynamic diameter of nominally 10 p.m
(PM..I from stationary tourcei. The EPA
recognizes thai condensible emissions not
collected by an in-Hack method are also
PMn, and thai emiesions that conlnbule lo
ambient PM,. levels are the sum of
condaniible emiasions and emissions
measured by  an in-slack PMi* method, such
&> ihis m*ihod or Method ZfflA. Thetefon>,
for establishing source contribution! to
ambient levels of PM,*. luch as for emission
inventory purposes, EPA suggest* that source
PMu measurement include both in-slack PMio
and condensible emission!. Condensible
minions nay be measured by an impinger
analysis in combination with ihis method.
  1-2  Principle. A gai sample if
iiokijietleally extracted from the lource. An
in-Hick cyclone ii used lo separate PM
greater than PM.* and in in-slack glass fiber
filler ii used lo collect the PMi* To maintain
iiokjnatic flow rale conditions a! the tip of
the probe and • constant flow rate through
ihe cyclone, a clean, dried portion of the
sample fas ai Hack lempefaiure is recycled
into the noxila. The paitieulaie misi ii
determined gravineuicaUy after removal of
uncotnbined water.

2.  AppcratuM
  Note Method S as cited in ihn method
refers la the method in 40 CFR part SO.
appendix A.
  2.1   Sampling Train. A schema tie of the
exhaust of Ihe amhault gsa recycle |ECR|
train ii ihown in Figure l of thii method.
  2.1.1  Norile with  Recycle Attachment.
Siamleit itnl (311 or equival«nii with a
sharp tapered leading edge, and recycle
attachment welded directly on the aide of ihe
nozzle (•*• icheinaiic in Figure 2 of this
method). The angle of the taper ahsll be on
the outside. DM only  iirtight sampling
nonlet. "Gooseneck" or other noBle
-------
 14250       Fedtvmi Renter /  Vol. 55. No.  74 I  Tuesday.  Apnj  17.  1990  / Rule*- ami  RegoJatk>n«
 cutension* deugrwd '<> 'em ih«
 flow 80- . u u htaliwd S uc not acsepwbie.
 Locate a thermocouple in the recycle
 attachment to im»a«r* >h* temperemi* of *«
 recycle IBI 11 .rKwn in Figure 3 of Ihw
 method. The wcycle iiikc-hmeni »K«8 be
 made of ititnle" *l«l and th^ll be
 connected to lne Prob* and noizle wrth
 naiolMi i1**1 fniifigi. Two noole »ixe«, a g .
 0,123 and 0-18D in,, ibnuU be available to
 ,How itokineiic snmpLTij to be conducted
 over • rang* of flow raie*. Calibrate each
 noiile aa deicrib*d in Method 5. Sccron S.I.
   2.1.2  PM.o Siier. Cycicne, meeting the
 specification* m Secaon U of ihu method.
   2-1.3  Filter Haider. 63mm. auintaa »te*L
 An Andersen filler, pun number SE274. has
 b«en found to be acceptable (or the in-aUck
 Tiller.
 NUM.- Mention of trade namea or unecific
 product* don nai con»i>tute endorsement by
 Lhe Environmental Protection Agency.
  11.4  Pilot Tube. Samp as i:i Method S,
 Section  2,1.3. Attach iht pilot to (he pilot
 tinea with iiajrJeaa tteel  fv.insi and :o the:
 cyclone in a configuration umiiar  to that
 thown in Figure 3 of this  method. The pitoi
 lines ihall be  made of heel rctiaianf material
 and attached  to the probs with nainlcM HeeJ
 filling*.
  2.1.5  ECRProtw. Steinksi necL
 1.5.9-mm (S-in.) ID tubing with a probe
 liner, itainleji ste-el 9.5J-mffl (%-in.) ID
 gtainlea* steel recycle  tubing, two 6.35-0110
 (•/•-in.) ID iteinless Meet tubing fcr the pilot
 tuba exienaioiu. three thermocouple, lead A.
 and one power lead, ill contained by
 atainlna iteel tubing with a diameter of
 approximately 51 nun (2.0 in.]. Design
 consideration* should include minimum
 weight construction materials Tufficieni for
 probe atnicural strength. Wrap ihe lamp I e
 and recycle tatm with • hearing tape to heat
 the sample and recycle gasea to itack
 temperature,
  2.1.8  Condenser. Sane n in Method 1
 Seel-on  2.1.7.
  Z.I. 7  Umbilic*] Connector. Flexible tubing
 with thermocouple and power leads of
 lufHcient length to connect probe 10 meter
jnd flow control console.
  2-1.8  Vacuum Pump. Leak-right oil-ten.
nanconiaiBinaring, with an abioiala filter.
"HEP AT typt, at the pump exit. A Gael Model
0522-V1G3 C180X p\imp ha a been  fonnd to b>
   .1-9  Meier and Flaw Control Console.
Syit«m constating of • dry gam me4er and
calibrated onfice for amnnmng Mmple flaw
rate and capable ef muauring vohima to ±2
percent, calibrated laminar Qom «!*rrMnu
1LFE"§) or equivalent for maaaorini toul end
•ample Row rniea, probe heater controL and
nti flow. Flow
meftsuremgnu include veloaty hud (ipl.
on Hoe dirferantial prMaure (AH|. total flew,
recycle How, «nd total back-preMur* through
the iyatera.
  2.1.10 BarooBler. S*aw ai in Method S.
Section n.g.
  z.i.11  Rubb«r Tubing. &js-mj»jsiHn4
ID flexible nibljcr rubina,
   i2  Sample Recovery.
   2.2.1  NoaJ«. Cyclone, and niter Hold*r
 DniahH. Nykwi briaile fartuhei properly uaed
 and ihaptd for cleaning the nozzle, cyclone.
 Filler holder, and prate or prolM liner, with
 nainlett reel w*r« ihaf:j and handles.
   2.2.1  vv'aah Boplea. Clan Sample Storage
 Containnr*. Petri DIWIM, Graduated Cylinder
 and Balojioe, PlaiUc Storage Container*, and
 Funnel*. S*me >a Method 4. Secbooi LZJ
 thraagh HA «nd iiB. reta«cliv«ry.
   2.3  Analylia. Sume ui in Method 5,
 Section 13.
 3.  fteagena
   The reogerra otrt in MmpKog.
 recovery, end analyaii an rtw
 specified in Method 5. Sacuon* 3 13— and
 3.3, reipectivoijr.
 <-  Procedure
   4.1  Sampling. The complexity of ihit
 method i»»och !h«L In orter TO obtain
 relialite results, tnten ahould be trained and
 experienced with tiw tm proudurM.
   4.1.1  PTBW« Preparation.Sam* as in
 Method 3. Section 4.1.1.
   4.1.Z  Preliminary Datemunationi. Same at
 Method 5. Section «.!_! eMept uae the
 dircctioni oa noaJe me lelection in  thia
 aeclion. Uw of the ECU method may require
 a minimum sampling pon di*mei«r of 02 m (0
 in.). Alao, the required majumnm number of
 aarr.ple travene PJIQU «; ^.y locatiuti ahatl
 be 11
   4.1.3-1  The cydone and filter holder matt
 be in-iuck or it ttack iemp«ntura duriog
 lamplir-g. The blockage effaeia of the ECR
 lampiing auembly will b« minimal If [he
 croai-seciionoi a.Ta of the jump I ing
 aiMtnbly ia 3 percent or leu of ihe craia-
 aeclional «rt* of the duel »nd a pitoi
 coefTicieni of Q.04 may be aaaignad to lh«
 pitot IT '.he croM-aactioaal avew of iKe
 aajembly a greater than 3 percent of the
 creai-iectional area of tha duel, then either
 determina the pilot coafCaent at lampliog
 condition! or UM a alandard pilot with*
 known cocRlcitm in a configuration with the
 ECR aampling auamlity aucfa that flow
 disturbance! art) rainiiBixnd.
   41.2.2  CoMtrucl • aalup ef preisure dropa
 for varioua ip I and tempataturea. A
 computer it uaeful lor ih«aa ulculaiiona. An
•kampla af tha outpni ef the ECR aetup
 pragran ii abown in Tigure 6 of Ihia method.
 and directions on it* uaa an in atct:on 4.1 J^
of thia mvihod. Compuwr piu^iunij. wnttcn
in IDM BASIC computer lanoiiag*. 10 do the*«
 typea of aatup and reduction calculation! for
 (he ECR pracedui*. are *v«ilabJ« through the
National Technical Information Strvicaw
 INTIS). AcotMioo numbw PBeO-SOOOOi S285
Pon Roy*! Rotd. Spraiffi01d. Vltgtai* 22161.
  4.1 JJ  The ECR a*lup progno allow* the
 leitar to aolect the noala liu btatd on
anticipated avertge stack condllioni and
pnnu a letup theet for Hold u»«. The anaount
of recycle through lha noizie ahould ba
between 10 and 80 percent, lapuu for the
ECR Mtup profpram an Hack tenparatura
(minimum, eiaxiraunv and a,vtBrtae>). alack
 velocity (miutmim. maJumum. and average).
atmaepheric pr«*aure. «Uck viatic preuure,
metar box  tefnptrarurt itack moiinm.
peroerU tk, and pcreea! CD, to tha alack gaa,
pilot coePVjenl iz«.
  41.2.5  The prcsaure upalreamof the LFTs
11 anumed to be cnnitnnt at 08 in, H; in the
ECR letup calculations.
  4.1.2.0  The setup ihcet ronsmieted using
thii pracedgre shall be similar in Figure 0 of
thu meihod. Inputa  needed for the calculation
ant the same aa for  the icwp computer
except thai luck velocities ere not needed
  4.U  PreparaUon of Coliection Train.
S^rae ai in Method  S. Section 4.1J. except
UM tha fallowing diraciiaru 10 set up ibe
train.
  4.1.3.1  Astemble the ECR wnpUng
device, and atuch >l to p.-ob* a* shown in
Figure ] of thia method. If Jiaci  le-T-peraturei
exceed 300 'C (500 'D, then useroblc the
ECR cyclone without the O-nng and reduce
the vacuum requirement to 130 mm Hg (S.Q in.
Hg) in ihe leak-check procedure ia Section
4.1.O.2 of ihU method.
  4.1.3.2  Conned the proble directly to the
Hlier bolder and condenaer aa in Meihod S.
Connect the condenser and prabe to the
meter and Qow control console with the
umbilical connector. Plu- in ibe pump and
attach pump linea u Ihe meter and flow
control console.
  4-1.4  Utak-Chtck Procedure. The leak-
check for the ECR Method consi»ii ol two
pana: the umple-flida «nd the recycle-tide.
The simple-aide leak-check ia required at  the
beginning of lha run wiUi the cyclone
attached, and after the run with  tha cyclone
removed. The cyclone li removed before the
poit-tMt leak
-------
Moisture Determination
      Volume or weight of liquid in Impingers
      Weight of moisture in  silica gel 	\
                                    ml or g
                                    9
Sample Preparation (Container Ho. 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 TUration of Sulfate

       Normality  of NH4OH
       Volume  of sample titrated
       Volume  of titrant
                                    ml
                                    ml
                                    N
                                    ml
                                    ml
Sample Analysis
       Container
       number
                            Weight of Condensible Participate, mg
Final  Weight     Tare Weight
Weight Gain
       4 (Inorganic)
       445 (Organic)
                                     Total
                                Less  Blank
         Weight  of Condensible Particulate
                       Figure 3.  Analytical data sheet.
-------
OiUlc*
                                                     n
   Us* Mion
MiffiM/uu liuottjli iyiium
PllS/litfJ
tkjli SyllMl




FknMRila
bicai* f
* lloUmal
	 If 	 .
	 II 	




                                 201pm
                      Ttiwrnocaiiplat
                                    Melai Ooi
                                          Tlppad In^tlngait
            Wlten Piitaig
     NOtogan lluoitgh System
                             2,   Scltoouii it:  of  post-teg I  itl I i'(i(:cii  purge  system.
-------
EMTIC CTM-005           EMTIC CONDITIONAL TEST METHOD                   page 8


fl.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 redvssolved 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 Nj 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.D., S.C.  Steinsberger, G.M. Pluramer, L.T. Lay,  G.O. 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/AUMA  International Symposium  on
Measurement  of Toxic and Related  Air Pollutants.  May 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  for Determination 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  So.und 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,  I960.

 7.  Wisconsin Department of Natural  Resources.  Air Management Operations
           Revision 3.   January 11, 198B.
-------
EMTIC CTM-005           EMT1C CONDITIONAL TEST METHOD                   Page 7
7.3  Mass of Inorganic CPM.

                                 V
                       mr
                                  1C
me                     Eq.  2
7.4  Concentration of CPM.
                                  ffl.                                    c   i
                                               •                        Eq. 3
8.  ALTERNATIVE PROCEDURES

8.1  Determination of NH4" Retained in Sample by Titration.

8.1.1  An alternative procedure  to  determine  the amount of NH4" 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 NH4OH to a pH of
7.0, as  indicated by a  pH meter.   The O.I N NH4OH is made as follows:  Add
7  ml of  concentrated (14.8  M)  NHjOH  to  1 liter of water.  Standardize against
standardized  0.1 N H:SOa 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  NH.OH that has been
standardized  against a  National  Institute of  Standards  and Technology
reference material .

8.1.2   Calculate  the concentration of S04" 1n the sample using the following
equation.

                               -48.03 Vt N

                        c< —     -
 where:

           N - Normality of the NH4OH, mg/ml ,

          Vt . Volume of NH4OH tUrant,  ml.

       48.03 • mg/meq.

          100 - Volume of solution, ml.

 8.1.3  Calculate the CPM as described  In Section 7.
                                                            ; I


                                                            V
-------
EMTIC CTM-005           EKTIC CONDITIONAL TEST METHOD                   page g

5.3.4  Analysis of Acetone  Blank  (Container No. 8).  Same as  in Method 5,
Section 4.3.

6.  CALIBRATION
Same as in Method 5,  Section  S, except  calibrate the 1C  according  to  the
procedures in Method  SF,  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.
      c   • Concentration of  the  CPM  in the stack gas, dry basis,  corrected to
            standard  conditions,  g/dscm (g/dscf).
      CSQ4 • Concentration of  SO/  in the sample, mg/il.
       m^ • Sum of the mass of  the  water  and MeCl2 blanks, mg.
       mc • Mass of the NH/ added to sample to fora ammonium sulfati, mg.
       m, • Mass of inorganic CPM matter, rag.
       mg » Mass of organic CPM,  mg.
       mr • Mass of dried sample  from Inorganic fraction, mg.
       mre • 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.
       Vic - Volume of itnplnger contents sample, ml.
 7.2  Correction for  NH4"  ind  H20.  Calculate tht 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 S0t".
                      «e-KCswVle                                       Eq.  1
 where:
     K - 0.020502
-------
EMTIC CTM-005           EMTIC CONDITIONAL TEST METHOD                   Page 5


(Note:  Do not use this aliquot to determine chlorides since the HC1 will be
evaporated during the first drying step; Section 3.2 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/MeCl2 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 MeClj.  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  3.50-™!'
weighing tin.

5.3.2.2  Organic  Fraction Height  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
(14.3 M) NH,QH until the sample turns  pink.  Any excess  NH;OH will  be
evaporated  during the  drying  step.   Evaporate  the sample to  dryness in a  lOE'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  SQ2 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 Aranonlun Ion (NH4*) Retained
in  the  Sample.  (Note: If NH4OH  is not added, omit this  step.)   Determine  the
amount  of sulfate in 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 NH/
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 Watar and HeC1z  Blanks (Container Nos. 9  and 7). Analyze
 these sample blanks as described above in Sections  5.3.2.3 and
 5.3.2.2, respectively.  The sum of the values for the water blank and  the
 MeCl2 blank must  be less than  2 mg  or 5 percent of the mass  of  the CPU
 (n, + nr),  whichever  Is greater.  If  the  sun of the  actual blank values  Is
 greater, then subtract 2 mg or 5 percent of the mass of  the CPM, whichever is
 greater.
-------
EHTIC CTM-Q05           IMTIC CONDITIONAL TEST METHOD           "       Page 4


Is operating at greater than ambient pressure and prevents that possibility of
passing ambitnt air (rather than N2) through the impingers.   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.

5.2.2  Sample Handling.

5.2.2.1  Container Nos. U_2_. and 3.  If filter catch 1s to be determined, as
detailed in Method 5,  Section 4.2.

5.2.2.2  Container jJQj__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 O.S 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  (MeClz Rinse).  Follow the water rinses of each
impinger ana  the connecting glassware,  including the probe extension with  two
rinses  of MeCl2; save  the  rinse products in a clean, glass sample jar.  Hark
the  liquid  level on  the jar.

5.2.2.4 Container No.^  (Water Blank). Onca during each  field test, placa
500  ml  of water in  a separate sample  container.

5.2.2.5 Container  Ho. 1  (WeC12 Blank).  Once during each field  test, place  in
a separate  glass  sample  jar a volume  of MeClj approximately equivalent to  the
volume used to  conduct the MeCl2 rinse  of the impingers.

5.2.2.6 Container  No. 8  (Actions  Hank).   As-described  in Method  5,
 Section 4.2.

 5.3   Analysis.   Record the data required on a sheet such  as  the one  shown in
 Figure 3.   Handle each simple container as  follows:

 5.3.1  Container Nos. 1.  2. and 3.   If filter catch Is analyzed, as  detailed
 in Method  I, Section  4.3.

 5.3.2  Container Hos. 4 and 5.  Note the Itvtl  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
 voluffletrically to +1  ffll or graviraetrlcally to iO.S g.   Remove a 5-ml aliquot
 and set aside for later  ion chromatographic (1C) analysis of sulfates.
-------
EMTIC CTN-005           EHTIC CQNDITIOKAL TEST HETHOD                   Page 3


4.2.1  Hz fias.   Nj  gas  at  delivery  pressures high  enough  to  provide  a  flow of
2Q liters/min f°r  1 hour through the sampling train.

4,2.2  Methylene 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  Methylene Chloride.

4.3.2  Ammonium Hydroxide.  Concentrated  (H-9 M) NH4OH.

4.3.3  Water.  Same as in Section 4.1.
                                                     .Oi'           i>^
4.3.4  Phenolphthalein.   The  pH  indicator solution, Irfl  percent  in^SO percant
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  H, 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 1s 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 avoid over- or
 under-pressurizing the Ifflpinger array, slowly commence the N2  gas flow through
 the line while simultaneously opening the mater  box pump valve(s).   Adjust the
 pump bypass and N2 delivery  rates  to obtain the  following conditions:
  (1)  20 Uters/rain or &H9 and (2) an overflow rate through the  rotameter  of
 less than 2 liters/rain.  Condition (2) guarantees that the Nz  delivery system
-------
EMTIC CTM-QQ5           EKTIC CONDITIONAL TEST METHOD	Page 2

3.1.2  A Teflon filter 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, MeCl,.  It is important to  remove completely all silicone grease from
areas that will be exposed to the MeClz 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  imoinger train from  a standard gas
cylinder  (see  Figure  2).   Standard  0.95 cm  (3/8-in.ch)  plastic tubing  and
compression  fittings  in  conjunction with  an  adjustable pressure  regulator and
needle valve may  be  used.
3.2.2  Rotameter.  Capable of  measuring  gas  flow  at  20 liters/min.
3.3  Analysis.   The  following  equipment  is  necessary  in  addition to  that
listed  in  Method  5,  Section 2.3:
3.3.1   Separatory Funnel.   Glass, 1-liter.
 3.3.2   Weighing Tins.   350-ml.
 3.3.3   Drying  Equipment.  Hot plate and oven with temperature  contro,.
 3.3.4—Burmi.—t*ml  aiio with O.Q1 m\  graduations.
 3.3.5  Pipets.  5-ml.
 3.3.6  Ion Chromatograpn.  Same as  in Method 5F,  Section 2.1.6.

 4.  REAGENTS
 Unless otherwise indicated, all  reagents must conform to the specifications
 established by the Committee on  Analytical  Reagents of  the American Chemical
 Society.  Where 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 1193-74,  Type  II.
 4.2 Sample Recovery.   Sane as  in  Method 5, Section 3.2, with the following
 additions:
-------
II
u

EC
-------
               EMISSION  MEASUREMENT  TECHNICAL  INFORMATION  CENTER
                            CONDITIONAL TEST METHOD
                    Detirmination Of Condensiblt Emissions
                            From Stationary Sources


1.  APPLICABILITY AND PRINCIPLE

1.1  Applicability.  This method applies to the determination of eondensible
participate 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 Hethod 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 Hethod  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 (SQ?) gases from the impinger  contents.  The impinger solution is then
extracted with methylene  chloride (MeCl2).  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
waste  burner  and two coal-fired boilers  are 13.0 ± 2.1  mg/m3, 3.5 ± 1.1 mg/nr,
and  39.S  +  9.0 mg/m1, respectively.

2.2   Interference.  Ammonia (e.g.,  in  sources  that use  ammonia  injection  as  a
control  technique)  interferes  by reacting  with  tht hydrogen  chloride  (HC1)  in
the  gas  stream  to  form  ammonium chloride (NH4C1) which would  be measured  as
CPM.   The sample may be analyzed for chloride  and  the  equivalent  amount  of
NH4C1  can be  subtracted from the CPM weight.


3.   APPARATUS

 3.1  Sampling Triln,   Same as  In Method 17, Section  2.1,  with the following
 exceptions noted below (see Figure  1).  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        EHTIC  CTH-Q05
 Technical Support  Division, QAQPS,  EPA                         March  21, 1990
-------
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              » < 9 m/i
                            4     6    fl  10



                        AERODYNAMIC DIAMETER
                                                  20
                                                               40
       FLgv*r«  3.   ECCLciency cru-elop« for  tho PH., cyclone.
    ssj—



    90



    BO
«   70
u.

u   SO
u
e
       40


       30


       20




       10



        5
            17 < » < 17 */•
             9 < * < 17 m/t
                 < 9 m/i
                           J	L
      0.1
                             0>    0.6  OJ  t
                                                              IIII41
             9.   Efficiency envelope for  firsc calibration stage,
        Figure


   (KR Doc. 9O-rao3 Filod 4-10-flO: MS am

        COM «M«-«-C
-------
14278      Federal  Reaisler / Vol. 55.  No. 74  /  Tuesday.  April  27. 1990 / Rules and Resulations
 TABLE 2.— PARTICLE SIZES AND NOMINAL
    GAS VELOCITIES FOB EFFICIENCY
   """''    r 1=10
10iO.S..
14 i 1 0..
20= 1.0..
" Muai median acrodv'miniiL d;nnn'li:

      CODE i
-------
                       Remitter /  VoL 5S.  N'u.  "4 /  Tuesday,  April 17.  1990  /  Rules and Regulation!       14277
                    in... - i.
                                  \ to"'
                                            It, + 4HOJ Cf~

C n
v d';
» f.
»„. fi


...
Norzia NO. i
!



in HjQ ,.,,».,...,
\r\ H,0 ' '•»• »

i i

] <
t
1 ,..,„ 	 	

;

Vcliir.i'v lriivef*r diila:
    l run lime, mmuiei =
Number of irni-crie point* •»
          in'   i      (Tntul run linin)
                  H	___^^^^
                                                     Ml At <  £p(Mi-lho<1 2)
                                                                              C.'
                                                           ,
                             I, a dwell lime nl fir?) imvune puinl.
                              minutes.
                             ip i «lhr vciocily ncud n( liit [irsl iruvcni:
                              poini (Irani a prcvioui (rovericj, in. tto
                             ip'^. = lliL> HJJJJ-E D/ the nvcraur iquurc
                              rue I of the ip'l (from a prcvimis vcl
                              irnvcrsf-). in, 11:0.
Al iulinKu.u«nl iruvcne points, mciisurp ihu
    veiacily Ap und calculute the dwell-timc
    liy uiinp Ihu ((jllnwinf! i
                I,-
                                              (in. is. n=ZJ.' " ' loml number of mimplinn pulnli
 i here;
                             4[i.-rtiiiujurtd vflnclty hcud Hi point n. In.      ^pp -dwell time ut fim Iruvurse puinl
i L-;u-i:rjie point n. niinutw,        H-.-Q,                                        minulus.
                                                                        Fipurv 6. Fjtnmplb worksheet 3. dm:;l linn:
   Pom:
           a !
  Plani	
  Dale	
  Run no. _
  Filler no.
  Amount uf liquid lost during
I run sport	
  Acitorie blank volume, ml -
  Acciqne wash volune. ml (4),
(5).
  Acclone blank cone, mg/mg (Equation 9-4,
Meihod 51	
  Aceionc wa>h blank, mg (Equnlinn S-S.
Method 5)	
                             ConUinwNO
                           I.__
                           J	
                                             Find
                                                     TUT
                                             Figure 7, Method 2T1A analyil* »heel.
TABLE   1.—PERFORMANCE   SPECIFIC*
  TIONS FOR  SOURCE PM,U CYCXONES
  AND NOZZLE COMBINATIONS
                                                                                        Una
                                                                                     Pgrnn	' Sucti tnai
                                                                                                  cotlKUon
                                                                                                         '«'»
                                                                                                  vi Iran
                                                                                                        S.2.B
                                                                                                          S.
-------
14276        Federal Reciater /  Vol. 55. No. 74  / Tuesday. April  17,  1990 / Rules and  Reflations
  Buromciri!" possum.

  Slock sidiic prcisurc.
P,. in. |[.Q«	
               icmperalur*.
  Metur lemoeraiurt, lm. Tm
  Orifice 1H». in. II-;O=
Gas nrmlysii:
        "
                                                     moisture c
                                           Molecular »eishl of Black gui. dry basin:
                                                            _ lb/iymoic
                                           Molecular weight of Hack gas. wet biisii:
                                             M. .M.11-B..I- 1S(B..]= _ l
                                               lb mole
                                                   nvck pressure:
                                                                                                   13.6
                                                                                                                      in, 11-;
Viicosr.y ufiluck gas:
  M, = 152,418-0.^52 I, J. 3.2355 < 10'»
    I.- + Q.5314? (".'-O-1-74.143 D,.=
    ^^_^_^_ micropoisc
Cyclone CJVK r;i!«:
                                     Q.-O.C02E37 p.
                                                       M. P.
                                                                                   d'/ram
  Figure (. ELium^lc workbheti I. nyriune
flow raie and iH.
                                           Orifice prc«jur« head (4H) needed for
                                              cycJone flow rale;
                                        Q, (l-B.,) P. t    i.
                               ill-  |  	t •-
                                          I,+ 400
                                                              ) 08a iH»
                                                                                      . in. H:O
         iH for three i
                                            Slack vmcuiiiy. ^
                                           micro pour
1.-P 1 i i
ax M.







                                             Abtolui* flack pressure.
                                           F. ta. Hi -  	
                                             Av«rag« jtick lemperacura.
  Cjelonc flow faie. fi'/mtn.
Q.	
  Method 2 pitoi cocfficienl.
C.'-	
  Molecular weight of slack gas. w«i bc.su.
M.-	
  Nozzle diarncior. D., in.  =	
Norzie vdoeiiv:
                                                     J.OSfiQ.
     mum *nd minimum velucilira:
                                        (LM37 4-
                                                                           ,,].
                                                                                              [i/sec
                                        0.+U7
                                                   (U890 -
                                                             02603 Q.*n.
                                                                           ,    1-
                                                                             *   ~
                                                                           1    J
                                                                                             .ft/I
  Figur* S. Example workih«ei 2. nozzle
sclcciioo.
                                           Mjuumuin nflxl ^•••»»»« velocity bcui
                                               value t:
                                    p*,. " 1-30.% X 10"
                                                            >.  ,
                                                            (I. f
-------
             Federal Regisler / Vol. 55. No. 74 / Tuesday. April ir. 1990 / Rules and Regulations
                                                                                      14275
                                 Cyclone Interior  Dimensions
                          Din
                          t
                0,10  in.  :	
                                       ,J
u
                                           •Ocup-
                                                         H
                                                         •Hcup,
                                                        J.


cm
inches
Dimensions (±0.02 cm, ±0.01 in.)
Din
1.27
Q.5QL
D
4.47
1.76
Or
l.SQ
0.59
§
US
0.7*
H
OS
174
h
124
0.83
Z
4.71
US
s
1.57
0.52
Hca?
125
0.89
Ocup
4.45
1.75-
a;
1.02
0.40
00
1.24
0.49
                   Figure 3.   Cyclone design speciffcatians.
BIUJNQ
-------
14274
Federal Re?frler / Vol. Si No. 74 / Tuesday. April 17.1990 / Rules ind Regulations
                   •;- -' — '' '-LjfJ,1/
Nozzl-
(inches)

 r.136
 0.150
 0.164
 0.130
 0.1S7
 0.2TS
Q.2S4
0.300
0.342
  Con*
  Angle, 9
   (degrees)

      4
      4
      5
      6
      6
      6
      6
      5
      i.
      4
      3
Outside
tapec, *
(degrees)

   15
   15
   15
   15
   15
   15
   15
   15
   15
   IS
   15
                                         Straight  inLe'
                                           Length,  I
                                           Ur.ches)
                                            <0
                                            <0.
                                            
-------
                                              IMPINGER TRAIN
                                                                 THERMOMETER
PM 10
SAMPLER
   vc*
FILTER HOLDER

     HEATED PROBE
NOZZLI
    X
 "S-TYPE
 PfTOTTUBE
                                  DISTILLED WATER    EMPTY  SILICA GEL
                                      INCLINED
                                     MANOMETER
                                FLOW  CONTROL  SYSTEM   COARSE
                                                        FINE
                                            CALIBRATED
                                      GAS   ^ ORIFICE
                                      EXIT
                                                                   VACUUM

                                                                    PUMP
                                             INCLINED
                                            MANOMETER
                                            DRY GAS
                                            METER
                Figure 1.  CSR Sampling Train
                                      76A
-------
Moisture Determination
      Volume or weight of liquid in  1mpingers_
      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  NH,OH required? ^_____
      Sample  extracted  2X with  75 ml MeCl2?

For Tltration of Sulfate

      Normality of NH.QH
       Volume  of sample  titrated
       Volume  of titrant 	
                                    ml
                                    ml
                                    N
                                    ml
                                    ml
Sample Analysis
       Container
       number
                            Weight of Condensible Participate, mg
Final  Weight    Tare  Weight    Weight Gain
       4 (Inorganic)
       415 (Organic)
                                    Total
                                Less Blank
        Weight  of  Condensible  Particulate
                       Figure 3.  Analytical  data sheet.
-------
APPENDIX J.3




ALDEHYDES
-------
Foraaldehyde, acncone, and 2 .^-dinisroanlUn*  contaalnation  Of  :ni  aquaous
acidic 2.--dinL:rephenyL-hydrazi-e (3NPH)  reagent  is  frequently  encountered
The reagenc BusC be prepared w;:hin  five day!  of us*  in  ch*  field And Jnuac
scored in an uneor. laminated envi-orjaenc :oth before and  after aaapiirvj  in
oriar :o air.iaire blank problem.  Sooe concentration of acetone con:a.-air.j:
ii unavoidAbli. b*caui« acicona  Li ublqulcouf  In laboratory  and  fltld opera-
tions.  How«v«r. ;h« actcont eoncaalnatlon muse b« alniatud.
          Aarieui and
          3.5.^ -I   A ich«nacic of ch« taopUng  criin  Is shevn  In  Figurt
35-1   This sampling :rain eonf ijuracion  ii adapctd froa E?A Hcchod ^
proc«dur»a   Th« sanplLng craln conaLtet of eh«  following coopon*nc» .  ?
Nozzl*. Picoc Tub«, DLff«r«nctal Prtnurt  G«u|«. Mactrlng Syscta.  Baroatcer,
and Gas Density DtcermlnacLon Equipaenc.

          3.3.^.1.1 Probe Hocxle:  Quire*  or (lass vtth iharp.  capered (30*
angle) leading edge.  The caper shall be on Che  oucsida co preserve a cons:i.-:
inner diaaecer.  The nozzle shall be buttonhook  or elbow design A range of
nettle sizes mi cable far Isoktlnetlc laapllng should be available  In incre-
ments of 0.13 cod/16 in), e.g., 0.32 co 1.2? ca (I/I  to 1/2 In),  of larger .:
higher volume taapling train* are used.  Each nozzle the 11 b« calibrated
according co the procedures outlined In Section  3.3,8,1

          3.3.4.1.2 Prob* Liner:  Bores illcace glass or quart i  shall be used
for the probe liner.  The tester should nee allev the  teener a cur a  in che probe
to exceed 120 + lt*C (24t £ 25T) ,

          3.3.4.1.3 Pleee Tub*:  The Fttae cub*  shall  be Type 3, as described
in Section 2.1 of EPA Msehod 2, or any other appropriate device.   The pleot
tub* shall be attached to the probe to allow constant  aenitoring of eh* stack
gas velocity.  The  impact (high pressure)  opening plane of the  pitec tube
shall be even with  or above the nozzle entry plan (se* EPA Method  2. Figure I-
6b) during saapling.  The Type S pttot tub* asseably shall have a  known
coefficient, determined  as outlined in Section 4 of EPA Method  2.
-------
2.5       S«maLi!-.|  g?r A-.der.vde  Jf1|  -dtni,crophenyl-hydrtiint
2 . - - dir.i:r±ir.ilir.= , ±is be  ••• •r.ily^l?«L i«?«rfar*nc Lf concencraciont art
nigh.  2 , 4-DlnitroanilLn« can coaluta wlch 2 ,4-dlnlcrophenylhydrazona af
foraaldehyda und«r high perfonwnc* liquid chroaacegriphy condicloni, which
•nay be used far  eh« arvalyiii.   High coneencraelons of highly -oxygeoacad
compounds, especially 4eecan«,  chac have the iaM racenclon eia« or nearly :he
same retention  C!A* a* che  dinicropheny Ihydrazone of f ora*ld«hyde ,  and cha;
also abterb ac  160 na, will InCerfara wich che
                                      3-153
-------
          3,5.^.1.4 Differential Prtssure Gauge:   The differential  pressurt
gauge shall be an inclined .nanometer or aquivalant davLet ai described  :n
Section 2.2 of £?A Method 2.  One tnanoaeter  shail be used for velocity-head
raadir.g and the other for orifice differential prtsiure  readings,

          3.5.4.1.5 laplngars:  The sampling  ;rain requires a miniaua of four
ispingeri, connected as shown . in Figure 3.5-1, with ground glaas 
-------
                    IhMOKMMMi
liaui
-------
          3.5.4.2,5 Rubber Policeman and  Funnel;  A  rubber policeman  and
fur.r.al art required co aid in ;he :ranaf«r of oacsrial  Lnco and ouc of
containers in che  field.

          3.5.4.)   Reagent Prtparaclon

          3.5.4 3,1 Boteles/Caps:  Amber  I- or 4-L bottles wich Teflon- lined
caps ace required  for scoring cleaned DNPH tolucion.  Additional 4-L  boc-lei
are required to collect va«ce organic solvenci.

          ] 5 u.3.2 Large Class Concainer:  AC lease one large glass  (3 :o
La L)  .» required  for nixing che aqueous  acidic DNPH tolucion.

          3.5.4.3.3 Stir Place/Large Scir Bars/Stir  Bar Re cr lever   a oagneeic
scir plate and large selr bar are required for tha aixing of  aqueous  acidic
DNPH solution.  A  stir bar retriever is needed tot removing the) scir  bar  froa
she large container holding the DNPH solution.

          3 5.4.3.4 Buehner Filter/Filter Haslt/rilcer  Piper:  A large  fil:ar
flask (2-4 L) with a buchner filter, appropriate  rubber stopper, filter paper
and connecting tubing art required for filtering  the aquaoua  acidic DNPH
solution prior to  cleaning.

          3.5.4.3.3 Separatory Funnel;  AC least  on* large saparatory funnel
(21)  is required  for cleaning the ONPH prior  to  uae.
          3.3.4.3.6 iMkari:   Bcalurs  (130 al,  230 ml,  and 400 «1) art useful
for holdlng/«»a*urlng organic  liquids  whan cleaning  tha aquaeusj  acidic DNPH
solution and  fee weighing  DNTH crystals.

          3.3.4.3.7 ruunala:   AC  lease one) large  funnol li nee dad for pouring
che aqueous acidic DNFH  into  tha  separator funnel.
                                     3-isa
-------
gas iniLyrtc, If necessary  (»» described  Ln  E?A Method  3),   The  :enpera:~;t
sar.sor Lisa!!/ should be  permanently  attached  :a che  picas  cube  or  laaplir.g
r:33« ;r. a fixed configuration such chic  the cip of  ;hs  s«nior «xcends  btyor.d
the itadir.g edge of the probe shtach  and  dots  ROC  couch  any steal.   Al:«rr.a-
tivaly.  :hi str.sor say b« aciachtd juic prior  co mt  in  ch« field.   So:e.
hov»ver,  :•*: if :h« c«ap«racur« str.sor is aeraehtd  Ln  :h«  field. :h«  ser.scr
T.US; b« placid in an incirfirtnct-frte arrang*m«nc «ich  rtspicc  :o  the  Tvpe 5
pi:oc openir.gi dee IPA Hechod 2, Figure  2-T).   Aa a  iecond alserna-i'-'e .  if 3
difference of no more chart  It in che  average velocity aeaiurenen: is co  b«
ir.crsduced, che eeoperaeure gauge need nee be  aecached  ta che probe or  ;.:;:
          1.3.4.2   Saaple  Recovery

          3.5.4.2.1 Prob« Liner;   Prob*  nozzle  and bcuihee;  Teflon bciscle
brushes wich icainleii  tceel wire  handles are  required.   The probe brush shall
have extension* of scatnless sceel,  Teflon,  or  inert &acerial at  least as Ion;
as the probe.  The brushes  shall be  properly sized and shaped co  brush au:  :.-e
probe liner, che probe  nozzle,  and che  inrpingen

          3,3,4,2.2 Wash Bottles:   Three wash  beetles are required,   teflon  or
glass vash bottles are  recommended;  polyethylene  wash beetles should not be
used because organic  contaainancs  nay be extracted by exposure to organic
solvents used  for staple recovery.

          3.5.4.2.3 Graduate Cylinder end/ or Balance:  A graduated cylinder  or
balance is required to  ewasure  condensed water to che nearest I ml or I g.
Craduaeed cylinders shall have  division not ?< ml.  Labor* to c=y e«l*n««i
capable of w»l§hing eo  ±0.3 g are  required.

          3.3.4.2.4 Aaber Class Storage Containers;  On*- liter wide-aouch
aober fline  glass bottles vith  Teflon* lined caps  ar* required to  store
iapinger water saaples. The boecles dust be sealed with Teflon tape,
                                      3-157
-------
          3.5.5.4   2>-dini::oph«r.ylhydca*i.ne  (ONPH),  ( 2 .4- (0,N),CIH,;SH.VH1 -
The quins i ~J of vacsr nay vary  from  10  so  30%.

          3. 5. S.fc.i The 2>-dini:rophenylhydrazine  rsagenc ausc be prepared 1-
;he Laboratory wi:hin five days of laopUng use  in  che  field,  Preparation of
:N?H can also be done in che field,  with coneLderaclon  of appropriaca proce-
dures required for iaf« handling of  loLvtnt in  eh«  fitLd.  U*h«n a cpncair.tr =f
prepared ONPH raagcnc ii opantd in :h«  fiald, th« cgnctncs of ch« opened
concain*r ihouLd b« o««d wichin ^8 hours.  All  laboratory §I«*iwara aui; b«
washad «i:h d«ctrg«nc and wac*r and  rina«d wich  wac«c,  ««chanol, and cntchy.are
chloride prior co
N'OTE.     DNPH crytCll* or ONPH lolucion should b« handUd vtch plastic glov«i
          ae all cijua wich proapc and txcaniiva oi« of rxmninf wacar in cai«
          of akin «xpoiur«

          3.3,3.4,2 Preparation of Aqueouj Acidic DNFH D«rlvacUtng Reaginc:
Each bacch of DH7H reagenc should b« prepared and purified wichin five days ::
saapling, aceordinj e» the procedures described be Lev.

NOTE;     Reagenc boctles for storage of cleaned DNPH darlvacizing solution
          ouac be rimed wich aceconicrile and dried "=«fore u»e.  Baked
          glassware is noc es«encl*l for preparaclo-  : DMPH reagenc   The
          glasavtr* mat, DOC bej riru«d wich »ce^^-;  r an unaccepcable concer. •
          crtcion of ace ten* concajitnacion will be Incroduced.  If field
          prep«racioo of 09111 ii perforMd, eaueion mat b« exercised in
          avoldinf Aeecoftt contajiinaclon.
          3.3.3.4.2.X    Pl«e« *n 8 L concain«r under «  fusM hood on a
nagneclc scirr«r.  Add • Urf« seir bar and  fill  chsj concainair half full of
organic- free reagenc water.  Save th« eitpcy  beetle  frost  cha organic -free  '
reagent water.  Start tha stirring bar and adjuae tha atir rata  to b« as fas:
as poaaible.  Uaing a graduated cylinder, naaaura l.fc •! of eoneontracad
hydrochloric acid.  Slowly pour the acid  into  che stirring wacar.  Fuaes nay
ba generated and che water aay become wars.  Weight che  DNPH crystals on a
                                     3-160
-------
          3.5,4,3,3 Gradua:ed -yUr.deri:  AC  lease one large gradua:ed
:•/•. L-iar (1 :o 2 L) la required far aeasurir.g organic -free reagent wacer'ar.i
ac:i when preparing the DN?H solution.

          3.5 - 3.9 Top-Leading Balance:  A one-place  :op  loading balance -.s
needed foe weighing ouc the DNPH crystals used  to prepare  :he aqueous ac.i:c
3NPH solution.

          3.5.^-3,10 Sp*cula«;  Spaculas ace  needed  foe weighing ouc DS?H .-.a-
preparlng the aqueous DNPH  10Luc ion.

          3.5 * ^   Crushed Ice:  Quanci:ies  ranging from  10-50 Lb may be
necessary during a stapling run, depending upon aablenc ceoperacure.  Stap.es
which have been caken ousc be scored  and shipped cold; sufficienc Ue for z'-Ls
purpose auic be allowed

3.5.5

          3.5.5.1   Reagenc grade chemicals shall be used  in all cescs.
Unless ochervtse  indicated, ic  is  intended chac all  reagents shall confon :;
:he specifleacioni of the Conaittee on Analytical ReegenCi af che Aaerizan
"hemical Soeiecy. where  such specification* are available.  Ocher grades lay
be used, provided  Lt  li  fine ascertained  chec  che reagenc li of sufificier.c./
high pur icy co  penic lea uje vicheue lessening the  eecurtey of che  decersi-i
:ion.
           1.3.3.2   Organic-tree reagenc v«tec;
      aecho^ refer to organic-free reagenc water,  aa defined in Chapter One

           3.S.9.3   Silica Gel:   Silica gel itul! be indicating type,  6-16
 mesh.   If  che silica gel haa been used previously, dry ae 17S'C (HOT) for  2
 hours before using.   New silica gel nay be used aa received.
 other cypea of deeieeancs (equlvalene or beceer) nay be used.
                                      3-139
-------
                                Table  3.5
                 APPROXMIATE AMOUNT OF CRYSTALLISE DNPH USED
                       TO PREPAAE A SATURATED SOLUTION
       Aaouns  of  Moiacuri  Ln  DNPH
Waighc R«quir>d par 8 L of Soluclon
           LO ufighc p«rc»nc
           15 wfighc parctnc
           30 w«ighc pareanc
                31
                31
                               Table 3.5-2
               INSTRUMENT  DETECTION  LIMITS AND REAGENT CAPACITY
                          FOR FORMALDEHYDE ANALYSIS1
Analyti D«ctccion Limit, ppbv* Raa(«nc Capacity, ppnv
Foranld.hyd*
Ac«c*ld«hyd«
Aerolfin
AC« cons/Prop Lonaldthyd*
3ucyrald«hyd«
MtchyL tchyl kccoM
VtiirtldahydA
I tov«iti«id«hyd«
H«x«ld«hyd«
BvnzaldAbyd*
o • /• • /p • TolutlcUhyd*
D Lmt ehylb«nx«ld4ihyd*
1.3 66
1.7. 70
»
1.
i
i
^
75
75
79
79
84
1.4 84
1.3 88
1.4 84
1.3 89
1.2 93
     L0xyg«n*t«d covpoundt  In tddicton co fora*ld«hyd* ira Ineludad for
companion with fera*ld«hyd« ; •KCtrulon  of  ch«  iMChodoloij Co och«r coapouniii
It poitibla.
     ID«cieclon  llaiei art
r«pr«i«nc ch«  opcloua
   Ln  tolvtnc.  Th«§«
                                                               chtr«fert
                                 of
                                    1-162
-------
ont-pUct balanct  (see  TabU  3-5-1 for approximet aaouncs) and add :o ;'-«
ssirri.-.g acid solacian.   Fill  :h* 8-L concmir.tr :o cha 8-L mark wi;h orjar.i;-
free rea§«ne wa;tr  and  jcir ovtrnighc-  If *li of che QNPH crystals hav«
disso'.vad ovarr.ig'r.;,  add additional QNPH and stir for two sort hours,
:ar.:ir.ua :ha prices!  of addir.g 2M?H wlch addicianal stirring un:il a sa:ura:e:
solution Has bttn  !arni«d.   "Lliic ch« DNPH solucion uiir.g vac-ua 5i'.:rar::r.
Gravity filzracian  may  b«  used,  buc a such Long«r slat is rtquicid.  S:sre :.-.*
:Ll:trad solucion  in  an aabtr  boc'la ac room c«mp«racuri

          3.5.5,4.2.2    "*L;hin fiva days of propoiad u««, piac* abou- '..6 '_
of  ;ha ;s?H  reagtnc in  a 2-L  scparacary funnel.  Add approximately 200 al ;:
ratthyltna chlocii*  and  icopp«r rh« funniL.  ?«rap :h« icopp«r of ;hi fup.r.el
wtch pap«r  :ow«l§  co  abiorb any i«akagt.  tnv«rc and vone ch«  funn«L.   Then
sh*k« '/igorouily foe  3  ainucas.   Initially. ch« funntl should  b« vancad
fraquanciy  (avary  10  -15 sac;.  Afcar ch* layers hav« s*p«racad. discard  ;ha
lowtr (organic)  lay*r.

           3-5-5^.2.3    Excracc ch«  DNPH a sacond cima wlch o«chyL«na
chlorida and finally  with cycloh«x*n«.  Whan ch» cycloh»xan* layar has
»«paracad  fro« eh* DKPH reagtnc.cha cycioh«x»n« lay*r will b*  cha  cop layer .-
:h« stparacory funnel.   Drain cha  lower layer  (che claaned axerace DNPH
roagant solucion)  ince an aabar boccla chat has been rimed wich aceconUr •. le
and allowed co dry.

           3,5.3.4.3 Quailiey Control:  Take  cvo aliquots of  Che axcraccad  DKPH
c«agene.   The  six* of the aliquoci  It dependent upon  che  a«act taapling
p»9<:*<*<,!!•*  
-------
         purposes,  2.t-dini:rophenylhydra*ine  is a.flammable solid when dry.
so vacer should noc be evaporated from ;he ioiu;ion  of the reagene.

          3.5.5.5   Field Spike Scand-srd Preparacion:  To prepare a formalde-
hyde field spiking itandard ac i.Ol ng/ml.  use a 500 Ml syringe co transfer
0.5 al Co 37% by weight of formal ehyde (401 mg/ml)  co a 50 nl voluatcric
flask containing approximately 50 ol of aechanol.  Dilute co 50 al vich
-lechanol-

          3.5.3,6   Hydrochloric Acid. HCL:  Reagent grade hydrochloric acid
(approxiaacely 12N) ii required for acidifying che aqueous DNPH solucion.

          3.3.3.7   Methyleno Chloride, CH,Cl,:   Mechyleno chloride  (juicable
for residue and pesticide analysis,  CC/MS.  HPLC, CC, Spectrophotoaecry or
equlvelent) la required for cleaning the aqueous acidic DNPH solution, rinsing
glassware,  and recovery of saople eralas.

          3.3.3,8   Cyclohexane, C,HU:  Cyclohexane  (HPLC grade) is required
for cleaning che aqueous acidic DNPH solution.

NOTE:      Do nee uae ipeceroanalyxed grades of Cyclohexane If this sampling
          methodology la extended to aldehydes and ketones with four or acre
          carbon a COM.

          3.3.3.9   Nethanol, CH,OH:   Neehanel (HPLC grade or equivalent)  is
required for rinsing glasavare

          3.J.3.10  Aeeeonltrlle, CK,CM:   Acetonitrlle (HPLC grade or equiva-
lent)  Is required for rinsing glassvare.

          3.3.3.11  Formaldehyde, HCHO:  Analytical  grade or equivalent
formaldehyde la required for preparation of standards.  Iff other aldehydes or
kecones are uaed, analytical grade or equivalent Is  required.
                                     3-16i
-------
:apt.   Af:tr ;ht bocilt  ii  labeled.  :ht  bocele  may  be  placed  In a  f ric::;r.- ::
= an ^painc can or equivalent) containing a  1-2  Lr.ch layer  of  granulaeed
;r.ar;oal and scored ac ambient  :emper*cure  until  use.

          ] 5 3 -.-.I     If  ;ht DN?H  reagenc  has  pasaed  :he Qualiry Car.zra'.
;ri:eria. ehe rsagenc aay be packaged co rates ntcassary  *hipping ttquLrestr,:i
ar.d stnc :s :ht sampling  ar«a,  If  :ht Qualify  Concrol crictria art -o:  =e:
:'r.e reagsnc solution a«y  b«  ti-*xtrac;td or ch« solusion aay  b* rt-preparsi
and "~« •xc;ae;ion i«quenca  rap«aced.

          3,5.5.4.4.2     If  sh« DNPH  rtagtnc  ii nee us«d in  cht fitld wi:hi-
fi'.-t days of txcraeeion,  an  allquoc nay  bi  ;aktn  and analyzed as dtacribfd  :.-
Mo;hod OOllA.  If :h* rtagtn: atacs  ;he  Quality Concrol  r«quir««tncj .  :ha
rtagenc aay b* uJtd.  If  eht r«ag«nc  do«i noc ottc  ch« Quality Control
rtquirto»nci , ch* rtagane ouac  b« discacdtd and new raagenc cause b« pr«parad
and c
          3,5.5.4  5 CaleuLaclsn  of  Aectpcabl*  Concenerationt  of Iapuri:its  -~
"NPH Rtagtne:  The accapcabl*  Impurity conctncracion (AlC.  ug/nl)  Is  caL:-!^:-
td from ch«  •xpiceed  aaalyct concincracion In  eht  saapltd gai (EAC, ppbv) ,  :-e
vol-jat of air  chac will  b*  $aapl«d  ac  icandard condicions (5VOL.  L) ,  :h«
formula wtlghe of  eht aaalyct  (FV,  g/ool) .  and eht volua* of  DHPH  rtagtnc  :~a:
•-'ill bt uiad In  eht  Lapingtri  (RVOL. ml) :•

AtC - 0,1 x  [EAC * SVOL  X fV/22-4 * (FW • ISO)/F«I (IVOI. * L.OOO)
          O.I  It  ch« acctpcablt concaainanc conctncrtcion,
          22.4 ii a factor rt lacing ppbv so g/L,
          180  Ii  « ftceo relating und*riv»clr«d CB d*rlv«tirtd analyct
          1,000 !• a unlc eonvtriion factor.

          3.3.3.4.6 DUpoial off Exctia ONPH Rtagtnc:  Cxctst ONPH rtagtnc aa
 bt  r«curntd ca ch* laboracory and rtcyclid or trtactd aj aqiotovu watet for
                                      3-163
-------
char.gi the nozzle/  Ensurt that -~.t propar dif ftrtntiai pressure gauge is
chosen for the rang* of velocity heads encountered  (see Section 2.2. of
-err.od 2)
          3.5-6.3.3 Select a suitable probe  liner and probe length so that il".
:rav«rse points can be saaplad.  For large stacks, to reduce the length of :-«
probe, considtr stapling froa opposlc* sides of  the stack.

          3.3.1.3.4 A ainimua of ^5 Cs1 of saapU voiuae is required for zr.e
deeerain*cion of the Descraccion and Reaoval Efficiency (DIE) of CoraaLdehvde
from  incineration systems (43 fe1 is equivalent te one hour of saapling a-
0.75 dsef).   Additional saaple voluae shall be collected as necessitated by
:h« capacity of the DNPH reagent and analytical  detection liait constraints.
To determine die ulniaua saaple voluae required, refer ea saaple calculations
in Section 10,

          3,5,6,3.3 Oecensine the tocal length of taarpllng elae needed  to
obtain the identified ainiarua voluae by coaparing the anticipated average
sampling rate with the voluae requireaent.  Allocate the saae ttae co all
traverse points defined by EPA Method I.  To avoid tiaekeeptng errors,  che
length of ciae taapled at each traverse point should be an integer or an
integer plus 0.3 Bin.

          3 5.6.3.6 In SOCM circuaatances (e.g., batch cyclee) it aay be
necessary to saaple for ehorter tlaai at  the traverse point* and to obtain
smaller gaj-voluM saaplec.  In these eases, careful documentation aust be
maincaLned IB ordar to allow accurate calculation of concentrations

          3.3.1.4   Preparation of  Collection Train:

          3.3.6.4.1 During preparation and asseably of  the saapling train,
keep  all openings where contaaination can occur  covered with Teflon fila or
iluainua foil until Juae prior to assembly or until saapling if about to
begin.
                                     3-166
-------
-  5 *     S*«Pl« -?ol\jr;'.r-  ?-«««rv*=iar-  *r.d  Handling

          3 5.6,1   Because o£ :he complexity of  :his aethoa,  field  perscr.rel
should be :rair.id in and exparitnced wish  she :sst  procedures  In  orfer  :a
obtain reliable resales .

          3.5-1.2   Laboratory Preparation:

          3.3.6.2.1 All the coaponenes  shall be aalntainad  and calibrated
according :o cha proc«dur« dascribtd in APTD-0576,  onl«si ochirwin  sptcifiec:
          3,5.6.2.2 r-«igh i«v«r«l  200  to  300  g  porcions  of  fiUca-giL  in
ai.r;ighe conc*in«ri eo  ch« n«*rist 0,5  §.   Rtcord  on  «»ch concaintr  ch*  :o;a'.
•jeijhc of =h* sllLc* gel plua conc«in*rs.   As an alcira»civ«  :o  priw«ighing
chc ilLLc* g«l, Le a*y  Lnaciad b»  w«lgh«4 dirtccly in th« Lfflpingtr or  sanpLir.;
holder Ju*t prior ta train
          3.5.6.3   Prtliainary Field  0«c«rtBinacioni :

          3.5.6.3.1 Select che sampling  tiea  and  eh* minioiua  nuab«r  of
sampling poinc according  es EPA Method I  or other relevant  criteria.  D«:ec-
•aine the itack prenure,  teaperacure,  and range of velocity head* uaing  l?\
Method 2.  A  leak-check of che picac line* according to  EPA Hachod 2, S«c :.;.-.
3,1. nuac be  perfonMd.   Deceraln*  th« scack  gaa  aolicure content oiing  E?A
Appcaxiaacion Mechod 4 or iti alcenuiclvea eo eetabliih  escioatei of iaokina-
:ie s«aflln§*r«c*  ••celnfi.  u«c«rvin* &n* *****  gas dry sslscul-; y-l»hr.  **
described la  EfA K«chod 2, Section  3.6.   If  integrated EPA  Method 3  saapiir.g
U used  for aclecular weighc deteraination.  the  integrated  bag iaopl« shall be
:aken jinulcaneovuly wlch. and for  the saae  total length of tiaw aj .  the
aaaple run,

          3.3,6.3.2 Select a nestle •!<* baaed on the  range of velocity  heads
so  chat  Is noe neceesary  eo change  the nozzle size in  order co maintain
isokineelc laopUng races below  21  L/ain (1.0 cfa). During che run, do  r.o:
                                     3-165
-------
          3-5-6-5   Laak-Chack Procadura*:

          ].1.6.5,1 Pra-casc Leak Chack

          3. 3. 6. 5.1. L    After ehe laapLing crain haa baen assaoblad,  :urn on
and lac :ha probe heaclng iy»ca» «c ehe daalead oparaclng tamp«:»curt.  Ai'.=u
:ine for :h« eaaperacura co scablHza.  If a Vlcon-A 0-rlng or ochar  Uak-free
connacclon Is ujod Ln aasaabling cha preba nozzle co cha proba liner,  Laak
chack :ha crain ac cha aaapUng jlea by plugging  cha nozzle and pulling A 33'.
T.I Hg (IS in Hg) vaeuua.

^OTE:     A lowar vaeuua nay ba ujad.  provldad chac cha lovar vmcuum  ii noc
          axeaadad during cha caic.

          3.3.6.5,1.2    If an aibaieoi icrlng Is uaad, do nee eonnaec cha
proba eo cha crain during cha laak cheek.  Injcamd, laak-chaek cha train by
flrac aceaehlng a carbon-fIliad laak check ioplngar co cha tnlot and  Chan
plugging cha inlac and pulling a 381 •• Hg US In Hg) vaeuua.  (A lowar vacuum
any ba uaad If  chls lovar vaeuua li noc axcaadad during cha caac.)  Maxc
eonnaec eha preba co cha train and laak-ehack at about 25 an Hg (I In Hg)
•/acuua,   Alcanuclvoly, laak-ehack eha prob* with the rate of cha laopling
-.-tin in ona tcap ac 301 OB Hg (15 In Hg) vaeuua.  Laakaga racaa in axcaas of
(a) 4| of cha avaraga aaopllng raca or (b) X).00037 «J/»in (0.02  cfa), ara
unaecaptabla.

          3.3.§.3.1.3    Th« folloving laak chock Inacruccloru for cha
sampling craln d«acrla4 la ADfT-057* and APTD-0111 m*j b« halpful. Scare cha
puap wich clM flo«-adjujt valve fully open and eoarta-valve cooplecely cloiad
Partially op«n  ch« co«rso*adju«e valve and •lowly elett ehe flne«adju«c  valva
uncll cha daa1rod VACUUM la raachad   Do noe raveraa dlracclon of ehe  fine-
adjuac  Uva,  aa liquid will back up Inco ch« erain.  If ehe daairad  vaeuua is
•icaad    eleher parform ehe leak check ac chit higher vacuum or end  ehe laak
chtck. ax ahovn belov, and icarc over.
                                     3-168
-------
          3.5.6.C.2 Pita  ".00 ml  a£  cleaned  ONPH  solucion  in  each  of  :r,«  f
:vo iapir.gtrj, ard leav*  :hi  :hird  iflpirgar  smpey.   If  addirionaL  capac::-.-
re-uired for high expec:ed cancan.zracion.j  of faraaLdehyda  in  :he slack  gas
ICO al of 2SPH per i^pir.ger say be  used  or addi:ional  iapir.gen may be  .sa
far sasplir.g.  Trar.sfac approximately  200  to 300  g  of pre-veighed  silica  j
froffl i:a container -3  "ha  fourch  iopingar.   Cara  should ba  :akan to ar.s-.re
:hac :he silica j«L is r.ot vncrainad and carriad  ouc  fron  :h«  iapir.gar
sampling.  Placa :ha silica gal concainar  In «  cLaan placa  or  lacer use  .-  :-
saapla racovary.  \LcacnacivaLy,  ;ha waighc  of  cha  tLlica  gal  plui  iap-.r.^er
may b« dacarainad :o cha  naarasc  0.3 g and racordad.               r

          J .  5 6 , i 3 '-L;ii  a glass  or  quartz linar,  inicail  cha  saleccad  r.;::.e
using a VLcon-A 0-ring wich scack caaparacurai  ara  <260'C  C500T)  and a  vo-.-er.
glass-fvbar  gaskac whan :a»paracuras ara hlghar.   Saa APTO-05'6  iRom,  .I'll
for dacails.   Qchar connaccion  sytcaas uciUrLng  althar 316 icainUis s:eel  :
Taflon Carrulas may ba ujad.  Mark  cha proba with haac-raslscant :ap« or by
soaa ochar aachod co danoca ch* propar dlscanca Lnco  cha  scaek or  due:  far
each saapling poinc.

          J.S.S.u.i. Aiaaobl*  cha  train as  shown in  Figure  3.3-1.   During
assaobly, do noc uia any  lillcona grease on  ground-glass  Joincs  upstream o:
:ha iapingtri.  Us* Teflon cap*,  Lf raquirad.   A  vary Ughc coating of
silicon* graaa* aay ba used en  ground-flan  Jolnci  downjcraaa of cha
implngars. buc  cha iilicon* grease  should  b« UaLtad ce eh* oucar  portion
APTD-OJ76) of cha ground-glan  JolnCJ  to ainialza silicon* graaaa  concaair.a-
  ion.   If n*c*isary. Teflon cap*  aay b*  u««d co seal l*«lu.  Connect  all
  s=?«r§?urf  ••"§or»  ca an approprlcc*  poc*ncloa*c*r/dlspUy unic,   Check all
  eaperacur*  ••niort  ac aafalanc  caaparacurai

          1.3.6.4,3  Pl*ca crviihad ica  all  around eh* laplngan.

           3.S.6 4.6  Turn on and s*c ch* prob* h**clng syicaa ac ch* dasirad
  pacacing  ceaparacura.   Allow cia*  for  ch*  c*ap*r»cura co scmbllUe.
                                      3-167
- 4
0
-------
       (0,02 C£B)  or s.% of che average sampling net (which«v«r  U   :ii).  :.-«
        ara acceptable.   If. howevar,  a highar  Laakage  rate  Li  obtained,  :'-«
:es;er snail record :he  Leakage  race  and void che  sampling run.

          } . 5 . 5 . 5   Sampling train Operation:

          15661 during che sampling run, maintain an  isoklnetic  sanpUr.j
race ~o viihin 101 of  crue isokinetic. below 20 L/nln (1.0 da) ,  .".air.zai- a
temperature around the probe of  I20'C  (24fl* + 25'F).

          3.566-2 Tor each run. record che daea  on a  daca  iheec lueh  as  :r.e
one shown in Figure 1.5-2.  9* sure ce record che  Initial dry-gas oecer
reading.   Record che dry-gai oecer readings ac  che beginning and end of each
laapLing time increment,  whan changei  in flow rate* are ud«, before and  af:er
each leak check,  and whan ianpllng Is haIced.   Take other readings required by
Figure 2 ac Lease once ae each sample poinc during each do* inereaenc  and
addlclonsl  readings when  significant  adjusea«nef 20* variation  In valocicy
head readings) necessitate additional adjuscMncs  In flow race.  Laval  and
zero che oanoaecer.  Because che «*no
-------
          3,5.6,5.1,4     «k«n  -*•  leak  chick is  coiputed,  fine  slowLv  re=ov-
:h« plug froB che  inlet  co  cha probe.   When  che  vacuum  drops  co  L27  am  (5  ;-
Hj or '.€91. immediately  cioi«  che  coane-adjuic  valve.   Switch aff  -hi  pus?:.-.*
svs:tm and rtepen  ;he  Sine-adjust  valve.   Do not rtoptn che £ir.e-idl us:  valve
.-til the coarie-adjua;  valve  has  b«tn  cioiad :o prtv«nc :hi  liquid  L-  :he
:.?.p ir.gt cs £zo« b«in§  foccad backward  in :h«  sampling ILna and silica jel fr:-:
-aing ancrainid bickvmrd in:o  chi  chlrd iopLng*r.

          3.3.6,5.2 L*«k Ch«cki  During  Stapling  Run:

          3.5.6.3.2.1     If. during :h« SAapLing run,  a conpontnc changt
(..t.. Itnpingtr) baeoa«i nactuary.  a l««k check shall  b« conducted '.aa*£:.i-i -
ly afcar eha  incsrrupcLon of stapling and b«fort eht change is aade.  7h«  '.
check shall be don* according  co che  procedure described In Section 3.5.6.
excepe chat is shall  b*  done ac  a  vaeuua greater Chan or equal "o che aa
value recorded up  co  chat poinc  in che  case.  It che leakage race ii found :s
be no greater Chan 0.00057 a3/Bin  (0.02 cfa  or 4% of the average  saapllng  :a:a
(whichever  La leaa),  th* results are acceptable.  If a higher leakage rare .s
obtained,  che tester  aust void ch* sampling run.

N'OtE;      Any correction of che  saaple volume by calculation reduces che
           integrity of the pollutant concentration data generated and BUS: :«
           avoided.

           3.5.6.5.2.2    lasted lately after  a coa^onent change and before
 simpUng is reinitiated, a leak check  ilallar co a pre-cest leak check auic
           3.5.6.3.3 Post-tesc Leak Check:

           3.5.6.3.1.1    A laak chick  li «*ndatory  at  tha  ccncluaton of each
 stapling run.  Ih« leek check shall be don*  with  eh* iaa*  procedure* as che
 pre-taat leak check, except  thae  th* post  cest  leak ch*ek  shall b« conduectd
 at a vaeuua greater than or  equal co eh* aaxlau*  v*lu* reached during  the
 sampling run.  If  ch*  leakage race  Is  found  to  be no greacer  chan 0.00057
                                      1-169        .   .
-------
          3,5,6,6.4 Whin thi scack  is under  significant  nagactva  prassura
•lequivalanc co chs haighc of cha  Lnpinger  seen),  cake  car*  co  cloic  che
:aacse-adjus: valve before inserting che probe  Into  cht  icaek  in  order  :o
?rev«nc Liquid from backing up through  che Grain.   If  necessary,  che  pump  say
3e turned on with che coarn• adjust valv*  cLoi«d.

          1.3.6.65 Uhan ch« prob*  is in potUion, block off :ht  op«nin;s
around cht probt and scack aectis perc  co pravtnc unrtprtstncaelvc dliu:ior.  ::
:h« gas icrtaa

          3,5.6.6,6 Traverse cht  icack  cross  stccion,  as rtquirtd by  EPA
Mtchod I. being careful noc co bump che probe nozzle  into che  scack walls  vher.
sampling near ch« wails or when removing or  inserting  che probe through che
access pore, in order co alnialze che chance  of txcraccing  deposlctd  aecerial

          3.5.6.6.7 During che cesc run. isaxke periodic adjuecaencs co keep :ha
itnperacure around Che probe *C che proper levels.   Add  oere ice  and, IS
r.teassary, jalc. co aelneain « csaperacura of <20*C  (6ST)  ac  che silica gal
ouclec.  Also, periodically check che level  end zero of  che aanoaectr.

          3.5.6.6,3 A single train  shall bejused for  che encire stapling rur.
excepc in cases where tioulcaneouj  saapling  Is  required  in  cvo or no re
separace ducts or ac cvo or acre  differenc Location* wlchln che sea*  ducc, or
in cases where tqulpejenc failure  necesslcacee a change of cralnj. An  addition-
al crain or addiciooaJ. eraltu svay also  be  used  for  sasqiling when  che  capacity
of a single craia it exceeded.

          3.S.i.$,9 When cvo or «ore cralnj  are used,  separacs analyse* of
cooponenci fron each eraia «h«ll  be performed.  If aulciple  eraina have been
used because che capacity of a single crain  would be exceeded, fine  tapingers
froa each crain aay be coabined,  and second  lapIngers  froa  each crain aay  be
coabined.
                                     3-172
-------
                                                                      Mote LMfytt
                                                                                           f •*•»***«
                                                                                                     l*MfMH
                                                                                                       Jo
o.
                                                                                                      fenulrapi
                                                                                                       •cm
I nf Minn
        i No

-------
          3,5.7,1.5 Savs 4 porcian of  all  vaihlng  solution  (nechyLena  ehlo-
   t, vacar) usad for citanup 41 a blank.   Tranjfir  200  al  of  each  soLucion
   «c:ly froa cha wash bocsla biing used  and  placa «ach  In  a separate,
                  container.
          3.5.7.2   Saapla Containers:

          3.5.7.2.L Container  L:  Probe and  lapinger Catches.  Using  a
graduated cylinder. oeasure to  che naaresc al,  and  record  the  voluoe  of  :^a
solucion in ih« fLrsc chrtc vapLngan.  Alc«rnaciv«ly ,  ch«  tolucLon aay  ba
•JiLghad ;o ch« naarcic 0.5 g.   Include any eondaniae*  In th« proba  Ln chis
d«c«rtainactan   Transfer :h« iapingcr lolucton  froa eh« graduacad cyUndar
in=D ch« aab«r flinc gL«n beccLc.  Taking ear* ch«c dujc  on ch« ouciid*  o£
:ht prob* or och«r «xc«rlor surfacai do«a not g«c  Lneo  eh«  lAoplc, clean all
surface! Co which che saople lj expeicd ( Including  che  probe netzle.  probe
ficclng. probe linetr, fine laptnger, and Lapinger  connector)  with m«chylene
chloride,  Ute lea* than 300 al for che entire  vaah (230 ml would be  bec;«r,
L£ poiflble).  Add the waahlng  eo ehe scople container.

          3.3.7.2.1.1    Carefully reaeve che probe noxzle  and rinae  che
injide surface wlch aeichylene  chloride froa a waah  boccle.  Brujh wlch a
Teflon briiele bruah. and rioae until che rtnae ahowa no visible parclcles or
yellow color, after vhlch aak«  a final rlnje of che Inalda  surface.   Bruih and
rinse che iruida parti of ch«  Svagelak fitting  with aaehylana  chloride in a
sLailar vay.
          3.9.7.2.1.2    ainae  the  probe  liner  with MChylana  chloride.
squirting the) atchylena chlorlda  into  che upper end of  the  probe,  tile  and
rotate the probe ao chae  all  Inald* surface* will  be veeted with  «e thy lane
chloride.  Let the aochylene chloride  drain fresi the lover  end Into che saaple
container.  The ceater aay uae  a  funnel  (glaat  or polyechylene)  co »id  In
transferring che liquid waahes  to che  container.  Follow the rinae with a
Teflon bruah.  Hold ehe probe  In  an inclined poeleton.  and  squire  aethylene
chlorlda  Into the upper end as  the  probe  brush  !• being pushed with a tviicLr.;
action chroufh che probe.  Hold the sample container underneath the lowar end
                                     3-1-4,
-------
          3.5,6.6.10     AC  :he and of  ;ht  stapling  run.  curn off  :he  caarse-
adjus: valve, ranova che probe and nozzli  from  che slacks,  turn off  che  puap .
recsri :ht fLnal dry gas sectr reading,  and conduce  4 pose- case  Leak chack.
Also, leak chick cha pi:oc Unas as dtscribid in  EPA Machod 2.   The lines -5.5
;ass iris leak chaclc in order co validate  che va
          3. 5. 6. 6. LI     CaLcuLaca parcenc  isokinacicity  (sit Meehod  2:  ;a
          who char cha run was valid or anochar  :asc  ihouLd ba madi .
3.5.7     Sajrpla Raeovacv

          1.5,7.1   Praparacion:

          3. S, 7. 1,1 Proper claanup  procadura baglni  «•  soon  ai  cha proba  is
rinovad froa  ch* stack ac cha and of  cha  laapling  period.  Allow  cha  proba  :s
coal.  «"han cha probe can ba handled  aafaly, wipa  off all  excamal parcicui*:
raaccar near ch« clp of the probe noizle and place  4  cap over cha  tip  EO
prevent lottng or gaining parciculace aaccer.   Do  not cap  che probe  cip
cighcly whlla che iaapling crain la cooling because  a vacuua will be  creazei
drawing Liquid from cha  lapingars back through  cha aaapling  crain,

          3.3,7.1.2 Before moving che laopling  crain Co che  cleanup si;a,
remove che probe fro* cha •aopling  era inland cap che open  ouclec. being
careful nee ca lei« mny  eond«nja.ce  chat alghc be preicne,  Reaove che uabll:
cal  cord  froa che l«4C lop Inge r and cap che laplnger.   If  •  flexible  Line  is
ujed. lee any cond«rued  water or liquid drain  into the  tapingeri.  Cap off  ar.
open Lnplnger inleea and outlece.   Ground gla«i • toppers,  Teflon  caps or  caps
of ocher  Inare aviterials say be used  to leal all opening! .

          3.5.7.1.1 Transfer che probe  and laptnger  aaieably eo in  area  cha:
is clean  and  protected froa wind so chac  cha chance* of eoncaainaclng or
losing che  saople are ainiaized.

          3.5,7.1.4  Inspect  che train before  and during disasieably,  and  note
any  abnormal  condition*.
                                      3-LT3
-------
'-ydrazone is * solid which  floats and  frochj  on  :op  of  cha  tspinger  iolu:iar.
Ar.y physical carryover af col'.ictad aois;-r*  inro  :he second  iapingar viLl
invalidate a breakthrough assessment.

          3,5.7.2,2 Container  2;  Staple  Blank.  Prepare  a  blank by  uiLr.g an
amber flinc glass concainer and addlr.g  •  volume  of DNPH reagent and  oachyler.e
chloride equal to che total vol.ua* Ln Concainer  1.   Process the blank in :he
     nannar a« Container 1.
          3.3.7.2.3 Concaintc ):  Silica Gil.  Noc«  ch« color of  ch*
i-.g silica gal co d«t«nnin« wh«ch«r  ic ham b««n compl«c«iy  ip«nc  and aaki a
r.otacion of Its condition   7h«  iapingcc containing  th« silica  gal oay b« ,se-
aa a saapl* tracuporc containtr  with boch andJ italtd with  cighcly fitting
capi or pluji.  Ground -jl»J« icoppcra or Taflon caps uyb«  uu«d.  Th« silica
gal impingtr should eh«n b« lab«l«d, eev«r«d vlch aluaiinua  foil,  and packaged
on ice for cruuporc co cho laboratory.  If eh« silica |«1  La raaovad froa  the
imping«r. ch« ctacar aay u*a a funnel co pour ch« silica (•! and  a rubber
policiaan co rtoMv* ch« silica f«l froa eho impingac.  Ic la nee  n«e«iiary  -.3
-«mov« cha aoall aaoune of dusc  parciclaa ch«c nay adhara co ch«  iapingtr wall
and ara difficulc co raaova.  Since  cht gain In weijhc It eo be uaad for
moiicure calculaclon*, da noc use wacer or ochar liquid* eo transfer the
siLLea gel.  If a balance la available in che field, the apene  silica gel (or
silica gel plua iaplnger) aaybe  weighed eo che neareac 0.3 g.

          3.3.7.2.4 Sappl* concainers should bo placed In a cooler, cooled by
(although noc In conucc vlch) ice.  Sample concainere Buac be  placed varci-
cally and. since they are (laja, proeecced frost breakage durlny; shipment,
Samples ihould b« cooled durinf  ehlpaenc so they will be received cold ae :ha
Laboratory.
-------
of :he probe, and catch  any aeihylane  chloride,  vactr,  and p*r:icu:a:e  =a::e:
:hac i.i Crushed  from  che  probe .   Run :ha  brush  ihrough  the probe  :hr«a  :l3Bs
or T.O re.  -Ich siainlau  i:eel  or achtr aacaL probas,  run :ha  brush chrs'-jh  .
t'-a tbo''« prescribed  manntc *c  *.a»»c six  ;i,nie»  linca  chare say b«  small
cravices  in which p*rt '.culaca nac:ar can  b«  «n:rapptd.   R:ns«  :ha  br^sh vi:-
.T.e:hyl«r.t c^lorid*  or wactr,  and  qu»nci:a:ivtly  collte: :h«j«  vaihi-j  ir. :r.e
samplt concaintr.   Afc«r  Che  brushing, nakc  a final  rini« of  ;^«  prob*  as
N'OTE :     Two  p«opl«  ihouid  clean  :ha  probi  in order co  ainimize
          Lossei    Becveen jaapLing rum ,  brushei  avmc be  kepc cltan and ;r°e
          froo conc*ffllnjcion

          3.5.7.2.1.3    Ulnse  che Lniida  surface  of each  of che  f'.rtc  :hrt*
i.npinger* (and connecting tubing)  chrei separate cimea,  Use a in* 11 porzior.
of mechylene chloride for each  rlnje,  and  brush each surface co which che
simple  is exposed vleh e Teflon brlsele brush Co enjure  recovery  of fine
parciculate eMceer.   tf«cer will be required  for the recovery of che iapi-gers
In addition co che specified quantity  of aethylene chloride.  There will b«  a:
lease  evo phases  In che Lopingeri.   This cvo- phase aixcure does noc pour .ell
and  a  significant adount of  the implnger catch will be  left on che walls.  The
use  of  water as  a rinse aakes che  recovery quanciceclve .   (lake a  final  rir.ie
of each surface  and of che brush,  us Ing -both me thy lane  chloride and water

           3.5.7.2.1.4    After all nechylene chloride and  water washing and
particulats utter havej been collected in  the staple container, tighten :ha
lid  so  the solvenc, wat«r,  and DHPH reagent  will nee leak  out whan che
container  !• shlppad ce eh«  laboratory. Hark the height of Che fluid lava I  :±
da ca mine whacher leakage occurs during transport.  Seal che container  wL:h
Teflon cape.   Label the container clearly  co Identify its  concents.

           3.5.7.2.1.3    If che fine cvo Lapingers are to be analyzed
separately  co  cheek foe breakthrough,  separate  the contents and rinses  of :r.e
two  laplngers  into Individual containers.   Care oust be taken  to avoid
physical carryover fro« the first  inplnger co the second.   The foraaldehvda
                                      3- ITS
-------
•'alv« iecvaen cha wac-caic aec«r and ;ha  Lnlac of  cha aecaring  iyic«a.
-a'.cuiace :ht *varaga valua of che calibration faccor.   If  che  calibracion has
changed by sort che 5», recalibrate che aecar over che full rang* of orifice
s«"ir,gi, as ouclirvad in APTD-Q576,

          3.3.3.3,3 Leak check of aecoring lyieea:  The parcion of =Ha
sampling criin froa che puop Co cha orlfica aecer  («aa Flgurt 1) should b«
liak chackad prior co IniciiL uia and afcar aach ihtpaanc.  Laakaga *f:ar t-e
puntp will rasulc In Lais voluma baing racordad Chan !• actually saapiad. . '."SB
:ha following procadura:  Cloia cha main  valva on  cha aactr box.  Insar: a
on«-hola rubber icoppar wtch rubber cubing attachad Into  cha orLCica axhauj;
pipa.  Dticonnacc and vane cha Low itda of cha orlfica aano««car.  Clos* off
:ha low ilda ortflca cap.   Pranurtra ch« tyscaa co 13 -  18 c«  (5 • 7 in)
wacar coluan by blowing Lneo cha rubbar cubing.  Pinch off  eh«  cubing and
obiarva cha aanoaACar far I aln.   A Ion  of praiiura on ch« aanoaacar Lndi-
cacaa a laak In cha Mcar box.  Laak* avuc b« corracead.

SOIL:     It ch« dry-f«j-««e«r coefficient vtiuat  obtained before and af:er a
          caac ierle« differ by >5%,  elcher the caic aerlea BUJC be voided or
          calculeclonJ for ceic icriei onuc be performed using whichever aacer
          coefficlenc value (I.e., before or after) give* the Lower value of
          cocal saople voluoe,

          3,3.8.4   probe) He«cer:  The probe heactng lyteea a\«c be calibr*:e<3
before ic« inlelel ua« la che field eeeordlnf co the procedure outlined Ln
APTD-0376.  Probee cooflCrueced eeeordln|  co 4TO-03I1 need not be callbracad
if the callbreCion curwe in AfTB-0576 art uuied.
          3.1.1.9   Teaperacure gtuget:  Each  cher*ocoupla BUJC be penenancly
and uniquely aArkad on th« c**eing.  All B«eeuz7*ln-|lMi r«fcr«nce  cheraoat-
can avuc conform co ASTM I«l 63C or 63F ipeclfleaclonj.  Themoeouplea should
be calibraced Ln che laboratory wlch and wlchouc  Che me of e*conalon Leadt.
If excenslon leadJ are used  In che  field,  che  thermocouple reading*  ac cha
aablenc air ceaperacurei. wlch and  wlchouc  che  escenilon lead, auje  be nocad
                                     3-178
-------
1.5.3     CaiibratLan

          3,5.S.I    ?robe Hazzle;   Probe  nozzles  shall  be  calibrated  before
ir.eir L-izial use  in che field.  Using  a  aicromater, aeasure  the  iniida
liaaeier af ;he nozzle to the nearest 0.023 am  (O.OOL in),  *ake  n«*surtatr.:s
a: three separats  places across the diameter  and  obtain  the avteagi of the
T.easurtnanss.   Th» difference boc«««n ch« high  and  low  nuabtri  shall  no;
axcaad 0.I ma (0.004 in),  whtn ch« nozzlts btcoac nickad  or  corroded, :hev
shall b« rtplactd  and calibrac«d before us«.  Each noczlt  nusc  bt  p•mar.tr.:'.-.-
and uniquely  Ldincifitd

          3.5.8.2    PLcoc Tube:  The Type S picoc c-obe  aiaeobly shall be
calibrated according co ehe procedure outlined  in Section  (* of  EPA Method 2.
or assigned a noainal coefficlenc of 0.84 if  it is not  visibly  nicked or
corroded and  if tc meets design and intercoaponent  spacing specifications.

          3.5.8.3   Metering System

          3.5.8.3.1  Before tcs initial  use  in the field,  the  metering sys;t=
shall be calibrated  according to the procedure  outlined In AFTD-OS76.  :-.s:eii
of physically adjusting the dry-gas aeter dial  reading!  to correspond to :.-.e
wet-test netsr readings, calibration factors  «ay  be  used co correct :he gas
meter dial  readings  mathematically  co Che proper  values.   Before  calibrating
;he metering  systea. it is suggested chat a leak  cheek  be  conducted.  For
metering systesu having diaphragm putsps,  the  normal  leak check  procedure will
not detect  leakages  with the puap.  Foe these cases, the following leak check
procedure will apply:  BMSU a cen-«inute  calibration run at 0.0003? »V«in
(U.02 cim").   AC che  end of CM ran. C«M  ci»  M*ffsrsr^c sf ths  se£*u;ed "*?•
:*st and dry-gaj aacer voluaet and  divide the difference by  10  Co gee the lt*k
rate.  The  leak rate should noe exceed  0.00037  «V«in (0.02 cf»).

           3.5.1.3.2  Alter each field use.  check the  calibration of the
.uttering systeti by performing  three calibration run* ac a single  incermedia;t
orifice setting  (based on the previous  field  case).  Sac the  vacuua ac the
maxiaua value reached during the  tesc  series.  To adjust cha  vacuua,  insect  a
                                     3.177
-------
          3,3,9.1   Calculation of Total  Formaldahyda:   TO  deearmini  she  ra:
fonaVdahydo Ln nj. usa cha  £aI Lowing  aquation;

                                            ig/nola  aldahyda]
Total a; forsaldahyda - Ct x V x DF K             _..             x LOJ ag/Mg
                                        (g/mola  QNPH daeivacwa}
«har«:
          Cj - maasurad conctncracton of ONPH • £orn«id*hyd« dtrivaeivg,
          V  - organic «xcracc voluaa  •!
          DF - dilution faccot
          3.3.9.2   Foraaldchyd* eoneancraclan  Ln  *c*ek  (a*
                    ch«  foraaldahyd* cencvncraclon  In th«  *cack gas  uaing  :he
          following tquaclon;

          Ct - H [cocaL  f or»ald«hyd« ,  af]
               K  -33.31 fc'/>] l>f VM|U, Is •xpr*aaad In English unlcs
                  • 1.00 m* /mj If '.,.«, is ••pittitjd In MCTIC unici
               V,(IU)  - voluat of gas aaopL* « Maiurad by dry gas ««c«r,
               cocraccid to standard condlclooj,  4*ca  (daef)
          3,3.9.3   Avaraga Dry Ca« Haitar Ta«p«racura  and Avtraga Orifice
Prasiur* Drop ara obcalnad froaj eh* d«ca sh««c.
          3.394   Pry C«J Veluaa:  Ca\leul«ec  ?,(,u> «"4 mdjujt for leakage
If nactasary, ujlng eh« «quAClon  In Sceeioa 6.1 of If A Itoehod 3.
          3.5.f .5   VoluM of Uaear Vapor  and MoL*cura  Concant:   Calculata  c
       of v«e«r vapor uid •oljcuro concone froa ao>i«eionj  3-2  and 3-3  of  EPA
Nachod 9.
3.3. 10    P« canntmclafl of
To dAcanlno tha nlnlsua  saopla voluao  eo  bo  eollteeod,  uao  tho  following
i«qu«nca of aquations.

                                     3-180
-------
and recorded,  Correction  >i necessary  if  =ha  use  of  an  extension  lead
products a change >l.5l.

          3.5,8.5.1 Impingar and dry-gas mater  thermocouples :   Tor  the
ihtr-ccaup Its used to measure the  temperature  of  the  gag  leaving the  1-pir.itr
train. three -poir:t calibration a;  ice water, room  air, and boilir.g  va-tr
:imptricuris is n«ciis*ry.  Accept :h«  :hermocoupLe«  only if  ;he riadir.§s  a:
all ;hree ;«mp«ra:urts agrtt :o -2C  (3.S"F) wich  choit of Ch« *bioi.u:t '-'4'. ,e
of ihe rt£irtnc§ checmoaiecer ,

          3.5.3.5.2 Probt  and stack  chirmocaupl* :   for she chiraocaupl'ts  ,5ei
;a indicace  che probe and  scack ;emperaeuces.  a ehree-paine  calibra::or a:  .-_•.
wacer, boiling vaeer, and  hot oil  bach  :enpecacucei ause  be  perforaed   '.'si  :
a poinc ac room air :enperacure is recooaended.   The  checaonaeer and  chernio-
couple auie  agree co wichin  l,3i ac  each of the calibration  poincs.   A
calibracion  curve (equacion) nay be  constructed (calculated)  and the  daca
•xtrapolatad to cover che  entice ceaperature range sug|eiC*d by the manufac-
turer .

          3.5.8.6   Baroaacer:  Adjust  cha barooater  Initially  and  before  ea::
test  series  to agree to within ±2 . S  am  Hg  (0,1  in  Hg) of  the  aercury  baront:*:
or the correct barometric  pressure value reported  by  • nearby National V«a:.-~:
Service Station (saa* altitude above sea_ level).

          5.5. 8. 7   Trtple-beaa balance:   Calibrate the  trtple-beu balance
before each  ceat serial . ualng Clan S  standard weights,  till weights BUI; be
within ±0,31 of the standard*, or  the balance  auac be adjusted  to a*et these
Limits.
3.5.9
Carry out calculation!,  retaining  at  leaat  one  extra decimal  figure beyond
chat o£ the acquired data,  Round  off figures after  final  calculations.
                                     3-179
-------
          3.5,10.4  Tha following analytical datsccton Ualti and 3NPH
-apaci:y (band on a cocal valuaa Of 200 nl in cwo Lsplngan) mu«c alto ba
           in deCaraLning a vgLonc :o ba saaplad.
                  Coneral
          3.5.11-1  Saapling:  Saa EPA Manual 60QA-77-02b for M«:hod 5
quality control ,

          3.5.11-2  Analysis:  Tha quality anuranca prograa raquirad for ;his
nachod includai cha analyiii of cha flald and aachod blanks, proeadura
validations, and analyili of fiaid ipikai.  fha anaiimane of combustion da:a
and poiiciv* idanclf Lcacion and qoanclcacion of formaldahyda ara dapandanc an
;ha Lncajricy of cha laaplai racalvad and cha praclaLon and accuracy of  cha
analytical ••chodoLogy.  Quality aiaucanca procaduras for this saehod ara
daitgnad to aenicor ch« parfomanca of tha arulyelcal MChodoloiy and eo
provida tha raquirad Inform* don eo ealu corracclva acclon If problau ara
obiarvad In laboratory oparaelons or In flald iiaplinf acclvlclaa.
          3,5.11.2.1     Flald Blanks:  Flald blanks aust be subalccad wi;K
:ha aaaplas collactad at aach sampling lita.  Tha flald blanks Ineluda :ha
samp It bocclas containing allquoci of «a«pla 'racovary so 1 vanes ,  aachylana
chlortda and watar, and unusad ONPH raaganc.  AC a alnloua,  on* coaplact
sampling train will ba asaaoblad In cha flald staging araa,  takan co tha
saapllng ara. and laak-chaetud ac cha baglmxlnf and and of cha tasting (or for
:ha saaa total nuabar of elsMs as cha actual smcpliaf craln) .   Tha proba of
-ha blank, train uuat b« htatad during tha aaapla cast.  The train will ba
racovarad aj  if It war* 4n actual case saopla.  No guaous saa^la will ba
panad through tha blank sampling train.

          3.9.11.2,2     HaChod Blanks;  A Bached blank oust b* praparad for
aach fat of analytical oparaelons. co avaluata concaalnaclon and arclfacci
:hat can ba darlvad froa glasiwara, raagants , and laopla handling In tha
laboratory.
                                     3-192
-------
          3.5.10,1.   Froo  pri-or  analysti  of :he waitt ft«d, she cor.cen;ra;;-r.
of formaldehyde  (FORM)  introduced  into che combustion syicen can be calcula: •
ed   The degree  of destruction  and raraoval ifficiancy chat if required .3 usec
:o dererair.e :he amount of  FORM allowed  to be preienc in she ef fluer.:.  TV.is
a.r.our,: lay ba «xpreaiid AS:

          Max FORM ««§s - ;  (-T)  (FORM cone)  (100 -  iDRE) :  /'.OO
          where:
                • 7 -       aasi  flow race  of viice feed per h,  g/h (lb/>.)
                FORM  -     cor,cencr*cion of FORM (we %) Lncroductd in:a  :r.«
                          conbuicion process
                ORE -     percent  Destruction and Removal Efficiency required
          Max FORM -     tnais  flow race  (g/h [lb/])  of FORM emicced froa :.-«
                          combuiclon icurces

          3 . 5 10 . 2   The average discharge concencracLon ot che FORM in :he
affluenc gas Is  determined  by  conparing che Max FORM with :he voluoecric flaw
race being exhausted froa che  source.   Voluaecrlc flow rate data are  avaiLab.;
is a result of  preliminary  EPA  Mechod I  • & determinations;
                !tax FORM cone - [Max FORM Mas a] / OVC(CC|U)
          where:
                D'»ifciui • volumetric flow race of exhauie ga« ,  dsca (dscf)
                FORM  cone  -    anticipated concentration of Che FORM in :he
                               exhaust gee streaa. g/dscm  (Ib/dscf)

          3 5.1.0.3   la BAklng  this calculation, le Li recoiaended chat a
safety aargln of «c  lease ten  be Included.
                                         eonc  ' ?«toi
           where:
                         detectable aaount of FORK In ancire saapllng train
                          alnloua dry standard volume to be collected at dry.
                          gas aeter
                                      M31
-------
                               table  3.5-3
                 EXPECTED  METHOD  PERFORMANCE  FOR  FORMALDEHYDE
           ?arta«c«r        Precision1   Aceurtcy*    D«c«ccion Limit3

     JUcrix:  DvuiL  crtlni    ±151 RPD      ±201       1,5 * LO"  Ib/f;3
                                                         (L.S ppbv)
                  dl£f«rtnc«  ILalc  for  du*i
zLLaic  for  fi*ld »ptk«  r«eov«rl»i.
3Th«  Lov«r  r«p«rtln| llaic having !•••  chui  Li  probabiltey of fkls«
dtcoeelon.
-------
          3.5.11.2.3     Field Spike:  A field spike is perforaed by :-;:3i,c
ing 200 *L of the Field Spike Standard ir.:o an iapir.ger containing 2CO .?.; :f
;N?H solution.  Scandard iapir.ger recovery procedures are followed and :r,«
spike is used as a check on field handling and recovery procedures,  an
aliquot of the field spike scandard  is retained in the laboratory far ieriva-
tization a~d casparative analysis.
3.5.12    Meehod Performance

          3. S, 12,1  Hechod performance evaluation:  The enpecced aechod
perforaance paranecers  for precision, accuracy, and dececsion liaiis are
provided in Table 3.5-3,

            Addition of a Filler ca che Forma Idthyde  SaapLing train
              I
At a check on cha survival of parciculaca aacertal through  che  iopinger
system, a filter can be  added co  che  impinger  train etcher  after the second
impinger or after the  third  iopingcr.  Since the  iapingers  are  in  an ice ba
there  ia no reason  to  heac che  filcer ac  chls  point.

Any suicable  medium (e.g., paper,  organic mentor ane) nay be  used for the f:.:
if the aacerial  conforms to  che  following specifications;
                                         «
1)        the filter has ac  lease 93% collection  efficiency (<3l pane era dor.
          for 3  urn  dloccyl phchalace  sooka  parttclei.  The  filter  efficiency
          test shall be conducted In  accordance) with  ASTM  scandard method
          02986-71.  IMC data  fron the  supplier's quality  control prograa
          sufficienc  sot chii
 2)         the filter has a low aldehyde blank velua (<0.013 mg foraaldeh-
           yda/cii2  of filter  area).   Before  the  case sertar.  daceraine  the
           averag«  for»«Uahyd« blank vilm  of at leaat three fileari (fraa  the
           loc to be uaed for sampling)  using the applicable analytical
           procedures.
                                      3-113
-------
                   far ^dahvdai *nd Keeonet fry  Mjgh
                         i"H?LC)  'Method
2 . S - 1     Seooe ar.d ApalieasLon

          ] 6,1,1   .".achod OOilA cov»rs  Chi determination of  free  foraaliehvie
Ln :hi aqueous samples and Uachacn and d«rLv«d  *ld«hyd«i/k«:or.«» co'.*.tc:ad
bv M«;hod 00 II.
          Compound Sam«            CAS So •

          Form*id«hyd«             50-00-0
          Ac«:ald«hyd«             73-07-0

          *    Chtaical Abicracc S«cvie*s Ragiiery Nuab«r

          3.6.L.2   Mtchod OOILA is • hifh p*rforaane«  liquid chromacogrjpr..;
(HPLC) a«chod opcimirtd for eh« daCinainacion of  fam*Ld«hyd« and tcica.ie-  :e
in aqu*ous «nvi.rona«ncal oucrlcti and l«achac«i of loUd iaapl«j and szack
samplti colltctid by Machod 0011.  ^"htn Chia aachod  La  uitd  co analyza
•-nfaailiar laapla .nacrict*. coapound idancificaclon  should b« supported by  a:
Lease oni additional qualicaciv* cachniqua.  A gas chronacograph/naii sp«c-
;roaacar (GC/MS) nay b« usad for eha qoalLcaclva  confirmacton of raiulci  :r:-
:ha cargac anaLycat, using cha axcracc pcoducad by ehis •«ehod.

          3.6.1.3   Tha Mehod dacaccion  LiaLcj (HDL) art liittd in TabUi
3.6-1 and 3.6-2.  That HDL tot • ipaciftc  taapla uy  dtffar from that Uicad,
depending upon eh* nscura of tncarfaraneaa  in eh* ia«pla nacrlx and eh* aaour:
of 5aapla us*d In eh* procadur*.

          3.6.1.4   Tha axer«,ceion procadura foe  solid  saaplas  Ls slailar :a
chac spacifiad in Machod 1311 (1),  thus, a singla sasrpl* nay b« excracted  ::
naaaura cha analycas includad .in eha seep*  of oehar  appropriate aaeheds.   The
analyse Is allowed cha flexibility co lelecc chronacographic condicUni
                                     3-IS6
-------
Racovar =h« axpond  filter  inco  a  laparaci claan container *"d racurn ;-a
consainar .ovar  lea co  cha  iaboracary  for analysii.   If cnt filcar Li b«i-i
a.-.a^vied for foraaldahydt,  :ht  fil:ar may ba raeoverad inco a concainar o:
::;?H reagenc for shipaant back  co  :ha laboratory.   If cha ftl:ar '.»  baing
«xaa'.r.ed far :ha prasanca of  parziculaca aacariaL,  :ha fj,L:«r say b«
."a a clean dry csncainar  ind  racurnad co :ha laboracorv,
                                       3-185
-------
aopropriace for ;he simultaneous measurement of  eoncaalnations of  :h
                                                                    est
          I 5,1,3   ThU siechod it restricted co use by, or under :he super.-. •
sion of ar.alyics experienced tn the uje of chronatography and  In cha  Lncar?:*-
:acion of chromacograaa.  Each analyst oujc demonstrate ch« ability :a
generate acceptable results vtth this method,

          3.6.1.6   The coxlcLey or carcinoganielcy of aach raagant usad  .n
:hi* aachod ha* noc baan practsaLy daflnad: hov«v«c, aaeh chtalcal compound
should ba craaead as a pottncial health hazard.  Froa ehla viawpoLnc, expos..-;
•-Q zhasa chamicals ousc ba raducad co cha lowasc poisibla lav«l by vhacavar
-eans avaiLabla.  Th« Laboracocy is rasponiibla Cor aalncaLning a curranc
awiranasi fila of OSHA rafulations rajardlng ch« *afa handHnj of cha chaai-
cals ipaciflad In chls nachod   A rafcranca flic of aacarLal safaey daca
shatcs should also bat a«4a available co all personnel lnvolv«d Ln cha chaoical
anaiyiii.  Ad4Lctena\L rafarancas to laboratory safacy ara avatlabla
          3.6.1.7   ForaaLdahyda has b««n  eaneaelvaly elasilftad as a kr.owr
suipaccad, human or aajmalLan carelno|«n.
352     s ufflaarv a t Machad

          3.6.2.1   Environmental Liquid* and Solid Uaehatas
          3.6.2.1.1 For vutas comprised of solid* or for aqueotu va*cas
concalnlnf •Ifjniftecnc ameunea of solid aacarlal, eho aqviaou* phaia,  If any.
.1 iaparac«d from      tolld pha\a« and •cored  for  later  analysis.  If  neces-
sary, the particle slxo of the solid* In the  wa*te Is reduced.  The solid
phase La eitraeced with an amount of extraction fluid equal  co  20 times cha
weight of the solid phase of  the waste.  A special extractor vessel is usad
whan casting for volatile*.   Following extraction, the  aqueous  extract it
separated from the solid phase by filtration  employing  0.6 co 0.8 MS  glass
fLbar filters.
                                     3-iaa
-------
                                Table  3.6-1

              H:CH  PERFGR.IANC£  I::L-:D CHRCMATDCRAPHY COND:T::N'S
                       METHOD SETECTIOS LIMITS CSINC SOLI3
                              SOU EOT EXTRACTION
                                           ia«
H?LC condi:ion>:   R«v«n« ph»t« CIS column.  4,6  x 230  am:  Liacriclc  •'..
using a«ch«nel/w«t«r (73:23,  v/v);  flow ctct L 0 nL/min.:  d«c«ecor  160

• Af:«r corriesion for Laboratory  blank.
                                Table 3.6-2

               HIGH  PERFORMANCE  LIQUID CKROHATOCRAfHY CQKOITIONS
                      METHOD  DETECTION LIMITS USING HETHYUNE
                             CHLORIDE EXTlACTION
                                Rtctnelon Tla«                 MHL
                                      7,1-                         7,2

                                      S.6                      171*
HPLC condition!:  livtri* ph«J« C1I eoluan. <»-4 i 230 ••;  UocracLe  •Luzi
u«in; ••chAnal/vaear (79:2S. v/v): Clew r*C« L.O «L/«tn ;  d*c«ccoc 360  na.
   Th«t« valutj Lnelud* r«af*ne bl*nk cone*ncr*clenj of 4pproxia*ctly 1
   forMld«hyd« «n4 130 wg/L aetealdchyd*.
                                     3-187
-------
:has« aacatialf »ujc b* toucinaly damonssracad co ba  Craa froa  ineacftser,cts
-ndar :ha conditions of :ha analysis lay analysing laboratory raaganc blanks

          3,6.3.1.1 Glassvara ausc ba scrupulously claanad.  Claan all
giasiwart ai soon is posslbla afcar usa by rinsing vich cha Use solvmc ustd
This should b« failow»d by dacargtnc wathing «ich hoc wacar. and rinsai vt:h
rap wacar and diseiiltd wacar.  Ic should Chan b* drainad, drlad, and h«i:«i
in a laboracory ov«n ae 130'C for sav«cai hours bafora us a.  SoLvanc r-.r.sei
with aachanol nay ba subitteuead for tha ov«n haacing.  Aftar drying and
cooling, giassvara should ba scorad In a claan anvlronaanc co pravane any
accuauLaeton of duac or ochar eoncaatnanti.

          3.6.3.1.2 Tha usa of high pur Ley raaganci and solvancs halps -a
ninlslza Incarfaranca problaaa.  Purification of solvancs by dlidllaclort  in
all-glass syicasa *ay ba raqulrad,

          3,6.3.2   Analyst* far fomaldahyda Is aapaclally coapllcacad by  L:s
ubiquitous occurranea in cha anvlronaanc.

          3,6.3,3   Matrix Incarfarancas a«y ba causad by eeneaalnancs chac
ara coaxtractad froa cha saapla   Tha axcanc of »acrix Incarfarances will v«:y
consldarably froa sourca eo sourea. dapandinj upon cha nacura and divarsUy o:
:ha matrix balng saaplad.  No Inearfarancaa hava baan obsarvad  In cha aacrlcas
siudlad as a rasulc of using solid sorbanc axcraceion aa opposad eo liquid
axcracclon.  If incarfarancaa occur in subsaquanc saaplas, soaa addlelonal
claanup aay ba nacaasajry.

          3.1.3.4   Tha axtanc of incarfarancaa thac stay ba aneouncarad using
liquid chro«aeographle cachniquaa has nee baan fully  aaaaaaad.  Although cha
HPLC condiciona dascribad alien for a rasolucion of cha apacific compounds
covarad by chis aachod, ochar aacrlx coaponanes aay incarfara.

3.6.4     Aaaaracujand Maeariala

          3.6.4.1   Raacclon v«s»»L  • 220 al  Floranca flask,
                                     3-190
-------
             -2,1,2 If conpACiblt  (i.t,, aulsipU  phases vLll noe  fora or,
              'he initial aqutous  phase o£  :he wait*  it added co cht aqutous
extract, and these liquids art analyzed zageshtr.   if  incompatible, cht
'.iquida art ar.aiy*td stparactly and  the rtsul;i an aachoaaeically coablr.td
yield a vo~kvae -oighctd aviragt concincraclan.

          3 5 2.L.] A ataiurtd voluat of aquaoui j*npl« or an ippropr'.ite
a.T.oun: of solids i«ach4C« is buffartd co pH 5 and  dtrivaclztd wi;h 2,--
iir.i;roph«nylhydr*ztn« (DNFH) ,  using tichtr cht solid  sorbtne or she atsr.v'.sr
i«rivacizacion/txtraccion opcion.  If cht soLid »orb«ne option i* ustd. :r.e
derivacivt is txcraestd using solid  iorb«nc c*rcridjt«, followtd by •lusiar,
vi;h achanol.  If :ht ntchyltnt chloridt opcion is uitd, :ht dtriv«civt is
sx:racctd wi:h ntchyltnt chioridt.   The atchyUnt  chloride txtrac:i art
=onctncr*t*d using cht Kudtrna-Danish (K-D) procedure  and iolvtnc txehangaii
i-to atchanoi prior co HPLC analysis   Liquid chroajcographic conditions art
describtd which ptraic cht itparacion and ataiurtmtnc  of foraaldthydt  in :h«
extract by absocbanct dtctecion ac 360 na.

          3-6.2,2   Scack Cas SaapUs Colltcctd by Mtchod 0011

          3.6.2.2.1 The tncirt saaplt recurned to  tht  laboratory is txccac:e
with oechylene chloride and the aaehylene chloride titrate is brought up :o A
-------
          3.6.4.8.5 Scrip-chari recorder compatible «ich decectoc  • r.'se of A
ia:a sysrea foe aeasurir.g ?**"* areas and ricaneion cisies ii r«coma«nd«d

          3,6.4.9   :ian fiber filler paper.

          3-6,4.10  Solid lorbenc cartridges  • Picked wlch 500 ng C13 (3akar
or aquivaitnc).

          3.6.&.11  Vacuua manifold • Capabl* of siouLtantoua txcractior. ::
= 3 12 safflpL«i (Sup«lco or
          3,6.4.12  SanpU rtsir/oiri • 60 al capacUy (Sup«lco or
Une) .

          3.1, 4. 13  PLp*e • C*p«bi« of 4ccur»c«ly d«Uv«rin| 0.10 ml lelucion
(Piptcaan or
          3.6.4.14  Vactc bach • Htaead, wieh ceneanerie ring cov«r, capab'.t
of c«Bp«rttur« eoncrol ((±) 2*C).  Th« b»eh should b« ui«d und*r • hood,

          3.6.4.13  VoLua«cric rUiki - 2SO or 500 al .
3.6.5
          3,6,3.1   RaagiRC grad* ehtaleali shall b« ua*4 in all
       oeharvlia LndLcac«d. It L» Incindad thac all rsaganea shall conform :a
:h« ipicifleaelon* of cha Co«iicc*« on Analytical Raagtncs of cha Aaarlcan
Chaaical Soelarjr, vtiara tueh «p«eiftc*eiona are availabla.  Other gradai aay
=• mid. provtdad ic is first aac«reaLna4 ehae eha reaganc la of sufficiently
high puricy ea peraic lea uaa vichouc Lessening ctia accuracy of che dectrmir.a-
:ian.

          3.6.3,2   Organic -free wacer • All  references  co waeer in ehii
nechod refer co organic -free reagenc vaear, as defined In Chapter 1 SU-846,
                                     3-192
-------
          J.6-4.2   Separacory funnel  •  205 si. vi:h Teflon s;opeock
          3,6.4.3   Kuderna-Oanish  'K-0) apparatus.
          J.6.4.3.L Concentrator :ube  •  10 al graduated (Konces K- 5TC050 • '.:Z:
:r equivalent)   A ground glass stopper  is used :o priv«nC evaporation of
extrac :s -
          3,5.4-3.2 £v«p0racion flask  •  500  al (Koncii K-57COOL -:G-" sr
equiv«L«nc) .   Accaeh co conctrrrator cub« wich springs, clamps, or equivalent
          3.5.i«. 3. 3 Snyd«r col'^an   • Thr«« ball a*cro  (Kanci* K- 503000 -Ci: 1 ;
          3,6,4,].<* Snydar coluan  - Two ball nacra (Koncis 1C- 56900L-.021? 7:
equivalenc) ,
          3.6.4 3.5 Springs • 1/2 inch  (Konctf K-662T50 or «quiv*l«nc).

          3.6.4.4   VLali • 10. 25 al,  glass wich Teflon lined screw caps or
crisp cops.

          3.6.4.3   Belling ships - Selv«nc extracted wich nechylen« chloride
approxio«cely 10/40 »«sh  (silicon carbid* or •quLvalmc) .

          3,6.4.6   Btltne* • An«lycieal. capable of accurately weighing to
the nearest 0.0001 g.

          3,6.4.7   pH a«cer  • Capable  of measuring to chi ntartsc 0.01 units

          3.6.4.S   High  performance  liquid chroaacograph  (modular)

          3.6.4.1.1 PiapLni •yteeoi  •  Isocracic, wtch conaeanc tlpv concral
capable of 1.00 •l/rnin.

          3.6.4.1.2 High  pCMaure  injection valv* wich 20  i*L  loop,

          3.6,4,8.3 Coluan  -  230 am x 4.6 aa  ID.  3 uA parclcl* size, C18 (or
•quivalenc) .

           3.6,4.1.4 Abaorbanca  decteeor •  360 na.
                                      3-191
-------
-sing O.L H HCl.   The formaldehyde conc«ncr*cion is calculated using :!r.e
fallowing equation;

:oncanira=ion (sg/al) - 30.03 x (N HCl) x (si HCl)  23.0
          where :
          N HCl • Mortality of HCL solution usad
          ml HCl - ol of standardized HCl solution usad
          10-03 - !« of formaldahyda

          3. S. 5. 14. 2 Stock formaldahyda and acaealdahyde •  Prepare by adding
ZS5 uL formalin and 0.1 g acataldahyda co 90 al of wacar and dtluca co 100  .-ol
Tha concancracton of acacaldahyd* in chi« »olutlon Ls I. 00  ng/ml .   CilcuLa:*
:ha coneaneracion of fornaldahyda in this lolutton u*tng cha rasulci of :ha
      parformad Ln Sacclon 3.6.5.14.1.1.
          3. 6. 3. 14. 3 Scock standard solution* BU>C b« rapUcad afcac six
montha ,  or soonar, if covparlson with ehack standard! Lndicatti « problta.

          3.6.1.13  Raaceton Solutions

          3. 6. 5. 13. 1 ONPH (1.00 vg/L) • DissoUa 142.9 d| of 701 (w/v)  raigsn:
                                            *
Ln 100 ol absoluta «thanol.  Slight ht«cln| or sonicatlon ««y b« naeassary  ;a
affact dtaaolueton.
          3 6.5.13.2 Actuca buffer (3 N)  Praptr* by lUucraHsing
acatle acid to pH 3 with S S M«OH lelutlon.  Dilute co standard veluoM with
wacar.

          3.6.9.13.3 Sodiia chlorld* iclutUn (t«curae«4)  Prtpara by nixing
at cha raagtnc frada solid with w«tar.

3.6.6          Saaala Callaeclon. Prasarvarlon. infl HMdllPl

          3.6.6.1   Saa th« Ineroduceory aaetrlal to this Chjptar, Organic
Analytts, SaecLon 4.1 of SW-146.
-------
          3.6.5.3   -echylsr-.a cr.Larida. CH,Ci,  •  HPLC  grada  or

          3.6,5.t   MathanoL, CHjOH  •  HPLC grad* or iquiv»l«nc.

          3.5.5.3   EshanoL (4biolu = i), CHjCHjOH  -  HPLC  grida or
          3.6.5.6   2 , *'Dtni;rophtnylhydrizin« (DNPH) (70% (•/•"))
                 in  organic-fret  naganc  vacar.
          3.6.5.7   Fonnaiin (37,6 pareonc («/«)), fora*ld«hvd« in organ.;; -
     r«ag«nc w«c«r,

          3.6,5.8   Acccic acid (glacial). CH,C02H.

          3.6.5,9   Sodl.ua hydroxide lolucioni S«OH, L . 0 N and 5 N ,

          3.6.3.10  Sodiufl chlorlda. S«Cl.

          3,6.5.11  Sodiufl sulflc* lolucion, Nt,SO,,  0.1  N.

          3.6.5.12  Hydrochloric Acid, HC1, O.I N.

          3.6.5.13  EKCTMCLon fluid • Olluc* 64.3 «1 of 1.0 N NtOH end 57  -
glacitl Acacie icid eo 900 al vlch or|tntc-frt« r««f*ne wacar.  Dlluca to :
li:«r vlch organic -fraa rt*|ane wacar.  Th« pH should ba 4.93 ± 0,02.

          3.6.3.14  Stock aundtrd lolucloiu

          3,6.3.14.1 Stock formtldahyda  (approilaaealy 1.00 «|/«1)  - Prepare
by  diluting 243 itl formal In co 100 al vlch organic -fra« raaganc vacar.
           3.6.5.14.1.1    Scandardizaeton of fora*ld»hyd«  tceck  solution  •
Tranafac a 25 al  aliquot  of  a 0.1 N Na,SO, loluclon eo a boakar and racord -,-t
pH.  Add a 23.0 al  aliquot of tho fonaldahyda  itock tolutlon (Sactlon
3.6.3.14.1)  and racord  tha pH,   Tltraca  chii alxtura back to tha  original  pH
                                     3-193
-------
for IS hours-   Fil:«r the axcracc =hrsugh gU*1  --^er paper  and  scar*  ir.
sealed bac:1.»» a!: -*C.  Each su of txcracs reprtsencs 0.010  3  solid,

          3.6.7.2   Cleanup «nd Separation

          15,7.2.1 Cleanup procedures nay roc be necessary  far  a  rela: !•/•:•/
clean sample oacrix.  tha cltanup procidurti rtcorara«r.d«d  Ln  chis mathod have
b««n used for the »naly§i.s of various sample :yp«j,  if parcicuLar c-.r:_--
s:ar.cta dtmand :h« usa of an al:trn«civt clsanup proctdur«,  chi  analys; ~-s:
d«c«min« :ht elucion profile and danonacract chac :ht rtcov«ry  of farmal.e-
hyd« is no loss chan 351 of recoveries specified Ln Table  3,6-3.   Recovery -i
be lower for samples which fora enuisionx.

          3.1.7.2.2 If che sadple la noc clean,  or che coapLexicy  is unknown,
:he entire sample should be cencrifuged ae 2500  rpa for 10 ninucei   Deeane
che supernacanc Liquid Iron che centrifuge boccle, and filcer  chrough  gLaas
fiber filcer paper  ineo a coneainer which can be cighcly  tenled.

          3.6.7.3   Deriv»ciz*clon

          36.7,3.1 For aqueous saaples. measure a 30 co  100 al  aLiquoc o: :.-
sanple.  Quancicartvely cranafer che sample aliquoc co che ceaccion vessel
(Section 3.6.4.L).

          3,6.7.3,2 For solid laaplei, I co 10 ml of le*ch»ce  (Seccion
36.7.1) will ujoally bei required,  the aaounc uued for e  particular saapla
oiuie be decerained  through preliainmry experiaenc*.
                                     3-196
-------
          3.6-6.2   Envitonn«nc»L  liquid  and  Leachate  imp In muac  be  :e:::-.
eracid ac ^*C, and oust be d«ri.vastztd  ytchin 5  dayi of  laapLa  eollec:;:n  ir.i
         vichin 3 days of dsr;v«cization.
          3 §.6.3   Stack gas saaples collected by  Method 0011  aus:  be
refrigerated ac 4"C.   It is recommended  chat  ia«pUi b« »x:rac:«d vi;r,i-  30
days of eoLltccion and :h*c «xcraccs b«  analyzad wichin 30 days  exsracziar,

3.6.7     Procidurt

          1.6.7.1   Extraction of Solid  Saaplai

          3.6,7.1.1 ALL 10 Lid saapLts should  b« homogintous   '."h«n -he  sasp'.«
is noc dry, diciraina  eh* dry vaighc of  ch« saispla. using a  r*prastneaeiv«
aLiquoC-

          3.6.7.1.1.1  D«ctrnin«eion of  dry w«ifhe  •  In c*re*in cas«s.  saapLt
reiuLcs ar« d«sir«d ba»«d on a dry  w«ighe  basis.  Uh«n such  daca It  das i red.
at r«quin
-------
Sota:     Tot all reactions, 'ht local voluoa of :he aqueous  layer should :«
          adjusted =o IQO al «i:h water

          35*33 Derivacizacion and entraction of che derivative can be
accomplished using :ha solid sorbanc (Section 3,6.7.3.4) or nathylene chloride
spzion (Saccion 3.6.7.3.3)-

          3.6.7.3.4 Solid Sorbanc Option

          3.6,7.3.4.1    Add 4 n l of acetate buffer and adjusc cha pH to 5.: ;
0.1 wi;h glacial acaclc acid oc 5 N SiJH   Add 6 al of DNPH :aaganc,  jaal :r.e
:an:air.ar, and place on a wrisc-accior. ihaker for 30 ainutai.

          3.6.7.3,4.2    AataabLa cha vaeuua «*nifold and connect :o a wacer
aspirator or vacuvui puop.  Ajaaabla solid sorbanc cartridges  containing a
reinioua of 1.5 g of CIS sorbanc, ujlnf connectors supplied by the aanufaccur-
oc. and attach eha sorbant train to th« vacuua manifold.  Condition aach
cartridge by passing 10 al diluta aeatata buffar (10 mi 3 N acataca buffer
dissolved in 230 al water) through cha sorbent cartridge train.

          3.6.7.3.4.3    Reaove the reaction vassal froa cha  shaker and add L*
-il saturated SaCl solution to eh* vessel.

          3.6.7.3.4.4    Add cht reaction solution to th« sorbent train and
apply a vacuua so chae eh« solution is drawn through th« cartridges at a ra:a
of 3 to 5 al/aln.  Rtlajua th« vaeuua after the solution ha*  passed through
;he sorbent.

          3.6.7.3.4.9    Clue* each cartridge eraln wlch appro*laately 9 al o:
absolute ethanol. directly Into a 10 al voluaacrlc flaak.  Dilute the solution
=o voLuaa with absolute eehanol, alxed thoroughly, and place  in a tightly
sealed vial until analyzed,
                                    3-L99
-------
                .ablt 3.6-3
    s:sci£ CPESUTCR ACC.TUCY A.SD PRECIS ::N
        USING SOLID SOJULST EXTRACTION

**cru
Muly=i Typt
Av«r«g« Se*nd*rd Spike N"'_-bir
Ptretne ^tviAcUn R*ng« 3f
Rteovtry ?«rc«ne -wi/L) Ar.il-.-m
Rsagtne
Final
Effluent

Phanol
form*U«hy(l*
Slu4ft	
96
                   90
                   93
9 i.
           '.1.0
           12.0
                                       LS-l'.lO
        ,6 8-li.lO
-------
          3-6.7.:, 5,5.1  Following K-3 concentration of -j,« mechylsne chlorite
ex.rac: :o < 10 nl using the aacrs Snyder column, allow che apparatus co cool
and drain foe at lease 10 minutes.

          ].S " ' " 5.2  Momencarily rtaove che Snyder column, add 5 al af :;-e
:?.s:hanol. a -:       . oed, or bailing chip, and accach che micro Snyd«r
column.  Concenerace che excracc using 1 al of a«ch*nol co prtwcc :he Sr./iar
coluan.  Plact ch« K-D apparacui on ch« w»c«r b*ch 10 thac th« concAncracor
:ub« ii partially Immersed in ch« hoc wac«r,  Adjuic ch» vertical pojtv.on of
:K« apparacui and che vacer teoperacure, as required. Co complece concar.:za-
::on.   At the proper -:   of dlsclilacLon the belli of che column will
actively chatter.        : chambers will noc flood.  When che  apparent voluise
of liquid reacr       ... remove the K-D apparatus and allow  le co drain and
cool for *c lease .J mlnucee.

          3.6.7.3,3.3.3  Remove che Snyder column and rinse che flask and  Lcs
lower Joint with 1-2 ml of aechanol and ad4 co concentracor cube.  A 3-ml
syringe Is recommended for this operation.  Adjust the extract volume to '.3
ml.  Stopper che concentrator cube and store refrigerated at  <**C If further
processing will not be performed Immediately,  If the extract will be scorid
longer than eve days, it should be cransferred co a vial with • Teflon- Lir.ed
screw cap or crimp cop.   Proceed with liquid chromacographle  analysis if
further cleanup is not required.

          3.6.7.4   btrMtlon of Stack G«« Saxplei Collected by Method 0011

          3.4.7.4,1 itaASJuze the aqueous volume of the sample  prior to extrac-
tion (for moIscure determination in case che volume was noc measured in che
field).  Pour ch« sample into a separacory  funnel and drain che mechyUne
chloride into e volumetric flask.

          3.6.7.4.2 Extract the aqueous solution with two or  three aliquot* of
machylene chloride.  Add the methylene chloride extracts Co che volumetric
flask.
                                    3-200
-------
          3.S.7.J.5 Macnylana Chi a ci da Ope ion

          3 5.7.3,5.1    Add 5 a of icacaca buffer and adjuie  :he pH :o 5 ] -
:.: -••.:;- slacial acacic acid or 5 S SaOH.  Add  10 mi of DSPH  reagen:, s«a. :r.a
rar.cair.ar.  and place on a vrisc-acsion shakar for 1 hour,

          3.6,7.3.5.2    Excracc =ha solucion wi;h chraa 20 ol portions of
,?,«-hylana chlorida, using a 250 al saparacory funnal, and eoabina cha aczi-.y
Lena chiorlda Layars.  If an taulflion forai upon axcraecton.  removi-hhii en:..-?
emulsion and cincrifuga ac, 2000 rpa far  LO alnucaa,  Saparaca  cha layars ir,;
procaad  wich :ha naxc axcraccion,

          1.6,7.3.5.3    AjtanbLa * Kudarn*-DanUh (K-D) coneancracor by
ac;achlng a 10 ml eoneancracer cub* ca a  500 al aviporacor  flaik.  Uath cha K-
0 apparatus with 23 al of axcraccion solv«nc co coaplaca cha  qutncicaclva
:ransfar .

          3.6,7.3.3.4    Add ona co cue  claan boiling chipa co cha avtpora:. ?
flask and accach a chraa ball Snydar coluan.  Praaac cha Snydar coluon by
adding aboue L al aachyiana ehlorid* co  cha cop,  Placa cha K-0 apparacuj on a
hoc w«ctr bach (80-90'C) so chac cha concancracor Cuba U ptrctalLy  Laaariad
Ln cha ho: wacar and eha anctra lovar raundad surf act of cha  Claak is bathad
wtch hoe v«por.  Adjuic cha varcieal poaicion of tha apparacuj and cha w*c»r
:aop«racur«, at raquirad, Co coaplaca eha concancracioo in  10-13 ain.  AC :r.e
propar raca of dtietllatlon eha balls of eha coluan will aecivily ehaccar, bu:
of liquid raaehaa  10 al,  raaovi  cha  K-0  apparaeua  and  allow  ic  co drain  and
cool foe a laaae 10 ain.

          3.6,7.3.9.3     Prior  co  liquid chroaaeographU  analysis,  cha solv«r:
T.USC ba axehangad  co aaehanol.   Tha  analyse ouae ansura quaneieaeiva  cram far
of cha axcracc  eoncancraca.   Thai axchanga is parfonwd as follows:
                                     3-199
-------
          3.6.7 5.1.1,2  Process each calibration standard solution through
:~.e derivat;zaeion op:-.on used for sample processing (Section 3.6.7,3.^ or
3,5.7.3.5)

          3.6.7,6.1.2    External standard calibration procedure

          3.6.7.6.1.2.1  Analyst each darivacizad calibration standard usir.g
the chronatographic conditions listed In Tablet 3.6-1 and 3.6-2, and tabulate
peak area against concentration injected.  The ritults may be used to prepare
calibration curias for formaldehyde and acetaldehyde,

          3.6.7,6.1.2.2  The working calibration curve aust be verified on
each working day by the meaaursenenc of on* or more calibration standards   If
the response for any analyte varies from the previously established responses
by more the 10%. the teac oust be repeated using a fresh calibration standard
after U is veriflid that the analytical syitea ii In control.  Alternatively,
t new calibration curve may bo prepared for that coopound.  If an autoiuipltr
is available, it is convenient to prepare a calibration curve dally by
analyzing standard* along with teat auplea.

          3.6-7.7   AnaLyili

          3.6.7.7,1 Analyze •aaplea by HPLC, uilng condlciona ettabiished in
Section 3-67.6.1. Tabl*« 3.6-1 and 1.6-2 Lilt the retention tiaes and NOLj
that were obtained under cheee conditions.  Other HPLC coluanj. chroaatogrtph•
ic conditions, or detectors may be used if the requirement! for Section
3.6,8.1 are Mt. or if the data are within the lialti described In Tablet
3.6-1 and 3.6-2.

          3.6.7.7,2 The width ef the retention eiae window used to uke
identifications should be based upon MasureoMnts of actual retention cine
variation! of standard! over the course of a day.  Three tlaiea  the standard
deviation of a retention time for a compound can be used to calculate a
suggested window sice; however, the experience of the analyst should weigh
heavily in the  interpretation of the chronacograas.

                                    3-202
-------
          3.6.7,4.3 Fill chi voluaecrtc  flaik  to  ehe line wich mtchyler.e
chioridt.  Mix wtll and rtmovt an allquoc,

          3.6.7,4.4 if high levels of formaldehyde art prtsenc. che excrac;
can be diluted vi;h mob Lie phase, ochervist cht txcracc ousc bt solven:
exchangtd as describtd in Seccion 3,6.7.3,3.3.  If low Itvels of faraa'.iehyde
are prestnc, che sanplt should be concencraced during che solvenc exchange
procedure.

          3.6.7.5   Chrooacographlc Condi.clone

Column1             CIS, 250 mm x 4,6 nun ID, 5 ua particle sizt
Mobile Pnait:       mtchanol/wactr, 75:25  (v/v),  isocracic
Flow Ract:           1.0 nl/mln
UV Dtceccor:        360 na
Injtccion Voluat:   20 itl

          3.6.7,6   Calibracion

          3.6.7.6.1 Escablith liquid chronacographic optracing parameters  :o
product  a rtctncion clot tquivaltnc co  chac indlcaced In Table 3.6*1 for  :he
solid  sorbenc opciona, or in Tablt 3.6-2 for aechylene chioridt option.
Suggtictd chromacographlc condlciona art provldtd in Stecion 3.6.7.3.  Prepare
dtrivaclztd caltbracion tcandardj according co cht proctdurt In Steclon
3,6.7.6.1.1.  CalLbCACt cht chroaacographlc sytceat ualng cht tictrnal  scandari
technique (Steclon 3.6.7.6.1.2).

          3.6.7,6.1.1    Prtparaeion ot calibracion  icandard*

          3.6.7.6.1.1.1  Prtpart  calibration  icandard toluciona of  fornalde*
hydt  and actetldthydt  in vacar  froa  cht «cock acandard  (Stecion 3.6.3,14,2)
Prtpart  che it  solucionj ac  cht)  following conctncraclona  (In >*g/«D  by  ttrial
dilucien of  cht  aceek  tcandard  soluclen:  30,  20, 10.   Prtpart addiclonal
calibration tcandard  toluclona  ac ch«  following  concencreeionj, by  dilution  o:
cht  appropriact  30.  20, or  10 Mg/«l  teandard:   3. 0.3,  2,  0.2, 1, 0.1.

                                     3-201
-------
          zacal Mg/raL - (RF) (are* of signal) (concentration factor)
where :
                                        Final Volume of Extract
          concentration factor -
                                        Initial Extract YoLuae

3-6.8     ?uaIL:v Canrral

          3.6.8.1   Refer :a Chapter One of Sf-gifi f0f guidance on quality
control, procedures.

3.6,9
          3.6.9.L   Th« HDL concencraciont Listed in Tab La 3,6-1 w«r» obtair.ed
using organic-free wacec and soLLd forbenc extraecLon,  Slnilar reiul;s were
achieved using a final effluent and sludge leachace   The HDL concentrations
lisctd In Table 3.6-2 wan obtained using organic -free water and aethylene
chloride extraction.   Similar results were achieved uaing representative
cnatrices.

          3.6,9,2   This o«thod has been ceiced for linearity of recovery fran
spiked organic- free water and has been deeons traced Co be applicable over :h«
rang* from 2 x .1DL co 200 x HOL.
                                            ^

          3.6.9.3   In a single laboratory ev«iu*eton ujlng several spiked
matrices, tha average recevariea presented In Tables 3-6-3 and 3.6-4 ware
obcalnad using solid sorbtnc and aechylana chloride excracclon. respectively
The standard devlatleiu of Che percent recovery ace also Included In Tables
3.6-3 and 3.6-4.

          3.6.9.4   A represencaclve chroaacograa is pr«t«nced In
Figure 3.6-1.
                                    3-20i
-------
          3,6.7.7.3 If che p«ak area exceeds  cha  linear range of  ;he calibra-
tion curve, a smaller saapi* "'olume should be used,  Alcernatively. che fir.a'.
solution may bt diluted with echanol and  reanalyzed.

          ].5.r.7.i. If ;he peak area aeasurenanz  is prevented by  che presence
of observed incerfarencas, further cleanup is requlrid.  However, none of ;l-.e
1600 aechod series have been evaluated  for ;his procedure.

          3,6,7.3   Calculations

          3.6.7.3.1 Calculate each response factor as  follows (mean value
baaed on 5 points):

                eancenrration of standard
          R? -      ar«a  of che signal
                               5
                              (I «,)
                      	       1
          mean - RJ - RT  -    	
          1.6,7,8.2 Calculate ch« concentration of  formaldehyde and acecalde
hyde as follows:
                «  
-------
                               Table  3.6-*
                    SIXCLX OPERATOR ACCL1UCY AND PRECISION
                     us IMC HITHYU.WE  CHLORIDE IXHACT:ON
AnftLyct "/P*
forBildthyd* Rtflfinc
•Actr
Ground-
vicar
Liquid*
u«eir
Ground-
vac«r
Liquid*
(2 eyp«*>
Solid*
Ptrctnc
R*eov«ry
X
91
92.3

69 6
40. 1
63. ft

44.0
31.4
ScindArd
D«vl*cion
P»rc«nc
P
2,3 '
82

16-3
3.2
10,9

20.2
2.7
Splk*
30-1000
50

230
30-1000
30

230
0,10-1. 0€
S'uaotr !
of
Ar.4-.-m
9
i

L2
9
12

12
12
it - Av«rtf« r«cov«ry «xp«eead far ehls a>ehp4
p - Av«r«|« luiMUird davl«tlon txp«ce«d Cor ehia  Mchod.
                                    3-206
-------
3.6,10
          F«d«r«L Regisctr, 1996, 51, i.0643- 40632; Noviab«r  7
2.         EPA Machod* 6010, 7000, 7041,  ?0«0,  7131,  76,21, 7^70,  7740, and
                             for £v«lu*ein| Solid
                                                                        .
                    SU-846, TKlrd Edition.  S«pciuib«c  L98S.  oefic* of  Soil!
                                                           .
                and Eaargtncy Miponit. U.S. Envtronmtrical ProcacrLan
          -Ajhingcon, D.C.  20^60,
                                     3-205
-------
                                        METHOD OOUA
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    •9 so-"*: aaa
    "«-'9« "ma:
     r ' I
   ' 1.'
          . (I
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     a^
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ia-91*.
•f 3 iOluff« •( 100
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                                             JC-*
                                     sr i«
                                 *r«rgii«t:
                                               10
                                              'f
M.4.4
                                         tnvitf
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                                  71* J
                                                                             •!'•»•§»•
                                                                              :•;-:§
                                                                                       ,'M
                                                                                   ! J »iu-: •
                                                  i?  -••
                                                                                     *« TJ  -7
                                                                               '5
                                                                               7 1 S 1
                                                                                     •• «§»•:• ii
                                                                                     -0 JIM'-:
                                             3-208
-------
                        Figure 3 . 5-i
«lM£S£
-------
                                                     00 UA
  'I      •••Mr*
'* S.I 2.!
IW11*

»*«• •»«« t||ilt«f
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                                         '9' out:
                                              rK

                                               r
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                                          3-209
-------
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 sem1vo1at11e Prfndpal Organic Hazardous Compounds
(POHCs) from Incineration systems (PHS, 1967).    This method also may be used
to determine parti oil ate 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  participate  pollutants  are withdrawn from an emission
source at an Isoklnetlc sampling  rate  and  are collected In a muIt1component
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 o.^aMc,-laden participate materials and
the  porous  polymeric   resin   to   adsorb   seal volatile  organic  species.
Semlvolatlle 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  in  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 nethylene
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  saopllng  train  configuration  Is  adapted  from  EPA
     Method  5 procedures,  and,  as such,  the majority of  the  required equipment
                                   0010 - 1
                                                          Revision
                                                          Date  September 1986
-------
                                  ••Sent**     I I!
T««np««li

        PtolM-*^
     H**«l A*e«


Sl«*MMI
                     HtvtfM-f yp* Piiol lit*
      o
      I
      IVi
                   fttot MafMnMl
                                                  fUcw culMwn Pump

                                                               TtttmMMMMfi
                                                     CbiNc*
it o
                                                                                                  Line
                                                               Diy CM Uelci    Ail lii^il Pt.mp
vO
t»
Ol
                                                         Figure I. Modi I led Mmtiod 5 Sampling Tram.
-------
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  semlvolatile  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-05SI (see Martin, 1971,  in Section 13.0, References); commercial
models of this  equipment  are  also  available.   Specifications for the
sorbent module- are provided In  the following subsections.  Additionally,
the  following  subsections  11st   changes  to  APTO-0581  and  Identify
allowable train configuration modifications.

     4.1.3  Basic operating  and  maintenance procedures for the sampling
train are  described   In  APTD-0576  (see  Rom,  1972,  In  Section 13.0,
References).  As correct usage  Is  Important In obtaining valid results,
all  users  should  refer  to  APTD-OS76  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 I.D.   The nozzle shall be buttonhook
     or elbow design  and  constructed   fron  seamless   tubing  (If made of
     stainless steel).   Other  construction  materials may be considered
     for  particular applications.  A   range  of nozzle  sizes  suitable for
     isoklnetic sampling should  be  available   In  Increments of 0.16 cm
      (1/16  1n.), e.g., 0.32-1.27   c«   (1/8-1/2   In,), or  larger  If higher
     volume sampling  trains are  used.     Each nozzle shall be calibrated
     according to  the procedures outlined  fn Paragraph  9.1.

          4.1.3.2   Probe Hner:  Boroslllcate or quartz-glass  tubing with
     a  heating system capable  of   maintaining  a gas temperature of  120  +
      14*C (248 + 2S*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  1s  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  boroslllcate or quartz-
     glass  probe  liners nay 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
     boroslllcate  1s  820*C   (1508T).   and for  quartz 1500'C  (2732*F).)
     Water-cooling of the  stainless   steel  sheath  w111  be  necessary at
      temperatures  approaching  and  exceeding 500*C.

          *•1-3.3   P1tot tubt!   T*P«   s'   **  described In Section 2.1 of
      EPA  Method 2,  orother   appropriate   devices   (Vollaro,  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  pltot   tube  shall   be   even with  or  above the
      nozzle entry  plane  (see  EPA   Method 2,  Figure  2-6b)  during  sampling.
      The  Type  S   pltot  tube   assembly  shall   have  a  known  coefficient,
      determined  as outlined  1n Section 4 of EPA  Method  2.

                              0010  -  3
                                                     Revision       0
                                                     Date  September 1986
-------
     4.1.3.4  Differentia)  pressure  gauge:   Inclined manometer or
equivalent device as described 1n Section  "2.2 of EPA Method 2.  One
manometer shall be  used  for  velocity-head   (4P)  readings and the
other for orifice differential pressure  (AH) 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 will  not  Introduce organic material fnto 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  or   120  +   14'C   (248  + 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  (S.4*n  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 nay  be  used.

      4.1.3.7   Organic  samel Ing module;   This  unit  consists of three
 sections,  Including a  gas-conditioning  section,  a  sortent  trap, and
 a condensate  knockout  trap.    The   gas-condlttoning  system shall be
 capable of  conditioning the gas  leaving   the back half of  the  filter
 holder to a temperature not exceeding 20*C (68*F).   The  sorbent  trap
 shall  be sized to  contain  approximately  20   g  of porous  polymeric
 resin  (Rohm 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 coomonly used coolant  1s   Ice  water  from  the Implnger  Ice-
water  bath, constantly  circulated   through   the  outer Jacket, using
 rubber or plastic tubing and  j   peristaltic pump.   The  sorbent  trap
 should be outfitted with  a  glass  well  or depression,  appropriately
 sized  to accommodate a small  thermocouple 1n 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  formed  vertically  downward from the
 ccfivil b'viiiiiy  ivvtlun,   through  the  adsorbent  media,  and into the
 condensate  knockout trap.  The  knockout  trap 1s usually  similar  in
 appearance  to  an  empty   Inplnger  directly  underneath the  sorbent
 module; It  may be oversized but  should have a shortened center  stem
 (at  a minimum, one-half the length  of the normal Implnger stems)  to
 collect  a  large   volume   of   condensate  without  bubbling  and
 overflowing Into the Inplnger  train.    All surfaces of the  organic
 module wetted by the gas   sample shall be fabricated of boroslHcate
 glass, Teflon, or other Inert materials.  Commercial  versions  of the
                         0010 - 4
                                                Revision
                                                Date  September 1986
-------
complete organic moduli  art  not  currently  available,  but may be
assembled from  commercially  available  laboratory  glassware and a
custom-fabricated sorbent trap.   Details  of two acceptable designs
ire shown In Figures  2  and  3  (the  thermocouple well is shown In
Figure 2).

     4.1.3.8  Implnger train;    To determine the stack-gas moisture
content, four 500-mL implngers,  connected  In series with leak-free
ground-glass Joints, follow the  knockout  trap.   The first, third,
and  fourth  fmplngers  shall  be  of  the  Greenburg-Smlth  design,
modified by replacing the  tip  with  a  l.3-cm (1/2-tn.) 1.0. gltss
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  acid  (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,  1eak-freepump,  thermometers  capable  of measuring
temperature  to  within  3*C    (5.4*F),  dry-gas  liter  capable  of
measuring volume to within   IS,  and  related equipment, as  shown in
Figure  I.  At a minimum,  the   pump   should be capable of 4  cfn 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
Isoklnetldty and of determining sample volumes  to within 21 may be
used.   The metering system must be used 1n conjunction  with a pi tot
tube  to enable checks of  1sok1net1c sampling  rates.  Sampling trains
using metering systems  designed   for  flow   rates higher  than those
described In APTO-0581 and APTD-Q576  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
m. Hg).   In many casts   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  1s applied  at a rate of minus 2.5 m 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  (asdescribed1n  Sections 2.3  and 2.4 of
EPA Method 2),  and  gas   analyzer,   If necessary  (as described In EPA
Method  3).    The temperature   sensor  ideally  should be permanently
attached   to   the   pilot    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
                                                Revision
                                                Date  September 1986
-------
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-------
     Alternatively,  the sensor may be  attached  Just prior to  use  In  the
     field.   Note,  however,  that If the temperature sensor is Attached in
     the  field,   the  sensor  must  be  placed  In  an Interference-free
     arrangement *Hh respect to the Type  S pttot tube openings (see  EPA
     Method 2,  Figure 2-7).   As  a second alternative, If a difference of
     no more  than  U  In  the  average  velocity  measurement  is to be
     Introduced,  the temperature gauge need  not be attached to the probe
     or pi tot tube.

          4.1.3.12  Callbratton/fleld-preparatlon  record:  A permanently
     bound laboratory notebook, In which  duplicate copies of data  may be
     made as they are  being  recorded,  1s  required for documenting  and
     recording calibrations and preparation  procedures (I.e.,  filter  and
     silica gel  tare  weights,  clean  XAD-2,  qual Ity 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 prob*.  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 may be extracted  by  exposure  to organic solvents used  for
sample  recovery.

     4.2.3   Glass  sa^>1e  storage  containers:    Chemically  resistant,
borostllcate 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  Pttrl dishes:    Glass,   sealed around the circumference with
wide (l-ln.) Teflon tape, for  storage  and  transport  of filter  samples.
      4.2.5
water to  the  nearest   1*  oL  or  1   g.     Graduated  cylinders  shall have
subdivisions not  >2  •(..     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.

      4.2.7   Funnel and rubber  poltceaan:    To aid in transfer of  silica
gel  to container (not  necessary 1f silica gel  1s weighed In  field).


                              0010 - 8
                                                     Revision  _ 0
                                                     Date  September  1986
-------
    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:     01st1Hed-1n-glass  grade  Is  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
            «0.001I) 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 MAUDLINS

     6.1  Because of  complexity  of  this  method,   field personnel  should  be
trained 1n  and  experienced  with   the  test  procedures  1n  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  APTO-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 may   Instead  be weighed directly fn the
     tmplnger 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 Petrf
     dishes) and keep the f 11 ten   1n   these  containers  at all  tines except
     during sampling and  weighing.

          6.2.4  Desiccate the filters at   20  * $.ft«C (68 * 10'F) and anblent
     pressure  for  at least 24 hr,  and weigh at  Intervals of"at least  6 hr to a
     constant weight (I.e.,  <0.5-ng   change from previous weighing),  recording
     results  to  the  nearest  0.1 ng.    During  each weighing the filter nust not
     be exposed  for  more  than a   2-«1n period to the  laboratory atmosphere and
     relative  humidity above 501.     Alternatively  (unless otherwise  specified
     by the Administrator),  the  filters  uy be  oven-dried  at IQS'C (220*F) for
     2-3 hr,  desiccated  for  Z hr,  and weighed.
                                   0010 - 10
                                                          Revision
                                                          Date  September 1986
-------
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  is  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 Is 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 Is not necessary to  change   the nozzle size In order to maintain
Isoklnetlc sampling rates.   During   the  run,  do not change the nozzle.
Ensure that the  proper  differential  pressure  gauge  1s chosen for the
range of  velocity heads encountered  (see Section 2.2 of EPA Method 2).

     6.3.3  Select a suitable  probe  Uner  and probe length so that all
traverse  points  can be  sampled.    For  large stacks, to reduce the length
of  the probe, consider  sampling  froa  opposite  sides of the stack.

     6.3.4  A mini nun of 3 dsca  (105.9  dscf) of  sample volume  Is required
for the determination of the   Destruction and  Removal Efficiency (ORE) of
POHCs froa  Incineration   systems.    Additional   sample  volume shall be
collected as necessitated  by analytical  detection  Halt constraints.  To
determine the   minium   sample   volume    required,   refer  to  sample
calculations  In  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 aln.
                                           4

     6.3.6    In  SOB*  circumstances  (e.g.,  batch  cycles)  it  nay 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 «1th  Teflon  film or
aluminum  foil until Just prior to  assembly or until sampling Is about to
begin.
                              0010 - 11
                                                     Revision
                                                     Date  September 19S6
-------
     6.4.2  Fill the  sorbent  trap  section  of  the organic module  with
approximately 20 g 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 3M Company,
St. Paul, Minnesota.

     6.4.3  If an Impinger train  Is  used to collect moisture, place 100
mL of water In each of the  first two Implngers, leave the third Impinger
empty (or  charge  with  caustic  solution,  as  necessary), and transfer
approximately 200-300 g of  prewelghed  silica  gel from Its container tc
the fourth Impinger.  More  silica  gel  may  be used, but care should be
taken to ensure  that  U  Is  not  entrained  and  carried  out from the
tmplnger during sampling.  Place the container In a clean place for later
use In  the sample recovery.   Alternatively, the weight of the silica gel
plus Impinger 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 stream  fro* circumventing the filter.  Check the
filter  for tears after assembly  Is  computed.

     6.4.5  When glut linen arc used.  Install the  selected nozzle  using
a VUon-A 0-nng when stack  temperatures  art <260'C  (500*F)  and a  woven
glass-fiber gasket when   temperatures  art   higher.    See  APTD-0576  (Rom,
1972)   for  details.     Other  connecting  systems   utilizing  either  316
stainless  steel or  Teflon  ferrules   may   be used.   When metal  liners  are
used,  install  the nozzle as  above, or   by a  leak-free direct mechanical
connection.   Hark  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  In  Figure 1.  During assembly,  do not  use
any slUcone  grease on ground-glass Joints  that  are located upstream of
 the organic  module.   A very  light  coating  of  si 11 cone grease nay 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   minimize  si 11cone-grease   contamination.
Subject to  the approval  of the Administrator,  a glass cyclone may be used
between the  arch* *nd thf flltfr  h«H*r Hh*n  th*  tQti! p*rttculit§  Citch
 Is expected  to exceed 100 mg  or  when  water droplets are present in  the
 stack.   The  organic module condenser  must  be  maintained  at a temperature
of  17   +   3*C.     Connect  all   temperature  sensors to   an appropriate
potentiometer/display 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
-------
     6.4.8   Turn  on  the  sorbent  moduli  and  condenser  coll coolant
redrcutitlng pump and  begin  monitoring  the  sortient  module gas entry
temperature.  Ensure proper  sorbent  module gas entry temperature before
proceeding and again before any  sampling  is Initiated.  It 1s extremely
important that the  XAD-2  resin  tenperature  ntver exceed 50*C (122*F),
because thermal decomposition  will  occur.    During  testing, the XAO-2
temperature must not  exceed  20*C  (68*F)  for  efficient capture of the
semlvolatlle 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-check procedures

     6.5.1  Pre-test leak-check:

          6.5.1.1    Because  the  number  of  additional  intercomponent
     connections 1n the Sem1-VOST train (over the M5 Train) Increases the
     possibility of leakage, a pre-test leak-check 1s required.

          6.5.1.Z  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  Vtton  A  0-Hng  or other leak-free connection Is
     used in assembling the probe  nozzle  to the probe  liner,  leak-check
     the  train at the  sampling site  by plugging the nozzle and pulling  a
     381-mm Hg  (!5-1n. Hg) vacuum.
     (NOTE:  A  lower vacuum may  be used, provided that  1t  Is 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  1mp1nger  (shown
     in Figure 4) to  the  Inlet   of the  filter holder  (cyclone,  11 applic-
     able)  and then plugging  the  Inlet   and pulling  a 381-nn Hg  (15-in.
     Hg)  vacuum.   (Again,  a  lower  vacuum  Bay be used,  provided that it is
     not exceeded during  the  test.)  Then, connect  the probe to the train
     and leak-check at about   25-e*  Hg  (l-1n.  Hg)  vacuum;  alternatively,
     leak-check the probe with the rest of the  sampling train  In one step
     at 381-nn Hg  (li-ln. Hg)  vacuum.     leakage  rates In  excess of 41 of
     the average sampling rate  or >0.00057 m^/mln (0.02  cfv), whichever
     is less,  are unacceptable.

           6.5.1.4  The following leak-check instructions for the sanpHng
     train  described  1n 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 1s 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 1968
-------
              lilt
                                                  21/11 «*i«
Joint
     Figure 4.  Leak-check 1 ginger.
                0010 - 14
                                        Revision       o
                                        Date  Septeatier  1986
-------
         6.5.1.5  When  tht  leak-check   Is competed,  first  slowly  remove
    the plug  from the Inlet  to   the probe,  filter holder, or cyclone  (If
    applicable).  When  the  vacuum drops  to  127  mm  (5  In.) 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.Z  Leak-checks  during  sampling run:

         6.5.2.1   If, during the sampling run,  a component  (e.g.,  filter
    assembly,  Implnger,  or   sorbent  trap)   change  becomes necessary, a
    leak-check shall be conducted  immediately after  the Interruption of
    sampling  and before the change  Is  made.   The  leak-check shall be
    done according  to the procedure  outlined 1n Paragraph  6.S.I,  except
    that it  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 m^/mln  (0.02 cfn)  or 4V
    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 (s obtained,
    the tester shall void the   sampllna 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   Teak-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-cheek  shall be  done with  the same procedures
    as those  with   the   pre-test  Teak-check,  except that It shall be
    conducted at  a  vacuum   greater than  or  equal to the  maximum value
    reached  during  the  sampling run.   If the leakage  rate 1s found to be
    no greater than  0.00057  oP/iln   (0.02  cfa)  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  Sampl1ng-tra1n operationt

     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  + 14*C
(248 * 25*F)  and  a gas temperature entering the sorbent trap at  a maximum
of 20TC (68'F).

                             0010 - 15
                                                    Revision     0
                                                    Date  September 1966
-------
     6.6.2  FOP each pun, 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  sailing  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 1n 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 pHot 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  In  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   pi tot-tube   coefficient are outside  the above
ranges,  do not use  the  nomographs unless  appropriate steps (SMgehara,
 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  laplnger   stea),  take care  to  close the
coarse-adjust valve before Inserting the probe  Into the stack,  to  prevent
water from backing Into  the organic nodule.    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 stick cross  section, as  required by  EPA Method  1
or as specified  by the  Administrator,  being careful not to bump the probe
 nozzle  Into the  stack walls when sup ling near the walls or when removing
.or Inserting  the probe  through the  access  port,  In order  to  minimize the
      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 1ce 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 aanoneter.
                              0010 - 16
                                                     Revision      0
                                                     Date  September 1966
-------
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                                                      figure 5.  Paniculate field data.
-------
         6.6.8  If  tht  prtssurt  drop  across  the  filter  or sorbent trap
    becomes too high, making  isoklnetlc  sailing difficult to maintain,  the
    filter/sorbent trap may be replaced 1n the  midst of a sample run.  using
    another complete  filter  holder/sorbent  trap  assembly  1s recommendtd,
    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 participate weight  shall  Include  the summation of all filter
    assembly catches.

         6,6.9  A single  train  shall  be  ysed  for  the entire sample run,
    except  In cases where simultaneous  sampling  1s  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  Implnger
     (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  nay   bt  combined  (as may the
     Implnger catches),  and one analysis  of  front-half catch and one  analysis
    of  Implnger catch may be  performed.

         6.6.11   At  the end   of   the  sarnie  ran, turn off the coarse-adjust
    valve,  remove the probe  and   nozzle   froa   the   stack,  turn off  the pump,
    record  the  final  dry-gas  meter  reading,   and   conduct a  post-test leak-
    check.   Also,  leak-check  the   pUot   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   1sok1netlcUy   (set  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 is
     removed froi the stack  at  the  end   of  the   saapllng  period.   Allow the
     probe  to cool.    When   the  probe  can  be safely  handled, wipe off all
     external paniculate Better neer the  Up  of  the pruov  naiile  itiu M'«£i «
     cap over the tip to prevent  losing or gaining  particulate  natter.   Do not
     cap the probe  tip  tightly  while  the  sampling  train   is cooling  down
     because this will create  a  vacuun  In  the  filter holder, drawing water
     from the Implngers into the sorbent  nodule.

          7.1.2  Before noving the  staple  train   to the  cleanup  site,  remove
     the probe froa the sample  train  and  cap the open outlet, being careful
     not to lose any condensate that night be present.  Cap the filter inlet.
                                  0010 - 18
                                                         Revision
                                                         Date  September 1986
-------
Remove the umbilical cord from  the  last  Implnger 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 nodule.

     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,  the  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 contalners;

     7.2.1  Container no.  1:  Carefully remove the  filter  fro* the  filter
holder and place  It  In  Its  Identified  Petrl dish container.  Use  a pair
or pairs of tweezers to handle  the   filter.   If  It  Is necessary to fold
the   filter,   ensure   that  the  partIculate  cake   Is  Inside the fold.
Carefully  transfer  to  the   Petrl  dish  any  part1culate utter 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.-wlde Teflon  tape  around  the  circumference  of the Hd.

      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  from the
probe  nozzle,  probe fitting,  probe  liner,   and  front half  of the  filter
holder by  washing these components  first  with nethanol/methylene  chloride
 (1:1  v/v)  into a   glass  container.    Distilled  water may  also  be used.
Retain a water and solvent blank   and analyze  In  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 methanol/-
      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  In a similar way until  no  visible particles remain.

                              0010 -  19
                                                     Revision     0
                                                     Date  September 1986
-------
         7.2.2.2  Hive 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
    p'robe  in 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  partlculate  matter  that Is brushed
    from the probe. Run the  brush through the  probe three times or more
    until  no visible partlculate matter  1s carried out with the solvent
    or until none remains In  the probe  liner on visual  Inspection.  UUh
    stainless steel or other  metal .probes, run the brush through In the
    above-prescribed manner at least  six  tines (metal  probes have small
    crevices  In which partlculate  matter  can   be  entrapped).  Rinse the
    brush  with  solvent and quantitatively  collect these  washings (n 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 contamination.

         7.2.2.5 Clean   the   Inside   of  the   front   half of  the filter
    holder and  cyclone/cyclone flask,  If  used, by  rubbing  the  surfaces
    with a  nylon   bristle  brush   and   rinsing with  Mthanol/methylene
    chloride (1:1  v/v) mixture.  Rinse   each  surface  three times or more
     If needed  to remove  visible partlculate.    Hake  a  final  rinse of  the
    brush  and  filter holder.   Carefully   rinse  out the glass cyclone  and
     cyclone flask   (tf applicable).     Brush   and   rinse  any partlculate
    material  adhering to the Inner surfaces  of  these  components  (nto  the
     front-half rinse sample.   After all solvent washings  and partlculate
    matter have been collected In  the sample  container,  tighten  the  ltd
     on the sample container  so that solvent will not  leak out  when  it  is
     shipped to the laboratory.   Mark  the  height of the fluid  level  to
     determine  whether   leakage  occurs   during  transport.     Label  the
     container to identify its contents.
module may 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 Is used as  the transport container, both ends should
be sealed with tightly fitting  caps  or plugs.  Ground-glass stoppers or
Teflon caps Bay  be  used.    The  sorbent  trap  should then be labeled,
covered with aluminum foil,  and  packaged  on  Ice  for transport to the
laboratory.  If a  separate  bottle   Is  used,  the spent resin should be
quantitatively transferred fro* 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 1986
-------
     7.2.4  Container no. 4:    Measure the volume of condensate collected
in the condensate knockout section of  the organic module to wlttitn +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 HquTd present and
note any discoloration or film In 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 nodule.
If condensate Js 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 Us
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 in
removing the  silica gel fran the Implnger.  It 1s not necessary to remove
the small amount  of  dust  particles  that  may  adhere  strongly to the
implnger wall.  Because the  gain  In  weight  Is to be used for moisture
calculations, do not  use  any  water  or  other  liquids to transfer the
silica gel.   If a balance Is  available 1n the field, weigh the container
and Its contents to 0.5 g or better.

7.3   Implnqer water;
                                             *
      7.3.1  Hake a notation  of  any  color  or fill  In the liquid catch.
Measure  the liquid  1n  the first three   laplngers  to within  *l mL  by  using
a  graduated cylinder or   by  weighing   it   to  within  +lance  (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   1s   required (tee
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 Is  used, measure the amount
of moisture  condensed either volumetrtcally or gravlmetrlcally.


                              0010 -  21
                                                     Revision      0
                                                     Date  September  1956
-------
     7-4  Sample preparation  for  shipment:    Prior to shipment, recheck all
sample containers to ensure that the caps  are w«11 secured.  Seal the Hds of
all containers around the  circumference  with  Teflon  tape.  Ship all liquid
samples upright on 1ce and all  paniculate filters with the paniculate catch
facing upward.  The paniculate filters should be  shipped unrefrlgerated.


3.0  ANALYSES

     8.1  Sample preparation;

          8.1.1  General:  The  preparation   steps for all  samples will  result
      in 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/HS.  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  HOL  when the  solvent  Is  reduced in
      volume to the desired level  (I.e.,   10 ml).   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.

          8.1.2  Condensate:    The   'condensate'   Is  the moisture collected in
      the  first implnger  following the XAO-2 module.   Spike  the  condensate  with
      the  surrogate standards.  The   volum*  Is  measured and recorded  and  then
      transferred to  a separatory funnel.    The   pH  Is   to  be  adjusted to  pH 2
      with 6 N sulfurlc acid,  If necessary.  The  sample  container and graduated
      cylinder are  sequentially rinsed with  three successive 10-aL aliquots 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 nln.  After
      complete separation of the phases,   remove   the  solvent and transfer  to a
      Kuderna-Danish  concentrator (K-0),  filtering through a bed  of precleaned,
      dry  sodium sulfate.    Repeat  the  extraction  step  two additional  times.
      Adjust the pH to 11  with 6 N sodium hydroxide and  reextract combining the
      acid  and base extracts.  Rinse the sodium sulfate  Into the K-0  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 ig voluaa with ffvin  solvent.  In  order tu  achieve tile
      necessary detection Halt, 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 redIssolved with  fresh  solvent taking the volume to some
      finite amount.  After adding a  standard (for the purpose of quantltatlon
      by GC/HS),  the sample Is  ready  for  analysis, as discussed in Paragraph
      8.2.
                                   0010 - 22
                                                          Revision
                                                          Date  September 1936
-------
     8.1.3  linger-.   spike  the  sample  with the surrogate standards;
measure and  record  the  volume  and  transfer  to  a separatory funnel.
Proceed as described In Paragraph 8.1.2.

     8.1.4    XAD-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 XAD-2 module directly over the
thimble.  The glass  frit of the module (see Figure 2) should be In 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
XAD-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 in 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 Is 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 1$ 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-0 and concentrate as described
In Paragraph 8.1.2.

     3.1.5   Partfculate  filter   (and   cyclone  catch):    If  paniculate
loading (s  to be   determined,  weigh the  filter   (and cyclone catch, if
applicable).  The  partlculate  filter   (and cyclone catch,  If  applicable)
Is transferred to  the glass  thimble  and  extracted  simultaneously with the
XAD-2  resin.

     8.1.6   Train  solvent  rinses:     All  train  rinses (I.e., probe,
Implnger,  filter housing) using   the extraction solvent and nethanol are
returned to the  laboratory  as   a   single  sanple.     If   the rinses are
contained  In more   than   one container,   the   Intended  spike Is divided
equally among the  containers proportioned  fron a  single  syringe volume.
Transfer the rinse to a separatory   funnel and add  a  sufficient aaount of
organic-free water so  that  the  methylene  chloride  becomes Imlsclble and
its 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  Sample analysis;

     8.2.1  The  primary analytical   tool for  the measurement of  emissions
from hazardous waste Incinerators  1s   GC/MS  using fused-slUca  capillary
GC  columns,  as described  1n 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
-------
    9-3  Metering system:

         9.3.1  Before  its   Initial  use   In  the  field, the metering system
    shall be calibrated  according  to  the  procedure outlined 1n 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, It 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 irK/mln  (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  rang*   of   orifice  settings, as
    outlined  In APTD-0576.

         9.3.3  Leak-check of Metering  system1:    That portion of the sampling
    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  In.)  water column by blowing  Into
    the  rubber  tubing.   Pinch off  the  tubing  and observe the manometer  for  I
    mln.   A  loss of pressure on  the  manometer  indicates a leak  in  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
Its Initial  use  In  the field  according to  the procedure outlined  1n  APTD-057S.
Probes constructed   according  to  APTO-OSfll  need  not   be  calibrated  if  the
calibration curves  tn  APTD-0576  are used.
                                  0010 - 25
                                                         Revision
                                                         Date  September 1986
-------
    with  sample  analysis,  prescreenlng  of   the  sample  extracts  by  gas
    chromatography/flame   lonlratlon  detection   (GC/FID)  or  with  electron
    capture  (GC/ECD)  1s encouraged.   Information  regarding the complexity anc
    concentration level  of  a   sample  prior   to  GC/MS  analysis  can be oi
    enormous  help.    This  Information  can   be  obtained  by  using either
    capillary columns or less   expensive  packed  columns.   However, the FIE
    screen should be  performed  with   a  column  similar to that used with the
    GC/MS.   Keep  in mind   that   GC/FID  has  a  slightly lower detection Hmti
    than GC/MS  and, therefore,  that   the  concentration  of the sample can b<
    adjusted either up or  down  prior  to analysis  by GC/MS.

         8.2.2   The mass spectrometer will  be   operated 1n a full scan (40-
    450) mode for most  of  the  analyses.     The  range  for which data an
    acquired In a GC/MS  run  will be  sufficiently  broad to encompass the inajoi
    Ions, as listed  In Chapter  Four,  Method 8270,  for each of the deslgnatec
    POHCs  1n an Incinerator  effluent  analysis.

         8.2.3   For most purposes,  electron  lonlzatlon  (El)  spectra will b<
    collected because a  majority  of  the  POHCs  give reasonable  El soectra
    Also,  El spect-a  are compatible  with   the  NBS Library of Mass  Spec--a am
    other mass  spectral  references,   which  aid In  the  identification    ;ces
     for other components in  the Incinerator process streams.

          8.2.4   To  clarify   soew  Identifications,  chealcal  lonlzatlon  (CI
     spectra using either  positive  Ions  or  negative   Ions   will  be  used t
     elucidate molecular-weight  Information  and  sl^llfy   the  fragnentatlo
     patterns of some compounds.   In no case, however, should  CI  spectra alon
     be used for compound Identification.   Refer to Chapter  Four,  Method 8270
     for  complete  descriptions   of   GC   conditions,   MS  conditions,   an
     quantitative and quantitative Identification.


9.0  CALIBRATION

     9.1  Probe  nozzle;     Probe  nozzles   shall   be  calibrated before thel
initial use In the field.  Using  a oiler  -ter, treasure the Inside diameter o
the nozzle to the nearest 0.025  on   (0....  in.).  Hake measurements at thre
separate  placet  across  the   dlaMter   and   obtain  the  average  of  th
measurements.  The  difference  between  the  high  and  low numbers shall  no
exceed 0.1'mi (0.004  In.).    When  nozzles bccoett nicked,  dented, or corroded
they shall  be reshaped, sharpened,  and  recalibrated before use.  Each nozzi
    1  h* n*m»HM»tw »nA n«1nii*1u  1H«nt1f1**l
     9.2  PI tot tube;   The  Type  S  pUot  tube assembly shall be calibrate
according to the procedure outlined 1n Section  4 of EPA Method 2, or assigns
a nominal coefficient of 0.84 If It 1s not visibly nicked, dented, or corrode
and If 1t meets design and Intel-component spacing specifications.
                                  0010 - 24
                                                         Revision      0
                                                         Date  September 1986
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          4.2.8  Funnels:  Glass, to aid In sample recovery.

     4.3  Filters:   Glass-  or  quartz-fiber filters, without organic binder,
exhibiting at least 99.951  efficiency  «0.05I penetration) on 0.3-ym dfoctyi
phthalate smoke particles.  The  filter  efficiency test shall bi conducted In
accordance with ASTN standard method 02986-71.   Test data from the supplier's
quality  control  program  are  sufficient  for  this  purpose.    In  sources
containing S02  or  503,  the  filter  material  must  bt  of  a  type that is
unreactive to SO? or SOj.   Reeve  Angel  934  AH or Schlelcher and Schwell 13
filters work welt under  these conditions.

     4.4  Crushed 1ce;    Quantities  ranging  from  10-50 Ib may be necessary
during a sampling run, depending on an&lent air temperature.

     4.5  Stopcock  grease:    Solvent-lnsolublt, heat-stable slllcone grease.
Use of sIHcont grease upstream  of  the  moduli Is not permitted, and amounts
used  on  components  located  downstream  of  the  organic  module  shall  be
minimized.  Slllcone grease usage Is  not necessary If screw-on connectors and
Teflon sleeves or ground-glass Joints are used.

     4.6  Glass wool:  Used to  plug  the unfrttted end of the sorbent nodule.
The glass-wool fiber should bt  solvent-extracted with aethylene chloride  in a
Soxhlet extractor for 12 hr and a1r-dr1ed prior to use.


5.0  REAGENTS

     5.1  Adsorbent resin;   Porous  polymeric  resin  (XAO-2 or equivalent) Is
recommended.   These resins  shall  be  cleaned  prior  to their use for sample
collection.  Appendix  A of  this  method  should  be  consulted to determine
appropriate precfeanfng  procedure.   For  best  results, resin used should not
exhibit a blank of  higher  than  4  rag/kg of total chroaatographable organic*
(TCO)  (see Appendix 8) prior to use.   Once cleaned, resin should be stored in
an airtight, wide-mouth   aufcer  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 gel;   Indicating type, 6-li mesh.  If previously used, dry at
175*C  (350*F)  for 2 hr before using.   New silica gel nay be used as received.
Alternatively, other types of deslccants   (equivalent  or better) nay be used,
subject to the approval  of the Administrator.

     5.3   Inclnqer solutions;  Distilled organic-free  water (Type  II) shall be
used,  unless  sampling is Intended   to  quantify a particular  Inorganic gaseous
species.   If  sampling 1s Intended   to quantify the concentration of additional
species,  the  1ginger solution   of  choice  shall  be subject  to Administrator
approval.  This water   should  be   prescreened   for any compounds of  Interest.
One  hundred  mi. will be  added  to  the  specified  1np1nger;  the  third  Implnger In
the  train may be  charged with  a  basic  solution (1  N  sodium  hydroxide or  sodium
acetate)  to  protect   the  sampling  pump   from  acidic gases.   Sodium acetate
should be used   when   large   saajjle   volumes  are   anticipated  because  sodium
hydroxide will react  with  carbon  dioxide   In   aqueous  media  to  fora  sodium
carbonate, which  may  possibly  plug  the Itnplnger.

                                  0010 - 9
                                                          Revision      0
                                                          Date  September 1986
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    o
    o
    »-*
    o

     I
    Kl
                                   RUBIER
                                             RUBBER     ORIFICE
                                             SfOfTEH
                                                                          •V PASS VALVE
                                                                                           VACUUM

                                                                                           CALM.l
                      Mlft ••*•»! !<•

                      «*•»«!• IMC Hit
                                                                                                •IAIN VALVE CLOSf O


                                                                                               AIRTIGHT

                                                                                               PUMP
M O
• 3
O
«•*
l»

§
i»
-»
10
oo
                                                         Ftguie 6. Leak check ol melci bon
-------
     9.5  Temperature  gauges ;    Each  thermocouple  must  be permanently and
uniquely marked on  the  casting;  all mercury-ln-glass reference thermometers
must conform to ASTN E-l 63C  or  63F specifications.  Thermocouples should be
calibrated In 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 Is necessary If the  use of an extension lead produces a
change >1.5X.

          9.5.1  Implnger,  organic  module,  and dry-gas meter thermocouples:
     For the thermocouples used to measure  the temperature of the gas leaving
     the Implnger train and  the  XAD-2  resin bed, three-point calibration at
     Ice-water, room-air, and boiling-water temperatures 1s necessary.  Accept
     the thermocouples only If the readings at all three temperatures agree to
     +2'C  (3.6*F)  with  those  of   the  absolute  value  of  the  reference
     thermometer.

          9.5.2  Prota and stack thermocouple:   For the thermocouples used to
     Indicate the probe and  stack  temperatures, a three-point calibration at
     fee-water,  boiling-water,   and   hot-oil -oath   temperatures   must  be
     performed;  It  Is recommended that  room-air temperature 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 m  Hg   (0.1  tn. 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  Clas$-S  standard weights;  the weights  must be within  +0.5X
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 tn tht gas  stream,  proportion by volume.
        Cd - Type S pltot tube coefficient (nominally 0.84 + 0.02),
             dimension less.

         I • Percent of Isoklnetlc sampling.
                                   0010 - 27
                                                          Revision
                                                          Date  September 1986
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    La - Maximum acceptable leakage rate  for a leak-check,  either pre-test
         or following a  component  change;  equal   to 0.00057 m3/mln  (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 "itn« component change (1 • 1, 2, 3...n) nJ/mln
         (cfm).

    LD • Leakage rate observed during the post-test leak-check, mVmln
     M   (cfm) .

    Md  " Stack-gas dry molecular weight, g/g-mole (Ib/lb-mole).

    M*  - 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, m Hg  (In. Hg) .

   pstd  ' Standard  absolute pressure,  760 nn  Hg (29.92  In. Hg) .

      R  • Ideal  gas constant, 0.06236 m Hg-Bp/K-g-mole (21.85  in.
         Hg-ft3/*R-1b-mole).

    Tm  • Absolute  average dry-gas  neter temperature (see  Figure 6), K
          CR).

    T$  • Absolute  average stack-gas  temperature (see Figure 6), K (*R).

   Tstd  " Standard  absolute temperature, 293K (528*R).

    V]c  •  Total volume of liquid collected  In the organic  module condensate
          knockout  trap,  the Inplngers,  and silica gel, ml.

    Vm -  Volume of gas sample  as measured  by dry-gas meter, dscni (dscf).
vm(std) * Vo^uoe of gas sample measured by the dry-gas meter,  corrected
          to standard conditions, dscm (dscf).

Mstd) " VoluM of water vapor 1n the gas sample, corrected to standard
          conditions, so (scf).

     v« • Stack-gas velocity, calculated by Method 2, Equation 2-9, using
          data obtained from Method 5, m/sec  (ft/sec).

     "a • Weight of residue In acetone wash, ng.

       7 • Dry-gas-meter calibration factor, dlmenslonless.

     AH • Average  pressure differential across  the orifice meter  (see
          Figure 2),  mm HjO  (In.  HjO).
                                 0010 - 28
                                                        Revision
                                                        Date  September 1986
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       ^  «  Density  of water,  0.9982  g/ml  (0.002201  Ib/mL).

        8  •  Total  sampling  time,  min.

       81  «  Sampling time  Interval  from the beginning  of  a  run  until  tht
            first  component change, m1n.

       9\  »  Sampling time  interval  between two successive component
            changes, beginning with the Interval  between  the  first and
            second changes, m1n.

       Ip  •  Sampling time  Interval  from the final  (n*n) component  change
            until  the end  of the  sampling  run, mtn.

     13.6  «  Specific gravity of mercury.

       60  »  sec/m1n.

      100  »  Conversion to percent.
     10.3   Average  dry-gas-meter  temperature  and  average orifice pressure
drop:  See data sheet (Figure 5, "aboveJT
     10.4  Dry-gas volume:  Correct  the  sample neasurtd by the dry-gas meter
to standard conditions  [ZQ'C,  760  TO  Hg  [68*F,  21.92  1n.  Hgj)  by using
Equation I;


                    Tstd    Pbar * &H/l3'fi          'bar * ftH/l3'8
             ' V  —	—	Ki*taf	        (i)
                      Tn        pstd                      '•

where;

     <1 • 0.3858 K/m Hg for Mtrlc units, or
     K! * l7.64*R/1n. Hg for English units.

It should be noted that Equation !  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 ia.
If Ip or LI exceeds I*, Equation 1 mist be modified as follows:

      a*  Case I (no component changes nade  during sampling run):  Replace vm
          in Equation 1 with the expression:
                                  0010 - 29
                                                         Revision
                                                         Date  September 1986
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     b.  Case  II  (one   or  more   component  changes   made during  the  sampling
         run):Replace Vm in  Equation i by the expression:



         V™ '  'Ll '  L.)91   -

         and substitute only for those leakage rates  (LI or Lp)  that exceed
         La"-


     10.5  Volume  of water vapor;
where:
        • 0.001333 B3/ml. for metric units, or
        • 0.04707 ft3/nL for English units.
     10.6  Moisture content;
                               *  vw($td)
     NOTE:   In  saturated  or water-droplet-laden  gas  streams,  two  calculations
             of  the  moisture content of the  stack  gas  shall  be made,  one  froir
             the  Inplnger analysis  (Equation  3)    and   a   second   from   the
             assunptlon of saturated conditions.   The  lower  of the  two  values
             of  B* shall be considered  correct.  The  procedure for determining
             the moisture  content based upon assumption  of saturated  conditions
             is  given  In the Note to Section 1.2 of Method 4.   For  the  purposes
             of  this net hod, the   average  stack-gas  temperature from  Figure e
             may be  used to make  this determination, provided  that  the  accuracy
             of  the  In-stack temperature sensor is +l*C  (2*F).


     10.7   Conversion factors;

                                       To           Multiply by
                                       i*           0.02832
                                       ar/ftj       15.43
                                       Ib/ft'       2.205  x 10'3
                          g/ft*        g/i*         35.31
                                   0010 - 30
                                                          Revision
                                                          Date  September 198J
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     10.8  Isok1net1c variation:

          10.8.1  Calculation froa raw data:

              100 V*3Flc * (VV ("bar *  1H/13'6>]
where:
          I
          0.003454 mm Hg-m^/ml-K for metric units, or
          0.002669 1n. Hg-ft3/mL-*R for English units.

          10.8.2  Calculation for Intermediate values:
                               I •
                                                          (4)
                                                                        - (5)
                                    r     Vmfstd)

                                    4 PsW
     where:
          K4  • 4.320  for metric  units, or
          K4  • 0.09450  for  English  units.

          10.a.3   Acceptable results:    If   90S  ^  I  ^ UOX,  the  results  are
      acceptable.   If  the results are  low 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 n1n1mua sample  volume that  shall  be collected,  the
 following sequence of calculations  shall be  used.

          10.9.1   Proa  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 tux 1 BUB  amount  of   POHC  allowed   to  be  present in  the
      effluent.   This  may be expressed as:
                (WF)  (POHCj  cone)  (100-lORE)
                       100
                      100
                                                Max POHC,  Mass
                                                           (6)
      where:

           WF

        POHCt
mass flow rate of waste feed per hr, g/hr (Ib/hr).

concentration of Principal Organic Hazardous Compound (wt 1}
Introduced Into the combustion process.
                                   0010 - 31
                                                          Revision      0
                                                          Date  September 1986
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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 Hass
              	 • Max  PQHCf cone                            (7)

                -Oveff(std)

    where:

         DVeff(,td)  '  volumetric  flow  rate of exhaust gas, dscm (dscf),

         POHCf  cone  •  anticipated concentration of the POHC  In the
                       exhaust gas stream, g/dscm  (Ib/dscf).


         10.9.3  In  making  this calculation,  It  Is  recomnended that a safety
    margin  of at  least ten  be  Included:

              LDLWHC  x 10
                                                                          (8)
                 POHC1  cone

     where:
             poHC ' detectable amount of POHC In entire sampling  train.
          NOTE:  The whole extract fro* an  XAD-2 cartridge 1s  seldom If ever,
                 Injected at  once.    Therefore,  If  allquotlng  factors are
                 Involved, the LDlpoHC -1* not  the  sane as the analytical (or
                 col ion) detection MBit.
             VTBC • BlnlBua dry standard voluM to be collected at dry-gas
                    eater.
     10.io  concentration or  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 voluM, typically 10 ml.

     CpQHC (ug/BL) * sample voluae (mL) • amount (ug) of POHC In sample    (9)
                                  0010 - 32
                                                         Revision
                                                         Date  September 1986
-------
     where:

                " 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) * XAO-2 (ug) * condensate (ug) * rinses (ug) * Imptnger (ug)   (10)

     3)  Divide the total ug found by the volume of stack gas sampled (m3).

     (Total yg)/(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.

     11.2  Analysts;  The  quality  assurance  prograa required for this study
Includes the  analysis  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 analysts 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  If  problems are observed In laboratory
operations or In field sampling activities.

           11.2.1  Field  Slinks:    Field  blanks  ust  be submitted with the
     samples collected at each sampling  site.    The field blanks include the
     sample bottles containing  all quo ts  of  staple recovery solvents, unused
     filters, and resin cartridges.  At a •fnlaua, ont complete sampling train
     will  be assembled in the field  staging area, taken to the sampling trtt,
     and  leak-checked at the beginning and end of the testing  (or for the same
     total number of ttws as the  actual  ttst 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  wert  an actual test saaple.   No gaseous
     sample will be passed through the  sampling  train.

           11.2.2  Method blanks:   A method blank nist be prepared for each set
     of  analytical  operations,   to evaluatt contamination and artifacts that
      can  be derived  frosi  glassware,   reagents,  and   saaple  handling  1n the
      laboratory.

           11.2.3    Refer  to  Method   8270   for additional   quality  control
      considerations.


                                   0010 - 33
                                                         Revision      0
                                                          Date  September  1986
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12.0  METHOD PERFORMANCE

     12.1  Method performance evaluation;  E  .luatlon of analytical procedures
for  a  selected  series  of  confounds  mus.  Include  the sample-preparation
procedures and  each  associated  analytical  determination.    The analytical
procedures should be challenged  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 (HDL).
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  Method precision and bias:    The overall method precision and bias
must be determined onacompound-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  -131  and  -161  have  been determined for
toluene and 1,1,2,2-tetrachloroethane, respectively.  A precision of 19.9* was
calculated from a field test  data  sat  representing seven degrees of freedom
which resulted from a series of paired, unsplked Semi volatile Organic Sampling
trains (Seml-VOST) sampling emissions from 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., Hooolya, J.,  McAllister,   R.,  and McGangley, J.,  Laboratory
and  Field Evaluation  of   the    Seal-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   Isold net1c   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-
Sampling Equipment,  Research Triangle  Park, NC,  U.S.  Environmental  Protection
Agency,  March  1972,  PB-209  022/BE,  APTD-OS76,  39 pp.

5.    Schllckenrleder,. L.M., Adam,  J.W.,  and  Thrun,   K.E., Modified Method 5
Train   and  Source  Assessment  Sampling  System:     Operator's  Manual,   U.S.
Environmental  Protection Agency,  EPA/600/8-85/003,  (1985).
                                   0010 - 34
                                                          Revision
                                                          Date  September 1986
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6.   SMgehara, R.T., Adjustments 1n  the  EPA  Nomography for Different Pi tot
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 Commercially Available Instrumentation for th«
Measurement of Low-Range Gas  Velocities,  Research  Triangle  Park, NC,  U.S.
Environmental  Protection Agency,  Emissions  Measurement Branch, November 1976
(unpublished  paper).
                                    0010 - 35
                                                           Revision
                                                           Date   September  1986
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                           METHOD 0010, APPENDIX A

                     PREPARATION OF XAD-2 SORSENT RESIN
1.0  SCOPE AND APPLICATION

     1.1  XAD-2 restn as supplied  by  the  manufacturer 1s Impregnated with  a
bicarbonate solution to Inhibit  mlcroblal  growth  during  storage.  Both the
salt solution and any residual extractable monomer and polymer species must be
removed before use.  The resin  1s  prepared  by a series of water and organic
extractions, followed by careful drying.


2.0  EXTRACTION

     2.1  Method l:  The  procedure  may  be  carried  out  In a giant Soxhlet
extractor.An all-glass thimble  containing  an extra-coarse frit 1s used for
extraction of XAD-2.  The frit  1s  recessed 10-15 « above a crenellated ring
at the bottom of  the  thimble  to  facilitate  drainage.    The resin must be
carefully retained  1n the extractor  cup  with a glass-wool plug and stainless
steel screen because It 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 In a beaker,
rinse once with Type II water, and
discard.  Fill with water a second time,
let stand overnight, and discard.

Extract with h^O for 8 hr.

Extract for 22 hr.

Extract for 22 hr.

Extract f6r 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-I  contains about 500 g   of finished XAO-2.  Any size may be
constructed; the  choice  Is  dependent   on   the  needs of  the  sawpUng programs.
The XAD-2  is held under  light  spring tension between a pair  of coarse and fine
screens.   Spacers under  the bottoa screen  allow for even distribution of clean
solvent.   The three-necked  flask should be of sufficient size (3-liter In this
case) to hold solvent
                                 0010 - A - 1
                                                          Revision      0
                                                          Date  September  1986
-------
Figure A-l. XAD-2 cleanup extraction apparatus,
                 0010 - A - 2
                                          Revision      0
                                          Data  September 1986
-------
equal to twice the dead  volume  of  the  XAO-2 canister.  Solvent Is re fluxed
through the  Snyder  column,  and  the  distillate  Is  continuously cycled up
through the XAO-2 for  extraction  and  returned  to  the  flask.  The flow is
maintained upward through  the  XAO-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  It  Is  very  difficult to cycle
sufficient water tn this mode.  Therefore the aqueous rinse Is 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/nln.

          2.2.3  After  draining  the  water,  subsequent  methyl  alcohol and
methylene chloride extractions are carried  out using the refluxlng 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 metnanol and methylene chloride.


3.0  DRYING

     3.1  After evaluation of several nethods  of removing residual  solvent, a
fluldlzed-bed technique has proved to be  tht fastest and most  reliable drying
method.

     3.2  A simple col nan with  suitable  retainers,  as  shown  In Figure  A-2,
will serve as a satisfactory column.    A  10.2-a  (4-tn.) Pyrex  pipe 0.6  m  (Z
ft)  long will hold all of the XAO-2   from tht extractor  shown In  Figure A-I or
the  SoxhUt extractor,  with  sufficient  space   for fluldlzlng  the bed  while
generating a minimum  resin  load at the exit  of  the  column.

      3.3  Method  I;    The   gas  used   to  remove the  solvent   1s   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 voluaes 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-In.) copper  tubing, colled to pass through a heat source.   As nitrogen  is
bled  from  the cylinder,  It  Is vaporized   In the heat source and passes  through
the  column.  A convenient   heat   source   Is  a   water bath heated froa  a  steam
 line.   The final  nitrogen  temperature should only be wan to  the touch  and not
over 40*C.   Experience  has  shown  that  about  500 g   of XAO-2 nay be  dried
overnight  by  consuming a full  160-liter cylinder of liquid nitrogen.

      3.4   Method  2;   As  a  second  choice,  high-purity tank nitrogen may  be used
 to dry  the XAO-2.   The high-purity nitrogen must first be passed through  a bed
                                 0010 - A - 3
                                                          Revision
                                                          Date  September  1986
-------
Uquitf Nlffvf
   rfindi
  (1101)
       Figure A-2.  XAD-2 fluldlzed-bcd drying apparatus.
                         0010 - A - 4
                                                  Revision      0
                                                  Date  September 1986
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of activated charcoal approximately 150  ml  In  volume.   With either type of
drying method, the rate  of  flow  should  gently  agitate the bed.  Excessive
flu1d1zat1on 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 resTiJual
extractable organlcs are >20 ug/ml by  TCO analysis or the gravimetric residue
is >0.5 mg/20 g XAD-2 extracted.   (See also section 5.1, Hethod 0010.)

     4.2  Four control procedures are used  with  the final XAD-2 to check for
(1) residual methylene chloride, (2)  extractable organlcs (TCO), (3) specific
compounds of Interest as  determined  by  GC/MS,  as  described In Section 4.5
below, and  (4) residue (GRAV).

     4.3  Procedure  forresidual methylene chloride;

          4.3.1  Description:  A 1+0.1-g sample of dried resin 1s weighed Into
a small vial, 3 raL   of  toluene  are  added,  and  the vial 1s capped and well
shaken.  Five uL of  toluene   (now containing extracted oethylene chloride) are
Injected Into  a  gas  chronatograph,  and  the  resulting  Integrated area 1s
con^ared with a reference standard.  The reference solution consists of 2.5 uL
of methylene chloride (n  100  ml.  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  chroma tog raph  conditions  are  as
follows:

               6-ft  x l/8-1n.  stainless steel  column containing 101 OV-101 on
               100/120 Supelcoport;

               Helium carrier  at 30 mL/mln;

               FID operated on 4 x  10'11 A/eV;

                Injection  port  temperature:  250*C;

               Detector temperature:   305*C;

                Program:   30"C(4 m1n)  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.l-g  staple  of  cleaned,  dried resin  is
 weighed into a precleaned alundum  or  cellulose thimble which 1$  plugged *Uh
 cleaned glass wool.   (Note that  20  g  of  resin will  fill  a thimble,  and the
                                 0010 - A - 5
                                                          Revision
                                                          Date  September 1966
-------
resin all!  float out unless well  plugged.)   The th liable containing the resin
is extracted for 24  hr  with  200-ml  of  pesticide- grade nethylene chloride
(Burdlck and  Jackson  pesticide-grade  or  equivalent  purity).    The 200-mL
extract 1s reduced  1n  volume  to  10-mL  using a Kuderna-Oanlsh 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  TCQ extracted from the XAO-2.  This
is equivalent to 10 ug/g of TCO In the XAO-2 and would correspond to 1.3 mj 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  oL  reduced to 10 ml) in a
similar manner.

           4.4.2  Experimental:  Use the  TCO  analysis conditions described in
the revised Level  I manual  (EPA 600/7-78-201).

      4.5   GC/HS Screen:    The  extract,  as  prepared  In  paragraph 4.4.1, Is
subjected  to GC/HS analysis for each  of the Individual compounds of Interest.
The GC/HS  procedure  Is described  1n Chapter Four, Method 8270.  The extract Is
screened at the MOI of   each  compound.    The  presence  of any confound at a
concentration >25  ug/mL  In the concentrated  extract will require the XAO-2 to
be recleaned by repeating  the methylene chloride step.

      4.*   Methodology  for  residual gravimetric  determination:   After  the TCO
value and  GC/MS 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
methyl ene   chloride  again until It   Mets  this criterion.     This  level
corresponds to  25  ug/g  In  the   XAO-2,  or  about   1.25 wg  In a  resin charge of
130 g.
                                 0010 - A - 6
                                                          Revision      0
                                                          Date  September 1986
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                           METHOD 0010,  APPENDIX 8

              TOTAL CHROMATOGRAPHABLE ORGANIC MATERIAL ANALYSIS


1.0  SCOPE AND APPLICATION

     1.1  In this  procedure,  gas  chromatography  Is  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.    Oata obtained using this procedure
serve a twofold purpose.    First,  the   total  quantity   of the lower  boiling
hydrocarbons In the  sample  Is  determined.    Then  whenever the  hydrocarbon
concentrations  in   the   original   concentrates   exceed   75   ug/m3,   the
chromatography results are reexaolned  to  determine the  amounts of individual
species.

     The extent of  compound  Identification  Is  limited  to representing  all
materials as normal alkanes based upon comparison of boiling points.  Thus  the
method  Is  not  qualitative.     In   a   similar  manner,  the  analysis   ts
semiquantitative; calibrations are prepared using  only one hydrocarbon.  They
are replicated but samples routinely are not.

     1.2  Application;  This procedure  applies   solely   to the Level 1 C7-C16
gas  chromatographlc  analysis  of  concentrates  of  organic  extracts,  neat
liquids, and of LC fractions.     Throughout   the  procedure, It is 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  Is   of   the  order  of  77  uV-V-sec-uL/ng   of   n-h*ptane and 79
uV'sec-ul/ng of  n-hexadecane.     Tht   Instrument  Is  capable  cf  perhaps one
hundredfold greater sensitivity.   The   level   specified  here  1s sufficient for
Level  1  analysis.

      1.4  Detection jtmlt;   The detection   Unit  of  this procedure  as written
1s 1.3  ng/uL  for a I   ul  Injection of  n-decane.  This limit  is  arbitrarily
based  on  defining  the  minima  detectable  response  as 100 uvsec.   This Is an
easier operational definition  than defining  the  minimum 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 in
      the specified boiling ranges and  thus  will  not bt reported,  and/or  (b)
                                 0010 - B - 1
                                                          Revision
                                                          Date  September  1986
-------
    will  not  elute from the  col nan  at  all   and  thus Mill  not be reported.
    Consequently,  the organic content of  the  sample  as reported 1s  a lower
    bound and should be regarded as such.

          1.5.2  Calibration   limitations:      Quantltatlon    1s   based   on
    calibration with n-decane.  Data  should   therefore be reported as, e.g.,
    mg C8/mJ  as n-decane.  Since  response varies linearly with carbon number
     (over a wide range the assumption  nay  Involve a 201 error), It is clear
     that heptane (C7) detected In a  sample and quantltated as decane  will  be
    overestimated.  Likewise, hexadecane (C16)  quantltated as decane  will  be
     underestimated.  From previous data,  It   Is estimated the error involved
     is on the order of 6-71.

          1.6.3  Detection  limitations:     The   sensitivity  of  the  flame
     tonlzatton detector varies from compound to compound.  However, n-alkanes
     have a greater response than  other  classes.   Consequently, using an  ri-
     al kane as a callbrant and assuming equal  responses of all other compounds
     tends to give low reported values.

2.0  SUWARY OF METHOD

     2.1  A aL aliquot  of  all  10-mL  concentrates  Is  disbursed for GC-TCQ
analysis.  With boiling  point-retention  time and response-amount calibration
curves, the data (peak  retention  times  and  peak  areas) are Interpreted by
first sunning peak  areas   In  th«  ranges  obtained  fro*  the boiling point-
retention time calibration.  Then, with  the response-amount calibration curve,
the area suns are converted  to  amounts  of  material  In the reported  boiling
point ranges.

     2.2  After the  Instrument   Is  set   up,   the boiling point-retention time
calibration   Is  effected   by  Injecting   a  mixture  of  n-C7  through  n-C16
hydrocarbons  and  operating   the   standard  temperature  program.   Response-
quantity calibrations  are  accomplished  by   Injecting n-decane in n-pentane
standards and performing  the  standard  temperature program.

     2.3  Definitions
          2.3.1  SC:   Gas chromatography or gas  chroma tograph.

          2.3.2  C7-C16 n-alkanes:   Heptane through  hexadecane.

          2.3.3  GCA ttmp«r»tur« program:  4   «1n isothermal  at 60*C,  10'C/mln
           2.3.4  TW  temptratur*  program:      5   «1n  Isothermal   at   room
      temperature, then program from 30*C to 2SO'C at 15'C/nln.


 3.0  INTERFERENCES

      Hot applicable.
                                 0010 - B - 2
                                                          Revision
                                                          Date  September  1986
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4.0  APPARATUS AND MATERIALS

     4.1  Gas chromatooraph:  This procedure  is  Intended for use on a Varlan
1860 gas chromatograph, equipped  with  dual  flame tonlzatlon 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  Hellua:  Minimum  quality  1$  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.

          4.2.2  Air:  Zero grade 1s 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 lot* bleed
during  the temperature program.    An  appropriate  septm Is Supelco Mlcrosep
138, which  1s  Teflon-backed.    If   septu»  bleed  cannot  be  reduced  to a
negligible level, It   will  be  necessary   to  Install  septua swingers on the
Instrument.

     4.5  Recorder:  The  recorder  of  this procedure  oust be capable of not
less than i mV full-scale display, a   1-sec time constant and 0.5 1n. per rain
chart rate.

     4.6  Integrator;  An Integrator   Is  required.   Peak area measurement by
hand 1s  satisfactory  but  too  time-consuming.    If  manual  integration is
required, the method of  'height  times  width at half height'  Is used.

     4.7  Columns:

          4.7.1   Preferred column:  6  ft  x  -1/8 In. O.D. stainless  steel column
     of 101  OV-iOl on  100/120 mesh  Supelcoport.

          4.7.2   Alternate column:  6 ft x  1/8 1n. O.D. stainless  steel column
     of 101  OV-1  (or other silicon  phase) on  100/120  mesh Supelcoport.

      4.8 Syringe cleaner;   Hamilton   syringe  cleaner  or equivalent connected
 to a suitable vacuua source.


 5.0  REAGENTS

      5.1  Pentanet  •DIstllled-ln-GUts' (reg. trade«*rk) or "Manograde"  (reg.
 trademark)  for standards and for syringe cleaning.
                                 0010 - B - 3
                                                          Revision
                                                          Date  September 1986
-------
     5.2  Hethylene  chloride:     "DIstllled-ln-Glass"  (reg.  trademark)   or
"Nanograde" (reg. trademark) for syringe cleaning.


6.0  SAMPLING HANDLING AND PRESERVATION

     6.1  The extracts are concentrated  tn  a  Kuderna-Oanlsh evaporator to a
volume  less than 10 mL.  The concentrate Is then quantitatively transferred to
a  IQ-irL volumetric flask and diluted to  volume.   A 1-mL aliquot Is taken for
both this analysis and possible subsequent GC/HS 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  1s started, return that sample  to  the sample bank and take the next
sample.


7.0  PROCEDURES

     7.1   Setup  and   checkout:    Each  day,   the  operator  will  verify the
following:

           7.1.1  That   supplies  of    carrier   gas,   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  gas  flow rate Is  30  + 2 mL/ra1nr the  hydrogen
     flow rate  Is  30 + 2 mL/nln, and the air flow rate~1s 300 * 20  mL/mln.

           7.1.4  That  the electrometer 1s  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 1s
     effected by placing  the  soap  babble  flow  meter  Inlet  tube aver the
     injection port adaptors),  and that no  septum  will be used for more  than
     20 Injections.

           7.1.7  That  the  Ust  of  samples  to be run 1s ready.

     7.2   Retention time 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 - B - 4
                                                          Revision
                                                          Date  September 1986
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                   NBP *C
           Reporting Range,*C
                   Report As
n-heptane
n-octane
n-nonane
n-decane
n-undecane
n-dodecane
n-tHdecane
n-tetradecane
n-pentadecane
n-hexadecane
 98
126
151
174
194
214
234
252
270
288
 90-110
110-140
140-160
160-180
180-200
200-220
220-240
240-260
260-280
280-300
C7
C8
C9
CIO
Cll
C12
C13
C14
CIS
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., Pol/science Kit) containing bottles of mixtures of selected n-
alkanes which may be combined to produce a C7-C16 standard; or (2) use of
bottles of the  Individual  C7-C16  alkanes  frosi  which accurately known
volumes may be taken and combined to give a C7-C16 mixture.

     7.2.3  Procedure for retention  time  calibration:  This calibration
Is performed at  the  start  of  an  analytical  program;  the mixture 1s
chronatographed 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 Is
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  tht  1nst
     temperature for five mln.
           7.2.3.7  Shut  tht oven door.
                  nt  to  run  Isothermally  at room
           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
     1s
                            0010 - B - 5
                                                     Revision      0
                                                     Date  September  1986
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7.3  Response calibration;

     7.3.1  For the purposes  of  a  Level  I analysis,  response-quantity
calibration with n-decane is  adequate.    A  10-uL volume of n-decane  1s
injected Into a tared 10  ml  volumetric  flask.   The weight Injected  1s (
obtained and the flask  1s  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 Is 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  callbrat jn:    This  calibration  1s
performed at the start of   an  analytical progran 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 In  the refrigerator  locker and are made up monthly.

          7.3.2.1  Verify that the Instrument Is  set up properly.

          7.3.2.2  Set  electroMter at 1  x  10-1°  A/aV.

           7.3.2.3   Inject I uL of the  highest concentration  standard.

           7.3.2.4   Run  standard  temperature progran 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
      £51.


 7.4  Samjle analy t1s procedure•.

      7.4.1  The following apparatus Is required:

           7.4.1.1   MS chrautograpn 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  Is  1 * 10-1° A/mV,-
      recorder 1s set at 0.5 In./mln and 1 aV full-scale.

      7.4.2  Steps In the procedure are:

           7.4.2.1   Label chromatogram with the data, sample number,  etc.
                            0010 - B - 6
                                                     Revision
                                                     Date  September 1986
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               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.

               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  F111 pi pet with pentane; run pentane through syringe.

          7.5.4  Repeat with nethylene chloride fro» a  separate plpet.

          7.5.5  Flush  plunger with pentane followed by methylene chloride.

          7.5.6  Repeat with  nethylene chloride.

     7.6  Sample analysts decision criterion;   The  data from the TCO analyses
of organic extract and  Hnse  concentrates  are  first  used to calculate  the
total concentration of C7-C16 hydrocarbon-equivalents (Paragraph 7.7.3)  in  the
sample with respect to the voluM  of   air  actually sampled, I.e.,  ug/m3.   On
this basis, a decision  Is Bade  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  ufl/m3  —  4  TCO  of less than 75 ug/ra3 will
require only 1C fractlonatlon and gravlMtrlc determinations and IR spectra  to
be obtained on each fraction.  If  the  TCO Is greater than 75 ug/m3, 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
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          7.7.1.2  Plot  average  retention  times  as  abscissae  versus
     normal  boiling points as o nil nates,

          7.7.1.3  Draw In calibration curve.

          7.7.1.4  Locate  and  record  retention  times  corresondlnq to
     boiling ranges 90-100, 110-140,  140-160, 160-180, 180-200, 200-220,
     220-240, 240-260, 260-280, 280-300'C.

     7.7.2  ftesponse-UDOunt calibration:    The  required  data  for this
calibration are on the  chromatogran  and  on  the  data sheet.  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  (uv-sec)  as  ordlnate  versus ng/uL as
     abscissa.

          7.7.2.3  Draw in the curve.    Perfora 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 chroaatograa and on the data sheet.  The data
reduction 1s performed as follows:

          7.7.3.1  Sua 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  (uY*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 1n  the sample.

          7.7.3.4  Using the  voluM of  gas saapled or the total weight of
     sample  acquired,  convert the  result of  Step 7.7.3.3 above to ug/n3.

          7.7.3.5   If the  value  of   total   C7-C16 hydrocarbons  front Step
     7.7.3.4 above  exceeds   75   ufl/i3,   calculate  Individual  hydrocarbon
     concentrations In  accordance with   the  Instructions   In Paragraph
     ' • ' t V . V 419 I WW .

     7.7.4   Individual C7-C16 n-Alkane  Equivalent Analysis:   The  required
data fro* the analysts are  on  the  chroMtograi   and on the data  sheet.
The data reduction  Is performed  as follows:
      ranges.
7.7.4.1  Sun the areas of  peaks  In  the proper retention time
'i.
                            0010 - B - 8
                                                     Revision
                                                     Date   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
          sampje acquired, convert the result of Step 7.7.4.3 above to ug/rn3.

8.0  QUALITY CONTROL

     8.1  Appropriate QC Is found  In  the pertinent procedures throughout the
method.


9.0  METHOD PERFORMANCE

     9.1  Even relatively comprehensive  error  propagation analysis Is beyond
the scope of this procedure.   With reasonable care, peak area reprodudblltty
of a standard should  be  of  the  order  of  IX  BSD.   The relative standard
deviation of the sun of all peaks  In  a  fairly complex waste sight 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 10-201.


10.0  REFERENCES

1.   Emissions  Assessment  of  Conventional  Stationary  Combustion  Systems:
Methods  and  Procedure   Manual   for   Sampling  and  Analysis,   Interagency
Energy/Environmental   R&O   Program,    Industrial   Environmental   Research
Laboratory, Research Triangle Park, NC 27711, EPA-600/7-79-Q29a, January 1979.
                                 0010 -8-9
                                                          Revision
                                                          Date  September 1986
-------
APPENDIX J.5



CEM AND GC
-------
W. M.
II
flantptlna equkpRNnM   f-nvlronmrMal  Pro
Uwlton Atm-p  Rraratrh Tilaiiflr  I'aik
M <; APTU Ml*  March, ini
  4 Snlth. W  a,. R  T  Rhlarriara. and w
P To*!  A M^hod o<  Inirrpertfc* mart
Oakapnrn  DeOa Papr* Prevented at Ihr tin!
Anrmal Meelkaa,  of thr  Ah ndlullan Can
Ual AakBClkittcni.  81. Louie Mo June If I*.
          40 CM Cli. I (7-1-19
  Ihr  maroi orguiir rofnpnnrnM ol  a B.M
mliluir arr tr|i*iair  «tl«T>  and indl«Mu>llr ouant ilfc-d by
Ilkmr lonbwllon. plmliiinnrullim. rlrrlum
r«p4uir  or  o4fi*f  BinunfHldn  drln Ihm
     kHPi, W. B. el al. Star* Uuflantpilna:
         •nd  ttkaeptlfepd with  Mr* Equb>
•eml AFCA Patter Mo. •) lit IM1.
 • efeectftaoJloaa tar InctnrraUw Tmlng at
•tedMVl PfcrMUtw  PHfl HCAPC. IMT.
 1.  Bhatrhara. R. T..  Adtaataenf*. hi tie*
IPA HHeauantiii  lot OMfemtl Pilot Tot*
            and  Orp  Molecular  WHaMa
                   i  1:1 II, October, l»1«.
 •  VaObro.  R  P. A Dvrcp of fmmiiilil
  Tlie  relrnllon llnm  ol  rarh
roenponrnl  are  iianparrd wllh  I how  ol
known mmpoulMkt undri  Idrnllral romM
liana  Therelore, the analm ronflrnk  Irw
ktrntllp and approilamlr> ronrrnirailon* ol
                                                   WHti Ihbj inforaMlton.  Ine tnalril
                                                     pare*) or purchaae*. njaMiinrMlp
                                                     kt*ndard mlktorea (a calibrate the
                                                                 ideniicaj to tr
                                                         The Hkllrai
                                            UH n«d l«r ••Bit dftaUm lo «TO*
llw« II IndHa to TTnrmr*—  U8
                  Acmrr,
              ch  llmairh Trbui«kF Put
                                                        far a
                                                          d»
                    UctmbK oonmrtrkUon of lhal romvound, or
                    UM conecnbvUon thai producaa a kbjnaj la-
                          ralto of Uirv* 10 onr. Tke
                                                   UK  pi«a»iii> eaUbraunn lot  each
                   Thto BkHhod appllca lo
                             H |)en»m of
                          riaMtod Itrmm an
                  II doe. not tattude Mch
                                            I ProrMoaaa
                                              Oaa ctiroaMtlaanpnlc ucfinlqikN IpptcaJlp
                                            provide • iiikifcdiii of I to I* percent rela-
                                            tive kUndard dewbuion (RBDI. bat an ekp*
        	will not  drteneilnr
      I thai lit are polpvoeikr (hhjh moknru
ku weajhl). ill can potrwrbv brforr anajp-
eta. or III have »rr> lo* .apoi prrvwrc-a ml
•lark, or tnaUiiaMnl condliloni
  I I  Prtnrlpfe
                      tai
                    •MMnlpenenM of Inetr i
                      ibl Aocwrae?. AnoJpaki "***• ol prepared
                                 are vHhbi I* pcrnnl of prep-
                    araUnn
                    « ImUrftr
                      neaoluUan  knte*lcrtnee«  lhat Map  occur
                    can  be  eWaJnated  bp appraprlaU  OC
                    coluMn  and dtetoetoi  chelre or bp ahllllm
                    the ralentlon thaai ihrouch changa l« lh*
                    cotunut  Ho*  ran and Ihr  uar ol Umpe««

                      The analrtlceJ arMtn k>  dmonatrated  ">
                    be aecrnlbdlp free fraea nmUoibianU t>T P*
                    rtodhnllp  analpllrtf Muikj thai conibit  »'
                    hpdrnrartoon free kjr or nHroirn
                      Hwnplr  ritmm conlamlnallon  lhal  off""
                    mhtn high l*»rl uul  tow Irvrl tmmirlr*  *"
                              krr analrvd alUrnalrlr. I" *K"1'
                                                                                              drill ollh bp Ihorouth puribifj ol Ihr (1C  trhkrroal.  Tmaji. HAD I rtc I loe
                                                                                              kampfe loop brlarrn aunpkra.                trj camplra
                                                                                                To aanii* romhrtrnl drtertor raepoiaM.    kill  Pvraonnel MaiapHn«  Pueap
                                                                                              rallbrallon iaan are conialnrd In  dry al«   brated. lor rollrrlltia adknrtarnt urbr i
                                                                                              To adhMI caBrous ovianhr roncvnlrallonk  >rp mmplra
                                                                                              •hrn emter rapor la ptnrnl to Ihr OMMpV.    B I |l  nthnlen  BpUn*  CalHnlrd  the
                                                                                              «ter  rapor conrrntrallor. arr drtan.dncd  Ahjllon kpabn« b> to be comtrvrted follow
                                                                                              lor I hoar  umpire, and a rorrerilon fartor b)  bMj  the  kprrlllralloni of  an  acrmUMr
                                                                                                                                   lo br
                                                                                                                               of iht In-
                                                                                   aa1 Prriaror* San
                                                                        rVrlnrm a niraurwr lor rath
                                                                       inlrd. Rvlrr la Flaw* II I.
                                                                       hxriullon can br collcrlcd
                                                                       tarrrn and mm srimmtt Oollccl «a>
                                                                       •unptea IhM ran be analnnl lo con'tra* Uw
                                                                                                                                                     Can
                                                                                                1.1 I* flMpk Probrk Pjrei or kUhileaa
                                                                                              •*rt of kBlla-irnl Irncth lo reach cmtmld
                                                                                              ol ilark. a* a point no rioarr to Ihc  waJIk
                                                                                              titan lai.
                                                                                                I I » Barometer To
                                                   ol the OTBanlr r»Ua1iik>                       11 I  Oriootard rtWOkd Water
                                                    II  Apfawklua  Thfcj apparaUai tlat  aan     III  Mrthplmr iNcbtekle.
                                                   applla to Srrtlom • aod \                      in  Cadlbntlon flaota A kerlea ol atand
                                                    III  Teflon TtiOkMf (MenUon of Indr   ankt prrparrd lor ernip rrmipoMnd of Inter
                                                   nanea or apMifk produrte doea not oonaU    ert.
                                                   lute tiidi»oninitl bp Ihe  U.B biebonn«ti      lit  Orranlr CoMBOHnd Oohitbana. Pare
                                                   Ul  Protection  Afcnip I  OfewaeHrr   and   IM>I peranmi. or mm pure mm an iraaniiklili
                                                   krnfth  drlcrakknrd  bp, tonnrtllon rewulrt    be obutned  Hquhl kanMpiee of an the organ
                                                   avntf of cpllndcr rvcnlaton and Ihc  OC    br curapoundi nrrdrd lo prepare callbraieon
                                                   AddHlonal Ivbeng Ik mttmmti  to connect   atandafd*
                                                   theOCaB»pkf looploUktatkajIr.              an  eT.lrarllon antoenu  »»r ealronion
                                                    111  Oka CnronMloatwnli. OC arllli ka*a    of adaarbrml lube eamptn fen prppuMlon
                                                   bte  drtcciar,  rorueana.   tewtperal<>r*«an    for anal pah)
                                                   iroUrd akMotr  loop and valve aaaraitilp. and     | j •  Fuel  Aa rrroamendrd bp the nan
                                                   Imperative proaramablc o*m. If neneakMp    ufactum lor operation of Ih* DC.
                                                                                                Ill  Can In  Oaa  Hpdranrbon  Iree.  ak
                                                                                              PCCOMHVMVMVfl wC *n*t IBBUtMlwkClllfVV fOf 4>fV
                                                                                              erallon of Ihe drtector  and iiaaiiaiklHIItt
                                                                                              •Mr, the ca4naa«.
                                                                                                tit  Zen dak.  Hrdrvcarhoa me air  or
                                                                                                                                 blank
                                                                                              Thr «C khall achieve aeiadUvKP reawb-e
                                                                                                 114  nowakcter* To	
                                                                                                 I I.I  RrutaUm  Uaed on fa* e»Onderi   nltracrn. Is br  laird lor
                                                                       lor CH: and for cpi
                                                                        11 •  Rcfarder. Recwrdrr wkUt
                                                                       tharl  to  •Infeeniai  acoeptablr. I
                                                                       logUonalUa rirri «iriiki«
                                                                        111  oprweje*. ••eat, I •- mmmt  It aklrro
                                                                                              prrparktlan. and standard preparaUon.
                                                                                               II .Ukaejllirel.
                                                                                               Ill  CsaOrctlon  of  Sakkpv* wUi Oiao>
                                                                                                                     tp kaeapkta can be
                                                                                                iu Uihl), for prciaHfeaj ralfcraUor. aland
                                                                                                 HI  Tubin*
                                                                                               fke rplbidm.
                                                                                                 I II  BeplwBi
                                                                                                 I I I*  Ola. Jan If
                                                    ft I II  Roap Pllrn  Pto* Mrter  To drkr
                                                   Mlnr flow ratea
                                                    Sill  Tmflar Ba*a. I* and W liter tapac
                                                   H» for orrparailon ol atamkudk.
                                                    » I II  D»p Oai Meter with Teatpriklure
                                                   •nd Piewnre Oautea. Ac«uta*r to  I 1 per-
                                                   «in. rot verparat tan of mm* Mamkirdk
                                                    > I M  Hk%r|   Imptmrr/llol  Plate  Ak
                                                   wnhlir Por prrparillon al mmm iLandaiito
                                                    1 I 15  fJampte Ptekk* Knr prrkurvfy iam

                                                    1 I !•  Ad*ot»iloii   Tiinri  II mi i•»11
                                                   *>li»li  luhn lllir.l «l	r.-rw*ir ukutrbriil
                                                                                                                                         llaai  aamplhn  fMaftj. Teflon  kiopoockA
                                                                                                                                         wlthoul jKaai. tire pnrlerred  Pkawu abould
                                                                                                                                         br cleaned at fatlom flcwwvr I
                                                                                                                                         froca bath endk of in* fladka. i
                                                                                                                                             i to remove anp frewat. data tne t
                                                                                                                                                  reb. and recetven w«h avthp
                                                                                                                                                   CVanafl a«k
                                                                                                                                         •BhMlon. Uten itoae «IUi Up I
                                                                                                                                         dbUlled  water  Plan the
                                                                                                                                         ajiea anneaMn* fiunace and applF heal up
                                                                                                                                         lo HO  C. Maintain at Ihlk lii»o»itl«rr for
                                                                                                                                         I hour Alter lhai lime period, khM off and
                                                                                                                                         open trie fuinacr la aHov Ihc naak lo cool.
                                                                                                                                         (irtw the anocacm* vrtUi atopnocfc
                                                                                                                                         uid rrlurn  Ihvm  lo the
                                                                                                                                         Purtr Ihr uerftablr with hkfh purttr nllro
                                                                                                                                         mm tar  I to 9 miiHiin  Clnar off  "•* •***>
                                                                                                                                         rarm*  alter  putilnc  lo maintain  a tllthl
                                                                                                                                         pmlllrr  nitrogen prnwirr Brcur*  Ihe ilop
                                                                                                                                         rnrkj with lapr
                                                                                                                                           P>riur*rp eamulra ran be  obtained ellhct
                                                                                                                                         br 'lr.»ln«  Ihr (un  Inlo thr prolowlr
                                                                                                                                         r«u-uilrd Hack (it br dr»ln«  Ihr «aon Inlo
                                         868
                                                                                                                                      HA a
-------
 ft. oO. App  A,
                         II
 and purging Ihe flas* »Mri a rubber iiK-liun
 bulb
   ft 1 I I  Evacuated r'lu«s Piorrdiirr  llw «
 high vacuum pump I" rvsi-uale llir lluk lo
 llir rapacity of the iMimu. thru rlue nil llir
 stopcock leading  l» Iht pump Attach a I
 mm outside dUmelrr lOUl glass tee lu llw
 flask  Inlet with  a short piece of Tel Ion
 tubing Belect • ••mm OD boraalllcale sam
 pllng prate, enlarged al one end In a 11 mm
 Oil and ol mfftelenl length  lo leach  Hi*
 ceniroM of the duct lo be aamplrd  Inacrl •
 glass moot  plug In Ihe enlarged eiul of  IM
 prate lo remove pankulale mailer. Attach
 the other end of Ihe prate to the tee .llh •
 short  piece ol Tellon tubing Connect  a
 rubber auction bulb lo Ihe Ihlrd leg of  UM
 tee Place Ihe filter end of Ihe prate at  Ihe
 cenlrotd of the duct, or al a point no closer
 to  Ihe .alls lhawt  I m, and purge the probe
 •llh Ihe rubber  suction bulb.  After  the
 prate  to completely purged and filled .lib
 duct gaaca.  open  Ihe sbipcock la the giab
 fssaa until the pressure In the flask reaches
 doct pnsaurt. Close  oil the stopcock, and
 remove Ihe prate fraaj the duct. Remove
 the tee Iron  the  lists and  tape  Ihe  stop
 cocks  to  prevent   teaks  during  shipment
 Measure and  record  Ihe  duct  temperature
 and) pressure
  B.I. 1.1 Purged  Plaak Procedure. Allarh
 one end of  the sampling  flask to a rubber
 suction bulb.  Allach  Ihe  otter end to a ••
 mm OD glass probe at drwtlted In Section
 S J.1.1. Place the filter end of Uir  prate at
 the cent road of Ihe durt  or al a point no
 r-loaer to Ihe sraJU lhan I  m,  and apply suc-
 tion srllli the  bulb lo rumpielfly purge the
 probe  and flask  After  the flags  has  been
 purged, cuse oil the stopcock near the sur<
 Hun bulb, and then cloae Ihe stopcock near
 Ihe probe. Remove the prate from the duel,
 and disconnect both the probe and suction
bulb Tape Ihe atoprnrk* lo prevent leakage
during shipment  Measure and record Use
durt temperature and pmaura,
  b.l.I  PVilnle Bag Procedure  Tedbar or
 alununtard  My tar  bags ran also he  used to
 obtain tte prcsitrvey sample. Use nrai  bags.
 and leak check Iheat before field use. In ad
dlllon. check  Ihe  bag before use  for con.
 lamination by filling II .llh nitrogen or air,
 and snalnAng in* gas by OC al high i
      aUperlrnoe Indfcrates thai II Is i
                                                            .a Ch.
                                             (•ill in
                                                       HU
                                                                    * In ilrli-imliir (hr
Me to allow the Inert •• u> remain U> tme
bag about  M hour* or longer la check  tar
deanrptloji of organta from Ihr bag. r\tlto%
In* leak check aad mmvte coHectkon proee-
dutca glten ta Brcllon f. I.
  ••I.*  netenntaiatlon uf liolilure Conlent.
r\M ranbuaUon or vain coitlialkn! praccoi-
n. nbtarn the moWurr rontrnl  from planl
peraonnel  or by fMruurrmrnl  durta^ the
preaurvei. II Ihr  mtun'r  is brlnv W C,
meautre the w»i bulb nxl dry bulb Irmprra-
lufft*, and ukulair Uir molitliirr ranlpnt
tulng • nrrhroiarlitc rlurl Al liialirr lem-
  44  llrlrrinlii*lioii  »l  Slmln
 ItblBlii llir alalH- inriwuir I«IMII
 IwiMMiiirl or m*a!ciifrinr"iil  H
 lulr Bird an huhiird nianomrter are tued,
 lake rire lo align llir |>ll»l lubr  tO' Iram
 llir  tllrifllon ol llir floiv. ItlaruiiiH-rt our ol
 llir  lutes to Ihe manomrln  •nd  read Ihe
 alsllr prrjaure; note vhelhrr llw rradli^ ti
 pobltlvt or n»i»Vli*
  & $ t'nllertlon ol Prmurnrir Kamitlrs Blm
 Adaorpi lun Tubr follow Brrlhm 1 * l«i nir
 uirvet iiaropllng .
 • Mmaliau Itrvrlupmrnt
  • I eeierllonul CM: P»r«melrr»
  • I I  Column I'tiotrr Kurd on Ihe InMlal
 contact atlUi irfant prrattnncl ronrrrning the
 plant p-ocra* and Ihe anllrlj>Bl«d rmlkmlum
 chocae  I column lhal pmtldes guod rnolu
 lion  an I rapid analysts lime. The rliolce ol
 am apptopflaie rohunn rsji be aided by a III
 rralure search, conlart «Mh manufarlurrn
 of UC loliBBni. and dfaeusalan millh person
 nrl si tite eraawkm SDUTCT
  Moal  eohnnri aaamifaeturen  keep eieel-
 lenl  reiords of Ihrti Broducts. Tneli terhnl-
ral srrvtcr departments sway be able to rec
omcnrnl appropriate columns and detector
type far  aepatallng  Ihe anHdpabrd com-
pounda. and they may be able to provide In
 formalin on ntiffferenrca, optimum off
al Ing c* ndMtona, and cotumii Itmlialioiia,
  KTsnln with  analyltcal laboralorlem  nisy
also  be. able lo provide Infnrmalloii Lsjtdards and cniumn oMalned1 in Sec
lion  • I I. perform InMlal teats tu determine
appropriate OC romfllUms  thai  providt
good feiiolullon ami mlntmym analysis lime
lor Ihe ijompounds ol Interest
  • I 1  Preparallon of ft«ur»ey Bampsta.
If Ihr lUBpkm »ete coJIecUvl on an adsorb
ent,  ealracl the aample *a recommended by
the  twsiiufacturer for removal of Ihe euro
pounds *tth a aolvefM auttablc  to liie type
of OC analyakt. Prepare other aamplea in an

  f.l.i  Prraurvey  Sample Analyiis  Beforf
analysis, heal the preauney sample to the
duct tmiperature. to vaporise any condensed
material.  Ajialyie the aamplei  by  the OC
procedure, and compare the retention limes
against those  of  the  calibration  m«mp»n
thai contain the rufaponenU eiperted lu be
sn the ilrrafo  If any cosnpoundi rannol be
IdrtHllh-d wllh certainty by tills prmfrturr,
Idrnllly them by oilier rneans sucli a* tlt.V
mam apectraarapy limiit" M'lMnil*
l,B*r brrii 4lelrrmliu-il. iieilwnn rr|»sl UM'T
HLIU ul tlir SBifiuli- lo rtrirrmliir Uir  rrlrii
,1	Inir al rmrl, rimipoiMHl Tn ln»rrl  •
ssiiililr  diao itainlilr lliriHilll «" •»"«» »' •
,.,ii.ll.nl r.lr 1100 ml/ml™ I«« J» «ero«d»l
|Ir rsrrful no!  lo preasiirlse M»r ian. In «l«r
loop T«rii ull  tin- p«mp and allo« Ihr gas
In Hie sample loon l« ftwnf In amok-ill pr'"
s,ne Arll.atc Ihe sample »•!»*.  »»M| 'word
Iiiirrtton  tltiw. toop  *rw(P««U««.  column
trmpetatuir. carrier ll.iw rale, cliarl  speed,
and attemwUir setlliig Calrulale the rrlen
lion time »l rarli peak  using Ihe distance
Irom inKiii-" l« »hr P««* mailnwim dlvM
rd  by  Hie . nart  speed  Retention Utn*»
sh

typest»l'lT...roVl.rs .ml MMnmr.rlally a.all
.hli ililul	systems can alsu br used,
  C .lllx.li  each  Ihi.mrler before "*•»
placing M  hi-lafii-.i llw dllurnl gas  supply
and «iltably ulu-db«ibbte meter,
   mft tr.l nM-t«-r Hrrur.l  all dala i
Plgurr It 4  WhlN  li l> at  may
iwnluflr  It  Tin- .-ii.H Introdured  by ualial
Ihr dllue.ii  ga.v lu>  rsllbrallor. Is  Instinlfl.
i.ul fur gas nusliurs «l up lo  I.PoH IO *.mm
uurn «l earlt nrniiih- rwinponeiil
   Oner Ihr  fkwmriers are caltbraird,  con
nect the ll,,.m, n - l» ihr rallbralhin aud
diluent  gas  miinilirs  u^ng  • mm  «*«''> i:on«rr.vhipm
  X  Mule ur volume  fiaciloi: ol Ihe organic
     In tin- rahbrali«m ga.i lo be dilulrd
  d, , plo. rate ol the calibration gaa lo be dl
     luted
  q,, - tMliM-ni gas !!»• rale.
  Single stage dlluUuns should be used lo pre-
  pare callbtatlon mlslurcs up U> about I:M
  dilution ISJ-UK
    r\K grralrr  illlultuns.  a double  dilution
  system I* irnMnrnriwIed. aa Bho*n In figure
  It •  Pill the T. rtlsi bag with lite Ollule gas
  from the M-rimd clage Record Ihr laborato
  ly l^mprraliirc. bartimrtrir  i>ie*uire.  and
  Btalir pri-^ure  ti-Billnga  CTorrrcl Ihe  float
  reading '<" l.'miifralure and iMeuure. Cal
  nilslr Hi.- i utN-eiilrallon  C. in IHMH ol the
  iirisiiir "•  ">•-  linal gas mlslure  as lollo»«
  Use Hi* OC conditions itrirrtuliird by ll»-
iwocrdtirri ol Bivlluii g I 2 liu Hit  Itisl l»
•rclIon  Vsiy Ihr (It: uaiainrli'i^  diiiinf
subsequent ln|Miiuiu Ml drlrrinliH- lln- <•!•<*
                                         070
-------
                                                                                     T
 P». M, Aa*. A, MwhY II


                         6  -
               Ce  •  10   X
                                     «d
  «0 CM Oi. I (7-1-19 IdMion)


'cZ
                                                                                                                  *O,
                                                                                                                                                                 A. Mcjlkk. It
                               lqcl  *  «<«  \qt*  *  ^2,
                                                                       fo-
 Where                                      troaen through • drr la* mrlri  lhal ha«
 II* -. Convercton lo pom,                      been calibrated In a manner ronibtrnt win,
 X • Mote or volume fraction  of Ihr organic   I**  procedure deacrlbed In Section ft I.I  O|
    In the calibration gaa lo be diluted.         Method • While the bag b lining u*e a B »
  wag on a amooth  aurf ace. and al
 Volatile MaJUrrml*. Record all data ahown on   ternatelr atprata iMjjiiallr rndea of the bag
 Plgun II I                                 H Urn** la  mil the gacca Record (he aver
  • 111  Oat Intaetton  Technhpic   Thta   aa-e  Mate* lomfwratare  and fmeauw, ihe
           a  applicable-  u>  organic  com    IBB  volume and thr barometric Drmmnt,
      I thai eirnt onUrelr at a gaa al arabl    Record  the  ifrtnae tenpcraluK and prra-
rnl oandllmna.  KVaruate a IO liter Tedmr   *ure befope Infection
hag that haa pacacd a ma-cheek <•** Bee-    CatcumU  each organic atandard COIMCA-
Uonf II, andBMter bill liter* of air or nl    I ration C, m ppm a* foltowa:

                           f,     «nV C vJ   "
                           UM  • 10
                                                      .llh Ihr oriairic Plat* Ihr «»rlrnc
                                                      Inlo tfit Implnarr InIM mini Ifw arfMum
                                                      umvldrd, and ln|m I In- liquid Into lh« llo»
                                                      In Mr  rtrcam  UH • nt-tHtr of nlflclcm
                                                      Irrwth  to  W"nH Inlcdlon ol the  liquid
                                                      ortov  in*  air  Inlet  branch  ol  (he  ire.
                                                      Rcmovr Ott ivilncc.
                                                       When Ihc tn« (* tilled, Hop Uw pump, and
                                                      clow  (he ta« bilrl nln.  M
                                                      outlet, and «lhr» «H  II uldr lo.  «i leaM I
                                                      hour, or mMaflt the bai to Inrare toropl*ie
                                               Mfaiure  lh«  MiNriil liquid  dcnallf  at
                                             ruom trntMrratiiir. br arcuiaulr •etflhln« a
                                             knoMi (Olumr al Ihf material on an UMlri
                                             leal nalanr.* U> Ilir nrmittt 1.0 mllltaTam. A
                                             • round |lu» Mavpftfd M mil
                                             flu*  01  a (laai abifipercd apeclllc
                                             bolllr to ntHabtr lor «lflilna:. Calnilalc the
                                             rrauH  In term ol |/ml. Aa  an  aflctwitvc.
                                             lluralurr valon ol the dnvHr of lh« UquM
                                             U M "C may b* u«ed.
                                               Calculaf earh w«m»c Manojard
                                             trallon C. In ppm ai lolHm
                                                              ^5-
                                                                                                          (Z«.0*4  i
                                                                                                                                  «.?« i 10
                                                                                                                                                 l.P  I
                                                                                                                             fq.
                                                                          ".
                                                                          760
                                                                                                                     IOOU
                                                                                            vhcre:
                                                                                                                             .
                                                                                               Uojuld ataBnk dcnatir «a oMmanwd. •/
                                                                                                 be nmllrmrd In thr              	
                                                                                                 and analyilni callbrkUon Mandank contain
                                                                                                 bi  multifile onjanfc
                                                                                                                          al m *K
                                    "
TED

 ) t
                                           1000
    H . Moiccwmr weight of
    It MB-Ideal gaa
       and TM mm rig.
    ia>.Can*eraionU>
I   iw».Con>«i«liin II
f    •! PreparaUon  of CallbrmUari  Gurvca.
    Falatrtfctir uimici OC conaWIOBB. UMB fbjah
    the mmr"~i loot) l°* •* an""'*' al a raw of
                                                                                            IM ml/mbi Alto* UM
                                                                                            lo eoullWraU to
                                                                                            activate  Ihc bitecUoa *•!*•
•here.
O.-Oa» ralunw  IK ofcantr  rompoutnl in
    iccted, ml.
. •- Connralon lo pen
P. -Absolute prvamre of cr'!"*'  brlor* In
    (tctlon, BMM Ha
T.-AtaoluU tenperalurr ol  (irrlnic belore
    •HFCllon. K
V..CIa« *oluaH> tndlcalrd t>» di 1 «a* meter.
    Mten.
V -Drr (aa meter eallbrallon factor. dJrarn

P.- Aaaohite preBBU* of dr^ caa meter. BIB
    Ha,
T.- Abaolute tciBBCtaturr ol drr !•• meter.
    -ff.
  • 111  IJqutd Injn-llon  IVrlmlqiir  Uv
lt>r mulpmcnl ihovn In M§urr I* • (.'all
IMBU in« dry >a> mrUi  BJ Jru-ilbril In tlrr
lk*>  a | I | aillh * vrl lr>l mrlrr  <>i • ipl
      roraeter.  Vff B  vater  nanometer lor the
      pnraaure aauce and «1aaa, Trllon. hraai. or
      •UJntaB BUei for all conmctloaa. Connect a
      ralve la Ihc Inlet ol the »lit** TMUar b*t
       To prepare Ihr ilamlardi.  anrmhli'  the
      •qulpinenl  aa ihoan  In Plaure  II •. and
      leak check I he iratem. CunptrLrlr r*aru«ir
      (he ba«, PUI the  ba* vllh hrdroraibon I'tr
      air. ant nacuate the bag again. Ctoat  Ihr
      Inlri vain,
       Turn on  the   hoi plate,  and  allow  thr
      ••ter  lo reach ballln*,  Connart the baa to
      the Imp4n(*r  outlet.  Record (he Initial
      mrter lewttng. opm thr baa- Inlrl *al>r. •'•!
      oprn (he cyltndrr  Adfinl. I he rate •> thai
      Ihr ba« »lll be mnptTlrlr flllrd In appro*!
      mktrlf It mloul*«  Hrrord  mrlrr prruurr
      and Irrnprralurc. ajMt Inril bari>m*>irlr P'"s
      •urr,
       Allnv lltt  liquid orfuilr lo rqiilllbrBlr lo
      inooi U-mprralurr mil Ittr I o 01  lOmxii,
      Illrr iyilii«r (u  Ihr drilrrd lluind »iiln""
                                                                                        Qualltr  Aaauranr*  for
                                                                                        	ImaMdmtelr a/ter the prcpara
                                                                                     i  of Utc callbrallon curxa and prior to
                                                                                  (he preaurvcr aample aaalrmy the anatiram
                                                                                  audit Jrmrlcea In M CPU Part «l. Appcn-
                                                                                  dli C, Ptwwdut* * "Fwctdnr* '«* PlHd Au
                                                                                  dhMng OC Anaiyahx"  ihould be performed
                                                                                  The InlormatUm  reojulred la  document Ihe
                                                                                  analrala of the
                                                                                  rtuded on Ihe nample
                                                                                          II I and II 1
                                                                                            ._.	j the vtendard bilecUoo umUl two eon
                                                                                            atcutlve InfncUona gf*e area cownte wtthtn •
                                                                                            pemcnl  of (heir average. The avrragv ralue
                                                                                            Mulllprcd far the altenualor factor b> then
                                                                                            ihe calibration area value for Ihc oottcenlra
                                                                                            lun
                                                                                              Repeat tMa procedure lor each  nandaid.
                                                                                            Prepare a graphical plot  of eanrcnuaUon
                                                                                            i C.I venui the tUlnratlon area  value* Per-
                                                                                            form a  rtgnaalon anal raw  and  draw  Ihe
                                                                                            bail louftrea line.
                                                                                              • 4  Remit** Heapon** PacUta. The call
                                                                                            brallon  curve generated from the  BUmfcvdi
                                                                                            (or • tingle organic can uauallr or.  related to
                                                                                            rich of Ihe  Individual  OC rcapona* curvea
                                                                                            !!%•! nr developed bi Ihe  lahoraiorr lot all
                                                                                            UH- rampoundl In the  aource  In  Ih* Ikflcl
                                                                                            •laniard* lor that ringfe  ofianlr can ilirn
                                                                                            br iixil lo "calibrate" Ihr  (Ml lor  all Ihr or
                                                                                                 i prcaenl  1'hui pracrHuir  ihould Hnl
                                                                      	
                                              ihould agnc mtt.lt the audB oBnceniraUona
                                              •Khtn  II penenl  When  BnUaMe.  Ihc
                                              Icate* mar obtain audn crllndm »>r coo
                                              tartlng    UB  BwlronawoUJ  Fn*	
                                              AgewT. Oi»*m«Ben«l MonlloHag HI
                                              lAboralor*.  Qi«lttr  Aawranot   I"
                                              "10?
                                              itandarda and analriki «|Mka»enl different
                                              f torn ll.«ar >ue* lor Ihe aa* man-larlorer •
                                              aji«lMl*  Verlllrallon to eomo»«te and ae
                                               rr|H>blr  •Urn Ihr  Independrnt
                                        872
                                                                                                                                    H71
-------
  It. M, Apav A, Math  !•
 rtmrenlrallon I* vllhln A prirrnl ol Ihr lk>
 manufacturer'* conmilrallon
 t  rlnaJ S*apMa* • •** tmalrtu Pnirrdarr
   Carakferlng oilety I flame  haiardil and
 Ihe aourer aondttkon* Mtoct an appropriate
 •ampung  and analfMa prorrdur*  iSeciluft
 Till 71. or i.ii. InaMualtorv Bhrrr a hy
 dmgen Haaae to g haaard and no bHrbttleai-
 ly  amfe OC to auUabw, uae Ihe fltilble bag
 caHacUon  technique or an adaorptlon tech-
 n*»j». It the avarcc leavperaturc to brtow
 IWC, and Ihe organic cunornuaumto are
 •MMahaf for the detector to be uaed. uat the
 direct Interlace method. If the aource gaata
 require dtluUon taw a dilution Interlace and
 cither the bag- attapfe or  adsorption tube*.
 The (hotor t»la*«n thcae two teehoique*
 •III depend on Ihe phyatcal  layout of Ihe
 alie, the Baurce temperature, and the auw
 age atabtllty of Ihe covajmunda If coMeded

direct Interlacing or dUutlon Interlacmg to
prevent ammple taa* by adaufpUon  on Uw
bag
 II  Integrated Bag
                                                       40  (lorn 1'ltrii ixnllliMi ll>r
                                             mm) vu-iiiint llnrs Ini um|illiig.  knct
                                             Ilir wlnBl umpllni. trrpliic Ilir nu- i«,,
                                             p»rlk>ni I u> i|tc ilarli vrlorlly  Urn m ptnrtu
                                             linn, dlirci itir IM nliiii<  Hie  romncUi
                                             *•>•? It m Mjnplliic |>rr*n«n«'l Al Ihv rnd
                                             ol  ihr  i«mpl« prilod, ihul  oil It if pun>n
                                             dUroiuvcl  IHc Mmiilf  tin*  IIMM ittr b*«
                                             •nd dtamnneci me  ••cuum  line liom uW
                                             bad ciaiWInei, RecoM the lourcr imnprt*
                                             lur*. terauMttlc prtnurv, amMrnl unprrii
                                             lure, mmvitnm no*  nUct •«! Initial MM
                                             final MiPplU* llow on Ihe n-t *ho*n
                                             In Plgut* It !• ProlcM UM T«« 111, rirtf* ptaa the  piuap MM
                                            needle lalfC brlwren Ike prate and Itie oj«
                                            Uav • p«B» Mid nredte «M«C oomrwEtcd of
                                            •Illnlnii clcel Of «at»e albei BMterlu iw« •!
                                            fccMd in a* «aet •••.  L**h  rtxc* in,
                                            ••MOB. Mid Uwi)  purvc  Mill
                                            btlon Ite  coutecUni  to U»
   I.I.I  BvaaaUed C^Ialner SaiapUaf Pro-
 cedure. In IM* procedure. the bage at* fiBed
 br evacuating- the rigid air tight container*
 that hold Ihe te«. Uw • field aaiapte data
 ah*** aa ahotm In Figure !•• I*. Cotktcl trip
 I teat* atunple  tram each aaavpie localjon
   1 1 I I  Appanlw*.
   1.1. 1. I.I  Ptobt.  Buintaga  atecL   Pjrei
 •KM. or TeftoB tubing prote. «~~^.^ to
 the duct  IcatpemlBi*.  vMh • 4 MM  OO
 Teflon tubing of  Mfltotn* length U> aan-
 nort la Ihe aiiafllf bag. Uw ataJnwai gtett at
   111  bptaaton Pta* Art* R|
 Proaed.**. Polio* i.l.i eieepi	
 pump  va/i  another  cvacuai«d can lace
 Plgur*  IB aat  Ueje UU* avrlhod *henever
 there to a pnaallilUtr of an eiploatan due u>
 punapa.  healed probe*, or other faune pro-
 ducing . Aa aa al
 UrnaUitt. eaUatt the aampaf gaa, and avawl
 lancoaily dHm» av to Uat Tvdau bag.
   In Ihi fbat immnlun,  heal Uw bom mo
                .  '  •*• 10 Uw aourc* lev*
 porataif. piurtdad Uw rianiu.iuiU of
               Connect  Hie
Iroe. UM Mrdle nltt la tlw Teflon
line tram ittr prate PU« Ihe cmf of Uw
prate «t Uv crairotd of  Ihe Mack or at a
point no clam la (hr •«!!> than I n and
Mart Uw PUBBP with the ramllp f UM- ad|iM|.
ed lo rleld a Horn ol q* Utrf/nOnuie  Utter
uloMiw MifllrtrtM «b»r to paf,*  UM im,
op««ral  lime*, mnnn-t itx  Tvuum line to
llie ba«, and >«Bcuai« until the  rot*Arl*r
                . Then U«papart the bag a*
                ~ar la the aiMlytkcal anai
                 r the heating, or eovcr lit*
 BOB B*H an ba»ilal>ng blanket. In Uw ana
 lyUcal M*B. kaep Uw  boa healed lo aman*
 »«mMttttan onttl apaltikt. Be awe UuM the
 awtnom of heaUM  Uw boa and the control
 lor the hcaUng dram are compatible «Mh
 Uw a»My natnctlona  required In each aira
. To mm Ihe veomd procvxku*. prefll!  «hr
 Trduw bag  «HJi a knovn auaniny of Inert
 a**. Miter Uw Inert gaa lnu> Ihe bag accord-
 Ing ho 'ihe procedure for Ihe preparation ol
 gaa  CTTtrrntrailon   atandarda  of  voaail*
 liquid iMVtrhUB iSerUati d.l.l.tl. but rilml

 partly lUlcd bag to the aourre. and mrUi
      urrr gal InKi Ihr bag (lirnugli liralrd
          lines and a l>r»lrd Ilitvmrtri. or
Triton pnelllvr dbolarrmritl pump  Vtilly
ilir dilution lacton peiliMllrally Irtniugh dl
IUIWHI and analyil* ol gafl<** ol knunn run
rnitratton
  lib  Analyila ul Rag Hamplr*
  1 I S I   Apparatus Hww u fln-lloii S  A
minimum of three gat  standard* are re
qulrrd
  T I • 1   Prnrrdurr Cilabltih pinper OC
operailng condlltona a* deacrlbed In Section
g 1 and record all data tlmird in PIgure II 1
Pnrpar* Ihe fX,' an mat gal can be dram
through Ihe aamplr ralve. Pluan Ihe aimlile
loop wtth gaa liooi one ol the three callbra
Hot)  oU»lurr».  and activate  the   valvt.
Obtain al leaat l«o chrowalocrams lor Ihe
taliture. The  RMIU are aoccptabvc  *hen
the peak  area* Iron two conaeewUve tn^c-
UOM agree to within i pervent ol Uwtr aver-
age. If Ihey do not. run additional anafyaai
or correct the analytical technvauM until
HIM requirement la a*et. Then analyac the
otfwi tarn caUbratlBti olilurea M the avaw
manner  Prepare a caJIbrmUao curve aa de
acrlbed hi the aame vaarmrr Prepare a call-
braUoo enrve aa dearrltied tn OftOtm •.».
  Anaiyae Ihe aourer gaa aarafHra by con
nertlng each bag to the aampUng vaivt »tvh
a Piece ol Teflon lubing Identified lor that
bag- PMlOB the apecUlcaUoiii on repllcalc
analyaea apcctlled lor the mibraUon  gaaea.
Hecorfl Uw  data IWc4  in Figure  U  II  If
certain Item* do not apply, uae the notation
• N A " Alter all aamptai  ha«e been ana-
lysed, repeal the analyam of tftc callbrallon
ga* mlilurcB. and generate a arcond caJIbm
Unn curve Oar an a»rrage ol the l*o mrvea
to determine the auaole gar ccormiraUona
II Ihr l»o eaUtvaUort curm dUler by aMire
than t percent Iron their mean »alue. then
report UM (Inal  reaulta by eompmrlaon  la
bath callbr»ttan curve*
  l.l.t DelnmlnaUon of Bag Water Vapor
Content, afeamre and record Uw aotbtenl
temperature and bafoaiclrlc IIIIBVIIII  near
the  bag.  Prom  a  water amuiraUan  vapor
preaBur*  table, determine and  rawed Uw
vjaler vapM  content aa a declaaal  figure
I Aamoat the retail** humldlly to br IN per
cent untcaf a train vahw. to kMMna.l II the
bag haa been maintained al an elevated teav>
prraiiwe a* deacrlbed In BccUon 1 I.I. deter-
mine the atack gai vater content by Method
i,
  ill Quality   Aaauranee.  Immediately
prior u» tr>e analyiM ol the alack gaa BBBV
plea, prrlorm audll anaJrae* ai dracrlbed In
Srrllon • S  The audit analyari  muil agrr«
vttit ttir »»rt» ronrrniratlona vjhMn 10 per
rrni  || ilir results are  acrrptablr. procrrd
atllh ilir aiialysrs ol the ifMircr kamplcv  II
Ihry do mil agrre  viilhln 10 prrrrnl, thru
rtrlrrtnliM' Ilir traMin fin ihr dlacrrvarwy.
•ml laar  «urrrll«r u'lhui brlurr piorrrd
                                                                                                                                                       PI.  Mi,  Mpp, m,  •»»•••!.  .-
                                                                                                1 I I  rlniiulmi < «l, .lUllom r*l«m Ilir •»
                                                                                              nm*r olibull ..... uivr drarribm In H*rtimi
                                                                                              •» I i . vtm Ilir »«IMC ui < . iliat nwf rtputMb
                                                                                              In ilir |>r*k *tra  < «lr"1»lr Ilir runcnitra
                                                                                              lion  «'. In inm>  di» te. ul rtcli uigaiilc In
                                                                                              Ilir tamplr u lollowa
                                                                                              <'.
                                                                                                                          Eq.   Ii-5
                                                                                                                   ilir  organlr from the
    (.'onrrnlratlon ol
    calltH ttkwi rur»r.
P,  nelnrncr  pieuuir.  thr   beromelrle
    prnwuie or ateuilulr taotuk- Mop prea
    •ore  rrrurdi-d duiing CBllbfaUoti.  MBB
    Hg
T, -Baanple hup innpriaturr at the Uaac ol
    •ample analyiu. "K
P. p RrUtUr irtponie lacUw ill applicable.
    •ee SexlkMi • ti
P. *Bar«m»etrlr  or abaolute  aantple
    prevaure al tlmr of aanpie analyaki. i
    «t
T. - fttfenrnce temperajurr.  the
    tme ol Ihe aanple loop recorded during
    calibration K
B_ «Watrt vapor content ol the bag aample
    or atack gaa. praportlon toy volume.
  7 I  iMrect Inlrrlaor Sampling and Analy-
tit Procedure. The direct Interlace prac*.
durc can be uaed provided that the mnamiiT
content ol the gaa doe* not tnterfen  «llh
thr analyiU proredure. Ihe phrviral irqulre
nwnte  of Ihr equlptnenl can be MMFI al the
alte. and the aource gaa concentration la lo*
enough that  drtector aalurallon  I*  not  a
problem Adhere lo all lalety terjulicmcnU
•Ith thte rmrlhod
  111   Apparatua.
  fill  Probe   L'onalrucird  ol  •teJnIcaB
•IceI. Pyrei glaa. or Triton tubing aa ra-
aulrrd by duct temperature. • * mm OO. en-
larged at duct end la contain glaav  araol
plug. If neceavary. heal the profer arllh heat-
(nd tape or « aperlal healing unll capable of
maintaining duct teiBperalure.
  1111  Samplr Unea. • « mm on Teflon
Hnea,  oral iracrO to  prevent rondrnaaUon
of avatertel
  f.I.l.l  Quirk    Conrtecu.   To  cmtnect
aamrrlr line u> gai lampllrMi valvr on UC Hi-
atAiownl and ut pump unll uard to •llh
dra* aourre  gaa,  llav a  gutck  connect or
tavjAvalrnt on thr ryllndrr ot bat ronuUnlng
caUbrtllon g,a& lo allovi rcMiitrrtlnn of Ihe
callbrallon *a* lo i IK ga* uun^rfing *alve.
  TI i 4  Tliniiiuruuplr   Hradoul llrvlrr
INWrnllumrlrr or digital thrrtoonwlrr. ta
mraauir iu>un r trinprtaluie Mid probe  tern
pr-ial uir
  1 3 I i  lli-*lrtl Cla* Sampling  Valve  Ol
tvtu ixuiium   kU IMUI  drmlgn.  In  allov
um|>lr liiu|i In tor puigrd »»lh souirr gal Ol
f« dlrrrl MHiri-r gas into Ihr (II.' IrudruMirnl.
                                       BTH
                                                                                                                                     815
-------
 ft. M, AM». A. Math. It

  111*  Needle Valve To rnnlrul gas Nam
 pllne rale from Ihe aourre
  1111  Pump l*aklem Triton roalrd dlB
 phraani-lrpe pump or roulvalrnl, cipaMr of
 B! Irmct | liter/minute mm0tlng rate.
  Ill*  Plowmeter, Ol lullablr  rang*  lo

  1.1.1,1  Charcoal Adaorbcr. To adtorb or-
 •ante  vapor oolie**ed from Ihe  aource  lo
 prevent eipoaure of pemmel to aourcc gai.
  I.I.I lo Oca   CyUnden    Carrier  gwi
 Ihellum or  nitrogen I. and oiyien and hv-
 tkroaen for a fmmc nntiallon or lector IPIDl
 If one to uaad,
  11 I II da* Cnranataampn Capable,  of
 being  moved toto Ihe field, with  detector,
 healed gaa campling valve, column rcourrod
 u. compart* arparatlon  of  deal
 nenla, and option for temperature i

  III II Recorder/lntewrBUM  To
  1.11  Procedure  To obtain a
        the mmriliin  Bretem aa  ahown  bo
       IB II Make cure all conaccflono or*
MM. Ttorn on  Ihe probe and  mmc-lr line
htaUfr  Ac Ihe limimiliire of the probe
and healed line  approachec the couroe tem-
perature ac IndHaliid on the thermocouple
readout device, control Ihc heating lo mato
lain a tcmpcralure of  a to re above the
                    While  Ihe probe and
                      ealod. diffmiim'i Ihe
        Unc  from  Uw gao  mmnling valve,
and attach Ine Bne from Ihe callbrmlkxi gwi
                ine m mil It  nap  with  call
                    Jpce a  portion of that
•aa. BuMocd the rmwrU  Afuv  Ihe colfbra
Uon gac Bacaple haa been nuahed tnlo the
OC motrumenl.  uam Ihe |mc campling valve
to fhawi poanion. then reconnect  Inc probe
• mil In  IBM lo the valve. Place  Ihc true*  of
Ihc probe at Ihe cenOold of Ihc  duct, or al a
peon* no rlour  u»  the vatto than  I m, and
           : eaa Into the prate,  heal ml IBM.
            loap,  After  thorough  ftuBhing.
                      Ing Ihe  aaeae rant*
      aa for Ihe  cattnraiion gal  mUlun.
         the  araupBto   on  an  additional
                < |he peak area* lor the two
        . and If Iher do not agree lo wtlhfen t
perBent of Ihetr mean walue. analroe aaol-
              i until tiro concorutlve anal*
                criteria   Record  the  
ralua  to arrmagod to thai  either a IO I  or
IwTi  "HIirttTiTf of the caanc gac can be di-
rected lo the ennmuMograph  * pump of
               to atoo reaumd, and Ihto
      anal bo heated  and pmc«d In Ihr
      > beta tin Ihc cample Une and Ihc dr
lullon apparmtuB
  1-1.1  ApparaUai The cojinnncnl required
In addition lo that cpodlkd  for Ihc direct
tnmfacc cintem to ac foUoaja:
  T.l.l.t   aampte  Pump-  Inklcai  Teflon.
coaled dUphragm trp* lhal can wHhctand
being healed lo IIB'C and deliver I ft ItUn/
                i PttBipe  Two Model A tH
                                                            lerf Ptolertion A|
  ll.l.t
Kocahrr Tetloa paaHlw dtoj>ln»anni type
dcUTCttrw IH ae/mtnuit. or equlnlcnl.  Ai
an option eallhralccl flovwHcn can be u*ed
bi  contunrUon  •tth  Teflon-onalcd A*
phracaa piMBpa,
  1.1 I.I  Varna  Tmo   Teflon  Ihrec war
(alwca. aullable for  ooonectlni to 1.1 mat
On Teflon tuMnc.
  11.1.1  nomm**ti*  Two.  lot  tneanin
awtfl of dthtcnt ew. eipattod drlli«r HOB
rate lob* I.BMoe/iBin.
  T.I.!.•  Diluent Ow vllti Cfllnden and
IU«ulaton  Oat eaii be ntliatcn or clean
     Ji.  drpendlnt  on the nature  of Ihe
  Til*  Healed Boi  auJUbte  tor
        la  IWC,  la  contain  Ihe  three
        lrme-«r  lain*,  and  aawlaUd
             The boi ehould be eaulpprd
•III) quit* oanncct  IIUtnc> to racllllalc con
necUon of; til The  healed ample line Iroro
Ihr probe, 191  Ihe  cai eamplIrM) ••••*. til
Uu callnratlon  |u nlilurea. and 14) dllurnl
•a* llnea  A arnemallc diafram ol Hie com
ponenl* and cnnneclloiu to ihovn In Fliuir
IB II
  I Nora Care tntMl be uken lo k>ik rtirrk
Ihr *fmUa> prior lo Ilir dllullone- K> u nul i»
rrrmlt m potentially  riulmln almocplirir >
  Tnr hraml boi iriiiwii In PlBiirr  II IJ '>
              rlvr a hr«lr«l Illlr Iriiill  1 l*f
,,|Dnr An onlKHiBl ilnlin U ID build a probe
Hiul  Ilial iliarlM-x  dlrrclly In Ihr healrd
bun  lu IhU WBI  Ihr healed boi  rwilalnii
Ilir ronlroli lor Ilir probr heilrn.  or. II Ihv
bill  U plarrd  aeairui the durl being um
pled. It mar br  puvalblr  lo eliminate the
pjobe  hciu>»  In  rllher  raw. a healed
Triton line  to uatd lo connect the healrd
bui u> the gac Bampllng *al«e on the cr.ru
oHlograpri.
  111  Procedure. Aaannhli  the appaimluB
t>r  connecting  Ihe  healed  boi. ahown  In
Figure  II I),  between the heated
IMC  from the  probe and  the gac
rtlie on the  rhroraatognpri. Vent  Ihc
•ourr* gac from Ihe gac  mmpllng  valve di-
rectly to Ihc charcoal filler, eliminating Ihe
pump  and  toiameler.  Heal  Ihe cample
probe, cample line, and healed boi. Invert
Ihe probe and courc* thermocouple to the
centrotd of Ihe dud. or lo a peM  no ctooer
lo the watto than I m. Mracurc Ihc aourcc
irmperahtrc. and ad|uat all neatmg unite lo
• lecnperaliin I lo I-C above Into tempera
lore  II Ihto temperature to above the cafe
oprrailng temperature of Uw Teflon compo
ocnta, adlual Ihe  healing lo pMlnlaln a leva
peialurr high enough lo prevent
lion  of  water  and orgarur.
Verily Inc operation of Ihe dilution eyaUsn
br anal/Ural  a hbjh coneen* rattan g»a of
blown  eompnaHloo throufh etther Ihc l» I
or IB* I dUuUon claaeB. la approprml*.  lriilBllniu Bame M Sec
lion l.l.S, •Hli Ihe dlluilon IBCUM applied
  1 I  Adsorption Tubr Ptorrdufc I Allema-
ilve  Piueedum. II to  lunmrd that  Ihe
tester rrlrr lo Ihe National InatnuU of Oc-
cupational  Halrtf  and  Health iNtOBHJ
method for  UH patlkralai orBBnlcc lo be
campled  Tlw piliirlpml Inlnlennt  will be
•aler »M««  II watei  vapor to pieotnt al
concenlfatloru) •ho»e 1 percent. ctUra gel  .
ahould he uanl In Irani  of the charcoal.
Where more Ilian one compound to  prcatnt
In Ih*  i,.iv.lorfc>na, then de«tap cchum ad-
aofpthe copBcllr uiformBllon,
  14.1   AddlUonal  ApoantuB. In •ddNlon
la Ihr eouipmrnl Itoud  to  Ihe   KIOHH
method for  Ihe particular  ormanirdl lo be
•Mnpted. the foltovlnt Hemi lot equtvalcntt
  14.1.1  Probe   lOptlonall.
glaai or flalntem cud. approibBatetr • mm
ID. with a healing •yttcm If water conden-
aulon to a problem,  and a filter (either In
atact or out alack heated lo i
lurei lo remove  partlcuUte miller In i
Inatanrei. • plug of glam wool to a aUtofac
torr tlHer.
  141.1  Pteilbte Tubtog. To connecl probe
lo adaorpilon twbea.  Uce a malrruJ that ci
hibtu minimal mmriH adaorpUon __^

trailed, conatam rate  pump. wHh a act of
Uniting (BonJcl orlfloca lo provide i
rala ftaai eaproilmatelr Id to II
  1 « it  Bubble Tube FV>*meU»  Vo
         wUhn  i   I  percent,  la caUbntc

  14.1.1  Btopivatrh To
immii rate callbralkni.
  1.1 II  AdaorpUi	
apMtned by MI08H. cuept  Ihc
                                                   Once the  dllulton ivctcm and  OC oper
                                                 aUonc an mltolartorr.  piooM't  with Ihc
                                                 •nalrato ol courc* g*c. ouunlalnwti Ihc came
                                                 elluUon Ktllnga •• need for the narnmrtto.
                                                 Repeal the  aiuu>irc until two oBncccullvc
                                                 •iluea do not varr br more than • percenl
                                                 liom their mean value are obtained.
                                                   Repeal the analrcii of Ihe calibration gu
                                                 mliiurea  lo verlfr  equlpffwnl operation
                                                  Analyu  ine Ian IteM audit mmplec uilng
                                                  'Mhrr Ihe dilution •(•vm, or directly con
                                                  "n-l lo the  BM aunpllrMi imitt a* requlrrd
                                                  Hrrurd ill data and rrpon Ihe irnilU lo Ilir
                                                                               ring.
 •JM/VM fat for charaoal I
 mf  for alllea vH tabca.
 Ihc  t
 lorbentauthMTciauaCaT XAD-I
  1.4.1.1  Paromelrr  AcrurmU to •
 U>  •im
 aatnpllnB  and 	
  T 4.1 •  Holameicv  O to  IOB  cc/i
 delect ehanBca bi flow tale >
  1,« 1  Sampllnc]  and  Anaiyeto, II to
 •ected that Ihc leWer folto* Ihc
 and  analr**  portion  ol
 HIOflH  method  CM
 durr," ccllbrale Ihe »—...	^Z-T_. ^
 Ike now r»U through adBorpUon tuhaj wllh
 Ihe  bubble tube Oowmrter be lore mjrf>llna,
 Thf ample ircUm can  be operated al a "r«-
 rlinilBlino. loop" lor  Into  nperalMn M«cord
 Ilir amWriil irmpriilure  and  bmromelrte
 utrviirr  Tlirti, during urapllnc uce lh« ro
-------
                        !•
       rr lo (filfr Ihal.lhe pump inq uriflrr
 •Mppllnj nu* m»»im romluil
   U«r • •unole profar. il irqulrrd in obtain
 Ihr Olinptt •! Ihr rrnlioM of Ittr OlH-i. of *L
 • polnl no ctuon lo the walb Ihtn I m  Mm
 Imb* Ihe felMlh ol (kid*  lufaJnf t»l»rvn
 the prate mint KBorpUon lubn Sr'vrtl ad
 •orplJun lirfM COT 6*  I'M onopl* mUm •!
 • unman cuff M«M for Ihe  llmlllru- orllln
 lo function • • •ntc orlrtrr Record Ihe
                       Oo* r*le lor  the
                          llw bvonetrlr
                     lenptnuure.  OMaW
            caoornUMJenUI of Ihe •oWMc
                              rnl bi the
                              1 la 3 ncr-
ocni. UM •dnrpUwc eaptcMr
ly ntfuocA OpcMla (he
•ononHnf lo We •wmif»«U0* • I
After
wtfi
                              Uie
                   T.«.«,*l, Inrn (he i
                    the uMlnta of
•uaple  unUl (he  rcteUve drvtaUut o« l*o
       Uve uiladlom doe* nol coated I per
  141 SUunduOi  «nl  CmKbrmllon   The
MamlMdi can be prrpaml •DOonMn* lo the
N»P*cU*e HIQSH MrUxxl. UK • i
of three different rtMdfcnfc. (elect UM con
onM«mllarai lo bmckel
          40 CM Cfc. I (7-1-** IdlH..)

    ' Hi  primary tiid bark up prxlli»i.i ul n,r
           lubri iffHtmlrlf  II  111*
 (H>ilk»i rirrrdi  10  urrrrnl  ul Ihr
 uMiunl (primary and bar* up I, repeal  in,
 aamull' | >Hh • Uiirr umplln* porlkan
  14 t It  Ankifdi   Audit   Inunedltlrlt
 brlrar Ihe •ample aralyara. miimlnr In*  tm,0
 •udlio In accordance •lilt Srrtlon T 4.1. Thr
 •JulrMi audH ihall  M*re «llh Ihe aooH
 cuncrnltmlton *|ihln  10 prrcrnl.
  14.4.4  Pump  LcoA  <1»rc*j and Volumr
 PIOB Mil*  Checfea Perform both of thn*
 rhecka inuaedMkirlr after ounptlni wllh 411
 •MBQUni Irmin  rwnponenU In  plan  Pw
 fan all kn« rheck* •ecordlni lo the nanu
 lM-lum i knauunkm, and record the rt
      Ua*  the   babbit lube  flo««wt«  la
        the ptOBO foJone flow rale «ttb
 UM ortf ta  «a«ri to UM Lot
 Uw ra»lt- If H ha* cfuncvd bf i
 but ban Uioa • prrarnt. cajcuwl* an i
 •«« fkw raw for UM U»*  If the fk»
      BW4
      rllt
  11 41 CaJnOaUooA. AH  calculation*

 MIO8H iHtiwd Corrart all I

 *I**m toB baeo uaed, OMdUptr Inc  reouHi
 by the aioroprtalc dOuUon mllo. Cornet all
      •r drrkHiHi b» UM iteaorpllnn «ffl
    ft tiMCtaaai  raluel Report rrculU M

  1.1  HmarUnj  of RaulU Al Ihe coMofct
Uan of  ilh* field wuJnai portion of  Ihe
olud*. enaun Uwt (be data iheeU ahown In
Phjure H1-11 h»*e been otMBnletcd.
    thai d*ta on the <
      II !•
                                                                                                        f»ol»cHon Aaomy
                                                                                                                              II


                                                                                                                             .•Is
                                                                                                                             u-lll
                                                         i
                                                                i»6» noil  .«d
                                                                        I87a,
                                                 10  rT* 41 KH 41111 4m« !•"
                                                 "  n.»t»m  i  t:i.ro-.io,.w
                                               ...Irnul U—* «»"""' '
                                               rlillllr Publlihlnf Cnmpon*. Mr.         _
                                                 II  llunrnm  J W . a '- »«'*"»«»• «1-
                                               » >  IMoZlun*  eP«/IEHI< RTF  Pror*
                                               dirt. Mtm.»i: I**''  '
                                                         MB   En»l.o.inn-nUl
                                                        cw.rch Trton.1. P-rt
                                                      Ho  EPA •»/!« "••••  Jut* IIF1"

                                               "MPII«IU J  c . H J H.M. P i.  if""
                                               ^1  D B UndMf •PA/IBBtBT P Prot,(
                                               *,„. for l*,rt I SHBpltni »d Af«l1«bvOf
                                                                                         slilulr l»l (>irll|>"l	•' ^•ll"" •l*d."
P.
         liH-«dV«» «• lli*umrnU,
A!   °>s
         Vul
                   J  OH 013 00»«l  4/IU,
ft  oil «»»)••
                                               lectkm        -
                                               IW:  Pubttrmllon Mo EPA o
                                               ftuui m* IM p
                                                  14  rtotm  W  B  II <•
                                               .rammed T-»P»r.l«rr Q« t
                                               phr  Joh" W"«  * a°™- lne
                                                                                                                            York.
                                                "J? Intcfiwlely Comntlllee  bH-lhodliol
                                                Air  aunp»n«   Mid  An»l»«ta   Amerlrwi
                                                Hrallh AMorUOon W*MHngUn. I*:. !•«
                                                     Joon, K  W .  R  U  Orwnn**'- P  =_
                                                    u  and T  B  Siwitor* Bi»(roiifnr«M«l
                                                                            ,
                                                  II UrNilr llwi  Bonelll. E J.
                                                Berkeley IM*
                                                  II Helwm  U  O (.'«iniroll*d T»sl  Almam
                                                phern   Prm.lpJn  "i""  Iwhiilourm  An"
                                                Arbor  Aim Arow Stlri*r PuNUhen  ir?l
                                                MTp
 0/»T
 order* *ddnprr< i-ii
  •  8rh«c«r>-  M.  T J I1-.I"
 Huddrll  BanMiUm:  •""  An«lr«i»         _
 ,lon> Iron. ».llon«i» 3iiu«M. I  Odot »nd
 Taul H»drOrBih.«ik Jo««rn»l ol Itw Alf r»i
 lullon  Control  « ""••»•' •="'•
 ^otM from (Miflaiiifr Suitirm  MS fc"»l
 rmuncnul ltui^«l-.» A«r»-» K'1**rL*J*1'
 MNllr Poifc, MC piiWlr«llon Ho  I.PA MO/I
      l Jul» in*  II P
       TrniMlfr  H.-lhod  lor  <;onllnu«u»
          »f T.rt»l llyOrprtibo.* In Mrt- Al
            liili-i.-rfK-H-IV  fwnmlllrr.  Am-rl
 , ...  IMWh  Mr ..... A.-»»UlK>n W»l»n«lon.
  IK 111] U ••• IM
   » 'iwcrB U  »;M*r HwMlliM* ull'liriniiB
  liifiBphr. V ..... MM-* I •!«! I' StH'rm.. Kui-ph
  ird KL'HC rVr«».  CN-wUi'd  1*11
lion berore aod  ftllcr
  1*4
  1441  DrteiMbMUon ol OMorpUon Bfll-
ctoncy. Duett* UM UoUna pro«r*a. deter
                    cflldrnti  bi UM ei
                               lor,
                         lo be wed. U«
                     A
Uan  cfdctrocr of
Lalned RcpoM  UM fhonrylion  drlcrnuna-
Uon until UM MkMlvc dntoUon of IM> con
        deKtufcmirim don not fined a
         Uoi UM o«eiM« dmorpilon elfl
   cr of tbao* t*o conaectaiw  deteratbM.
Uam for UM tunattloii apKtlled In Section
7 4 4 a M th* dtMivUan elllcim* of UM
co*opoiil>dla> of  bitrinl  t»  qunitonkbtr
under actml aampUng rondllkHM. UH of the
Hethoa of BUMMlaid Addlllunc a»r be help
ful lo detennlne thai »»l*i*
  1.4.4.1  Oetetvl«Miuon of Horaplr  (Jollvc
Iton Cfftclrntr Par (he mourn •ampin «,„
  I. lloii man anejtlr for Te
rtali C.  rhrouch C. Hro>ocmrfaoo* In  UM
         m  by   OH  C3uaaMi««rmpbp,
       D mm-lt. pmn U. PfcllodrlpnJa. Pm
n«M  MII  in*.
  1 Com on. *. V. Hctnodafoii far CoUerl
•>• ond Juodyilnt Orfjanic Ate PoUutoou
U«   &ntnMnnn»ul  Protecuon   A*cnri
Puollratkn  No,  EPA fd*/l !• *41  Prom
w in*
  1, Onniteka. A . B, K  Krol«uMiioU. 4,
WhHfleld. A. O Donnrll, *nd T, Biuvwahl
BnrlroiaBnilal  Odenot  >nd  Technolatr-
HI »»: i MI int in i
  4. BMerum. P. T,, and P M Netaen. Ou
ChronuuUiirapnk AiuUntt  of Engine  Km
bouM and AteaopncrE. An»lrlt«-»l Chemn
Uf. J««l: IMulM) Itfifl
  k PolrlMHIn,  V. N..  P  J  M>rn. I) H
Hurbv ud U L Huibj  TrelmlrtJ Mviu«l
for Plocat Honpilnt B4r»lr«tn »M <)r««n*r
HkUflab)  11.8.  EnvlronnwnUI
A*rnry KrorMrh Trluiih-  P»ik. Nf
»Uon  Ho  KrM oOO/l 7«  III  April ICTi
nip
                                                                                                                                  H19
                                      878
-------
Pi. 40, Iff. A, MUtV It

I.  mm tftMMV
«« CM Ch. I (7-l-M
      et tr ft* It It
11.
   •M«tttrltl
            l:  Ittch	Cntl
        fteftf tf k«Uh «• cfclt _
        •nl «« to l«tt	
       Cyclic
           PffMr*  1S-1.  PrtltalMry tunwy tfita sNwt.
                                        Pt. M, Ap*. A, MUHi It
III.
                                       Mta
                                                                         Sit* «nfrlpi«M _
                                                                         feet AM* toi iln
                                                                         MUrtel _
                                   Sin •? prt
                                   Slntf
                                                                      I.  frtptrtltt tf pi
-------
, 40, A»*. A. *•«*. )•
 c.
4DOI Ch I iri-fVEdHlon)   j  f«*lf**MMital
                                                                                                     M, Apr  A, M.H>. It
        tol humm to ta
                 M4lnU
    Mricl* tnfnt r»lt§
 t.  lit* «
    ir
     tpm U-l (o»tlM4).
                                     to
                                                               mm flow r«to ___
                                                           Ctolojni tftapoxatarot
                                                            lB)«ctiaB port/siunplt
                                                            Ootootor u«0«r«tiiro
                                                            Dotoctor flow ratoll
                                                	*e
                                                     *c to
                                                 loop toaporataro
                                                                                                     •t 	^-C/»JUi
                                                                                                  MtOBMtiOO
                                                                                •toorapltlr condition* 4*ta *n*«t
                        882
                                                                                      883
-------
 «O.
                   II
                *r*Mratle* of Sta*«r*i  In
                        aatf C*llfcri|l«*  Cunt
                                               CP • CH. i
                                                           -w MM*,
        Pr*Mr«lt«* O*LI:
                                           •I "turf
                                             ij
MM
    fat atl
    ! «t»r
      at atlcr calibration  fact*r
                    (Hurt)
                      illt*rfl
Nitmtf *•!•• illMrtl
%«r«9t Mlw l«p*r«t«rt
Avtrtft •»«•*• prtftvr*.
                    III
                        ««p |» MB I
                        «r« 
AttM*attM 'actor
Paw h»lpkt ftp!
•aai araa laVT
P*at araa • attmvatlea factor  tmtl
CalHlal*i caa«a*traila« Ippai
  flo^ailaii It-) ar II 4|

riot Mat araa m •lla^Mlloo factor afal
ta a»ul* catlaraiia* c*r«a.
       fpwr It-].
                                          calcol*U4 co«««tr*|(on
                                                                                   •nlal Proloction Aponcy
                                                                                                                             M. App A, M*ifi. It
                                                                                          Or  IdtfltlflCatlOH
                                                                          M*.

                                                                          riot f). a»J «ra« a
                                                                          MMlft cwva.  If lia flaMMtar fecliif callferat»4  It a rouawUr ar *tiwf
                                                                          fla* M*Ua IMI It •lK*tltf *»aa4a«i. It Mr ba oacattary  ta MMrate a
                                                                          •faally* af call brat loo cor«tt that co»tr tk* aparatlaf praiiojr* mt
                                                                                     ra*fai  of tba floMMlar.

                                                                                                                                      M. II Mf
                                                                           ifeila UM f«lla«liif lacMlwt  ika«I« M »»riri«4 Mfar*
                                                                           ka Mtttftlt I* calCMlat* flM  *••!• r*a*laft far rvlaavlari al
                                                                           ta«*ltl*at Q|t4 •*
                                                                                                                        I/t
                                                                                    lav ratt
                                                                                                                              flw rata
                                                                                             !•-«.
                      cat lira!!«• c«r>*.
-------
                                       't-t|
I


1
s
£
i
iivuumM
                             nuvuieam
                                            IJ
-------
                                       1

            j-  SYVINGI
BOIUN6
 «AIEI
 IAIN
-------
I
                                                  •i-fl
 d

 S
 9
  I
  4

  1
                                                                                           S
-------
I
       ftat	fcU	
                                003
                            	      	      	>i
                            '^^^^^^mmmm      •^^^^^^*mm^      •^•MM
                       ro
                                                                    I.  •»M**l  tftfMl
                                                                                          n rci
                                                                                    ••«
                                                                                             tall
                                                                                                 <•€»
       Nalifctta            	       	                   I                 WMI !•«/«• tatoi
                                                                             Caniai «•• fl«* vau
                                                                                              fCI
                                                                                              •r tail*)
                     W-M.  rtoU M^W *U Mwt - MUr	. ^^n,
                                                                             UtetlM fM ffter ••••
                                                                                      It-11. rtaU «Ml]r*l« *u Btat
                                                                                             893
-------
                             f
                             *

                             i
  I
I
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                                                             •

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I
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                               1    r
                               :    r
                                                                                  a
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CK
                                                    ••c
                                !•»».  Mf«t
                                                                                  7


                                                                                  8
                                                                                  .
                                                                                  $
-------

                   •M MCtafCMl
   frm Pit*
         Oriel
              I.I
                     1M
                     cc/Mi
                        10:1  100:1
                              ?• i*
                         ti1«H
                         W0:l
                (MtM to it lift Ir
                                                      I
                                             (OR Ovtjt*
                                             Of
                                              n» tit* ftf ft
                                              1MO ec/Wii
       1A*1S idi^Htle MMPM »f tta iMt^ tei
       W^ftV* ••WiWVM V "* V *1^p>lRHF V* •••• nHRBMH ••"•
                                                      M
'I!
 Ji
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1:1
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                                                3 ,  Z

          ooo  B DDO  o o a   o  sac c::c c      IS


                                           f    !  i

                                                -II

                                                -II

                                                -II
-------
EPA METHOD 3A
-------
ft. to.

padtr
rrru-d
lurr.
tot or
il
             A. M**. 1
hu  cauti
by  varM
     t
     Uw
rllnl «•
                   Calibration »l||  Or  *f
                   In Mad IK* l*mi»-r*
                         ltp. and ntolrru
                UM promdurr In Srrllun
                UM •T-MT— i dr>lra> pa
                  tMcr»al Irrqurncp lufll
                   profile c*ch projvai ry
                  iniB «w*», A
                     r Hay to iimd.
              «. CWM**No«
                          Dr*lcc. Uaf the
                                1  t. MMl
                                              «o «• CH. i (7-i-i*
•1>I>IX  llir  umr  prilarmwr
I'allbrair  tlir mraaiiilita'  driiri-  vlili ihr
prim-Ilia! ilmrt |U lo br mraoiird >t m . mtt,
nilroarn*  Malm I  •  aundard  irrrtrnrr
mrlrr  A r*IIto*l*d dry |a* iwtcr h an «c
r««UM» rtlrtcnra m»l«>  Idndlr. nilhraia
Ihr mruuiln* dr*HK In llM Ck-W »llh llw
•rlual  t« to kc irnnirrit ftot nwuurtr^
drrlm  UMt  INK • *Mmc  r«lr iradout.
cBlculBic UM •naitlm Arvlnc csllbrallon
ctM-fltctrnl. T^ lot Mich t«n M follow*
                                                     In Urn «Hd ta«
                                          fewwwtet pttat to Uw n»M
                                                     |h« (Uck |M| (to* rale. Q_  M
                                                     Eq .10-1
                                       T.
                                                  I-Q»» Ajiuvai* MM C*uop Dto«
                                              IH. OlTaav. Kacaa* Am. u* DBV Mo

                                          I. fMBCtpt) M4 J»p(iiwMli|a-
                                      "*     I.I  PrlnclM*  A CM •ajatple to riUMUd
                                          fraM • MX*, br am* of UM foilBvtn* ^nh
                                          •dB'. Ill Btnglt.pofaL  grab laMplIni:  Ol
                                          •kMlr point,  miccntrd  aM-pHn«  or  in
                               i~.  H..   «»ulll-|i«*H. IntcaTBlad  naaplln* Th* gm
                               inc. w-   aaaapl* to aoajpamd for pCTfMM rutan dtoi

 i Ortflo. Het^ta, of *Mm> o^ A«en   *JC^-T12^1^^CT,IT".
               M^Arilngtan. VA Report   ^ nMrtecuto* •cl.hl dxtcnjlralton to l» to
                                       606
                                                                  •lot
                                                                                                                                                               40, App. A,
      rllhrr an !
           I lot-in* analyalt, foi t
_		. ralr rorieclkin factor
nation, an OtMl mnmtr*** mtmt to uard
  I 2  A|W>ltr*BlHI» Thta mrlhud U i
Mr  lof drirrmlnln* CXI. and (>•
lion*, rirrm mil. and drr nwlerular
of a laniptr tram • (B* Hiram of • luavll

•too M appltraolr la othw-i  vtocca«a •!«••«
II  ham torn  drirnBlnrd  thai
other lltwt CO.. IX CO. ami i
at* not nrrarnl to eoncenirmllon* Mff
l« af led UM reatilu.
  OlIMf B»lhod» a. mil •• modllhalloo. la
UM iHvrrOu'* Aacrllvd iMrcln. arc atao ap
       > lot «••* at all of |h* mban dclcf •
           •••MOln of Aperinc mrtnod.
                         (11 • aiuHl polnl
                                      r to
                                      I M
           III • BMtltOd «•»"• CO. IN  O.
• lull Agrnry
                                                                                                                                                           II Ji f.'ioliunrrwntat  Ptoli-r
                                                                                                                                        Am an «lir«M«u»r lu llir B«mi>|lna mpfmim
                                                                                                                                      tim  *IH|  ifilrms drmlbrd  hrtfln  ot»v»r
                                                                                                                                      Muttplii« •»•!» mi lnlii« «  irprrariuallvv (Binplc
                                                                                                                                      UKt RiBlnlAlntnt • COMUM. ••cHtn« imlc,
                                                                                                                                      •ml «r« o
                                                                                                                                        1 1 I  Proa* Th» pco*>r itxmld he madr ol
                                                                                                                                      •ulnlna  M»l « nofuvltkmi* gtm
                                                                                           ___   ^ ----- -
                                                                                           •ad MaltliMwtrtr
                                                                                                               * m ^^«— •  »'  '» — -- —  --
                                                                                                               trtr ealnilMlani la  •»
                                                                                                                •* lor
                                                                                                                                lor
                                                                                                                       .     . or oU
                                                                                                          MMI iMdinaUoni OHIP te
                                                                                                but M* M*|ecl la Uw •mranl ol llw
                                                                                                 wl|M. ki Um erf
                                                                                                                                            cxil liar* (IHn lo rrmuv* p*rtlruhkir iMilur
                                                                                                                                            <• eta* 0' VMM *uol to uU«r*rtMr for thh
                                                                                                                                                      Aii» o*r»*f main Mi |nMl lo IK
                                                                                                                                                 CO,  and N. UMt inMuM la H-^ffura-
                                                                                                                                            twnr •! MMpHni catMllllaiiB "•» to «•* fat
                                                                                                                                            UM  ptoto; ••Miffm  of  well awlcftol •*•
                                                                                                                                            •hHBlnaai, rapfwr. «u*ru «!•« Bad Tcllam.
                                                                                                                                              ill  FWip « anr traf nn»f»«t ouH>. at
                                                                                                                                            tavl*alrnl.  !• W»M  IB  lr>
                                                                                                                                            wnpl* la Ihc •
                                                                                                                                              1.1
                                                                                                                                              1)1  Ptoto  A ptato  suck M Uut
                                                                                                                                            •rtta-d in atcttai II I
                                                                                                    'Mention of umtv nunn CM •prrlllr prvd
                                                                                                  urU don nol cmullluU mdunfmrnl by llir
                                                                                                  Eii>liutunrnUJ
                                                                                                                                          6U1
-------
PI. Ml.  App. A. Mplh. 3
    40 CHI Ch, I (7-1-W Fdtllon)
            „      /
Ml lldi  ItltlMfi
                 HI UN 161*11*0011
                                                                 /      10 MAI V|| „
                                    MMf M tm»
                                      3 I  Gi
                          fonl
                                       808
                                                                                                                  Protect!** Agency
  111  CiMxtrretrr  An ill rooVrd or »alrr
1'iiolrd cotMlriii*f,  o§ other corwlenarr  tlitl
vlll not rrmorr O., Co.. CO. and N. may be
iiard la remove nrru mottture whkh *auM
Inlrrlrrr vllh the operation of I he pump
and fla* meter,
  I II  Vatic A nerdle valve Is uaed to
adjiul aampfcr ia* do* rate.
  1 It  Pump A leak free, diaphragm  type
pump. or equivalent. I*  tued U> Iranapart
••mill*  gaa (u ilir llrilblr teg  liuUII *
•mall auric  lank  between the  pump  AIM!
rale mciri  lo eliminate Ittf pulaallon rllrat
ol the diaphragm pump on Ihe rotametrr.
  1,14  Hale  MtUr  The  rotameier, m
e«ul»aienl ralr meter. uaed ihould be cap*
Me of Bicaaurlng flo* rale to vllltin i 3 or* •
cent  ol Ihe •elected' (low ml*.  A Oow  rate
tan** ol KM to IM» ruVmln b MiuralMl,
  tJ.f  PVatblc  BM  Any Ink Irec ptm^tc
M.  or c«Hl*«lenl. lM*lm • c«|McUp  con
•IMfiM *Nli Uw wlcrted  Oom nte and  line
lm«th ol the Icat run, m«r be UMd A t»-
      In lit* tMwe of M to to lltcn t*  lug-
                                                                                                   To leak-chccft  Uw tag. connect II  U> •
                                                                                                  *Mer iBMMMnctrr «nd praouittc Ihe Ing la
                                                                                                  t la  10 en H.O  II lo 4 In H^)>  Alto* lo
                                                                                                  •land lot lo mfenulcB. Any illmliiiiiiiiil In
                                                                                                  llw  «mi«r  aaananrKi InjBtmm * lettt, An
                                                                                                  •netmllic Ink dMcft mrlhod I* (o prnuw-
                                                                                                  Mc llw DM lo tt la lOrm HjOlt u>4 tn  H.O>
                                                                                                  Mid *lto» la Mjuid ovrmlchl  A drflMcd b>|
                                                                                                  Indlcmtra > irftk
                                                                                                   1 1.1  PrcMur*  Otu«c  A **lcr filled  U
                                                                                                  lube  ounoatrUr. at rrtul*atmt. ol about M
                                                                                                  am in bvi h uwH for the flCBllHe UM  leUk-
                                                                             ciu-f
                                                                                                   1.1 •  Vu-uum CtaufE A
                                                                                                 »t*r. m muliBjcni. ol •!  k^ 1W •<• Hi
                                                                                                 <» In Ho b wrd f«M UM ••mplli* ItMn
                                                                                                   I i
                                                                                                 durca, folio*) the maUuctlcm i
                                                                                                 by the manulaciurcf. unfcai otlM
                                                                                                 tiled herein
                                                                                                   111  Oty Molecular
                                                                                                 Uon An Oraat analraer oc Pyrtu type com
                                                                                                 bunion gaa analyacr may be iaMd.
                                                                                                   1.1.1  ^—«—«— Hale Correction Partoi or
                                                                                                 B»eea» Air Determination An Onat analyt
                                                                                                 ei muat be uaed.  Par la* CO. (leaf than * •
                                                                                                 percent! or high O, (greater thai IS* per
                                                                                                 unl I concent ration*. the mcaoirlng bufrtte
                                                                                                 ol the Oraat muM ha*« al In at O.I
                                                                                                 > D*» VobCMter WdgAI Octermlaalloii
                                                                                                   Any ol Ihc Uirec tmmpHitt and •nalyllril
                                                                                                 voc«duica drwiltxnl brio* may be usrd fur,
                                                                                                 dcKrmlnlnc ih' dip raolrcular wrlilil
                                                                                                   1 I  ainato Polnl. titan Hjun|illiia UMI An
                                                                                                 *lrl leal
                 PI. 60. App. A, ftUth  3

   1 I I  The sampling  polm  In the  duct
 •hall rliliri br al Ilir ctntroid ol the croaa
 •mum or al a point no rloarr u> Ihe walla
 than I M m U 1 II i, unleaa olherwlae apecl-
 llrd by Ihe Admlnulralui
   I.I 1 Hr[ up Ihc equipment a* ahovn In
 Figure 1  I. making Mire all oMtnecttena
 ahead of Ihr analyicr  we light and leak-
 Iree. II an Onat inalyier t* uacd, U la nee-
 onunrnded that Ihe analyser  be leaked
 checked by lollovlni Ihe procedure In Sec-
 tion 8: hovrtrr. Ihe leak-check at if* IT*
   1 I 1 Place Ihe probe In the alack, *llh
 Ihe  lip of Ihr. probe paarUmied at the aajn
 prlng point: purge the aaa»pHng line Orav a
 •ample Into the analyier and liaaawrtlalrli
 anaiyar II lor prrcenl CO. and peroenl Ob.
 Determine the percentage of the gaa that I*
 N. and CO by auMractlng the auaa of the
 percent CO, and percent O, from  IM  pet
 cent. Calculate Ihe dry  molecular vetghl aa
 bMMcated In Bectlan • J
   111 Mental  |he aampllng, artalyaai, and
 calculation procedure*,  until the dry i
 ular  *dghli of any three   grab
 dtlfer Iruoi their mean  by no more than • I
 g/gaaote  iO»  Ib/lbrnolri  Average  Iheac
 three molrcular velghli. and  report the re
 aului  In  the neareal Ol  f/g mote llb/lto
 molel
   1.1  Single Point.   Integrated  Sampluig
 and Analyllcal Procedure.
   Ill  The aampllng  point  In Ihe  duct
 •hall br located at apedltod In Section 111.
   1.11 Icakchcch loptlonall Ihc fleimle
 bag  aa in flection  lit, Set  up  the emilp-
 anenl al aho*n In Figure 1 1. Jual prior U>
 aaBopllng. teak check 
-------
1*1. 40,  A*a». A.
Detenntne the pcratntac* ol the «u (h»i to
H. and CO by  •uMrartlntl Ihe mm of ihe
prrarol  CO, and «cmmt  t). from IW pti
ami. T^m'™'-'-  the dry molecular •eight ai
mmmiMl In auction • .1.
  l.I.S Repeml  the analyse and mlcuiallon
proigtUmo until UK Individual dry  nmlecu-
ku  veighU for any Uircc analvK* differ
from Urctt mean by  no more than  0 ) •/«
•wto «• 1  M/aVawtel. Average thcae  three
mnlM-uhii  wrigttU. and report the reaull* to
UM !••»•! a | g/g aMlle I* I |b/lt> mote)
  1.1  HulU Pomt. Intcvraled 8ampllng MMl
Analytmi Proeadun.
  Ill  UntaH  ntoarwfac  aperlfled  by the
                         i of eight  Umvcrae
                    id  to* circular Bt*c9J
                    i Umn • •! • (M m.l, •
                            I foil
                            •iiaaliii mat
Uwo  •.«! •> 1M m.>. and •  airntonna ol
l*a«v* Invayaa pntoui atuul be •acd for an
           . Th* invvrac ponta anal I be to-
                te Method I. The «a* of
fMPft paint! to •BBjBtf  to «npntal of the
                40 CFI O  I {1-\-m IrfltUe.)

                   -3 • S*aa*t*M>n>Mt
  S.&al  PMtWat UM iwcKWkdmWcc fivflifiwl fen
fmrtfcma 111 Ihrmarh S.l.t. e»eept for  Uw
following- Uaverav all campling potnU and
aaaaplt al aach potnl for an equal length of
Uaat. MaDord mmpltng data  a* chown to
figure I I
4.  SmitBitm  Hale  Comcifon  Factor  or
I****** Jlr Deiermlaatioa
  Mom A PTTHe type combuctlon gai ana
lywtr hi not acceptable for eco*m all or eaua-
atom rale corrwcUon  factor ortermmaUon.
ueitoav. afajt'ovad by Ihe AdaBtoMralor. II
botli paiutiit CO, and percent O. are
and. Uw aoalyUcaJ reaulu of any  of  Uw
threa procauuraa given below may atoo be
      for cakulaUng Uw  dry molecular
        4.1.1  Pmot the probe to  Ihe BUM*, irtth
       Uw Up of Uw probe poaNloned al the *anv
                  pom Uw •amptlng Itoe. Draw a
                 i Uw analyarr  Por emamton rate
                 actar determtoatlon. towiinttote
       ly analyae Uw •amplr. a* outlined to Sec
       lion*. 4.1.4 and 1.11. for percent CO, or per-
       cent tx If aaeaa* ah- M deatred. proceed aa
       futkiaa: 111 wamawftatdy analvat the aampw.
       aa to uwrltoiw) 4.1,4 and  4,1,1. for percent
       CO. «X and CO. tSI determine the percent
       an of Uw caaUaU • H. by aubtrartlng Uw

       cent CO from It* percaet: and ill atteoml*
       percertt eicaat ah- a* outlined to aectloo • I
        4,1,4  To  toaure ccaaptete afeaorpUon of
       Uw CfX Ok or  U apptlcaMe. CO. make re-
       peated paaan through each absorbing aolu.
       Uon unto two cooaecuUve reading*, are Uw
       aame. Several m>i«n ithree at four) ahouM
       be  made between  readtowa.  at the omtrntd of UM croav-
aaetlon or at a paint no daaef U> Ihe wmlto
than I m> m (II ftl. unloai otherwlac apeel
Had by UM AomtnMraU*.
  « 1.1  BM UB the •outpmenl a* ahown hi
        II.  aajtlng mtrr all owmectlon*
       of tnc analyaer are light and lea*
frae/. Laak-dMck UM Ofaal •nalyier acrord
Ins to the procedure deacrfbed In flecUon I.
Thai mafe -check li nuuirfaLDf y
filing and analyl^al peocmlure
           In  nonjanctlan a4th  a alngle
      grab Bamming and analytkBal proof-
dare for a poOwUuii. only one analyato to or
dtnarffly conducted. Therefore.
muat be taken la obtain a valid i
analyato  Although In moat caaea only CO.
or O, to  rtiqutred.  U M recommended  thai
both CO, and O. be meaaiired, and that Bee
Uon 4.4 be uaed la validate the  analytical
         1.1  Blaxte Pobil,   lnlcar«U4  aaaapllng
       and Analytical Procedure
        ' 4.1.1 The aaaaplttig potnl In the duct
       ahall be totaled aa apeclfled In flection t I.I.
         Ill leak-etwc*  (mandabwyl Uie  fleil
       Me bag a* In Section I.U. Bet up the equip.
       merit  a* ahoam In figure IV Jiot prior ID
       ammpllng, leak check I mandatory i the train
                                        010
                                                                                                                toi Pioloclton
                                                                                                                       60, App A, M.lh 3
  hf placing a vacuum ••iifr al Ilir  before
  Uw analyato ff ciccyj} klr to desired, proceed
             U)  wttnln 4 hour* after tht-
           taken, analyat It faa to Bed ion*
  411 through 4.111  for percent CIX CK. and
 CO. llrdriermlne the percentage of the gai
 that to N. by auMractlng the mm of the per
 cent  CfX percent O* and percent CO from
  !<•» percent; III calculate percent eiceu air
 ai outlined In Scctton 4 1
   4 J.»  To tnaure  complete  absorption of
 the COk Ob or If applicable  CO. make re
 peated pame* through  each abaorbing aolu
 lion until taw eonateuUve rradlngi are the
 avow  Several pame* Ithree of four I ihouM
 be make  between  rauHiMja.   ilf constant
 reaaln«a cannot be obtained after three con
 eecollve rcadtog*. replace Uw afeaorbtng an-
 luUon.l
  4.1.0 Repeat  Uw  analyato unUI the lol
 towbig criteria are mel
  4 I.i.l  Pot percent cOb.  repeal the ana
 Irtlcal  procedure unto Uw raaalu of  any
 Ihree analywe* differ by no more that ia> 01
 pernml by vohnm when €7Ob hi greater than
 40 percent or Ibl ».l  percent by volume
 when CO. to lem than or equal to 4.0 per
    . Average the three acceptable valuta of
                                                                                                  eent.
         .         .
  4.M.J  Ft* percent CK repeal Ihe analytl
eal procedure until the train* ol any three
analyat* differ by no more than lal • 1 per
rant by  votum* when  O. to Irm  than IfiO
percent of  ibl 01 percent by rolurar when
O, to greater (tun or equal la IS a perrcnl
Average the three acceptable value* of per
cent €1. and report Hit reatilta u> thr iM-aicit
01 percent.
  4.1.4TJ  For perrenl CO.  repeat Ihr ana
lytlcal  procedure until Ihr  rrmlu ol any
                                                                                                    Hirer Dialer* ililln by  „„ mnr,  lttmn aj
                                                                                                    priiviu   Ari-mgr   Ilir  Ihrt-r   •rrriMahlr
                                                                                                    vaiiii-... »l iH-irnil  ihr Ofial  inalyu-f
                                                                                                    MINT •••Hi. *,  he valid. llic
                                                                                                    llriai  uializri  mini  pau ihli Irak  ir»l
                                                                                                    before *n illrr the analyila.

                                                                                                      No»t.  AHIuMiiti m nxMI InMancea only
                                                                                                    ct». or O, to required, II  to recommended
                                                                                                    IMM both CO. and O. br ntraauretf, and Ih.l
                                                                                                    Section « 4.1 be uir« U>  validate the analyll
                                                                                                    eal data.
                                                                                                     « 1  Mulll Putin. IniniBinJ Sampling and
                                                                                                    Analytical procedure.
                                                                                                     4 J 1  Hwlli Ihr minimum numbrr of cam
                                                                                                    Vllnt point* and the campllnc point  km ion
                                                                                                    •hall br as (perilled  In Section 111 of ihli
                                                                                                    method. The uae of fever potnla than apecl
                                                                                                    fled M Mibirct to I he approval of the Admta
                                                                                                    •Orator.
                                                                                                     4.J 1  PMlow  the  procedure* outlined hi
                                                                                                   Section. 411 through 4.1,1. eicept for the
                                                                                                    10110.1m  Tiaverat aj| aimnllng potnj. .^
                                                                                                   amamit al each point io> an equal lentrth of
                                                                                                   Ifcne.  Record aampllng  d,u u ihown  M
                                                                                                   Plajurr • I
                                                                                                     44  Qimllty Control Procedure*
                                                                                                     44.1  llal*  Validation When  Roth  CO,
                                                                                                   and U, Af e Hruitrrd  Allhouih m mam In
                                                                                                   ilanres, onlf c.YK ur Oi  mrMuremenl  b> le
                                                                                                   quired. II  U recommended that bnlh  t:O,
                                                                                                   and I*, br mraiuipd to  protlde a chert on
                                                                                                   the quililr ol Hie data. The follo«liig gual
                                                                                                   I11 rnnlrol prureilure li
                                                             percent CO, and report the reauMa to the   "°"
   Hun Hlra-e the method lor vtlldallrai the
  O, and O, analyie* a baard on eombuatiun
 of organic and fomll  lueto and dilution of
 the gai it ream with atr. thai method doe*
 not apply Ut aourcei that (11 remove CO, or
 O. through  ptOttawa other than  comhua-
 Uon. Ill add O. leg. oiygen enrichment)
 and N. to proportion! dlffernrt from that of
 atr, 111 add CO, le g . cement or lime kiln.)
 01 441 have no fuel factor. •„ value* obtain-
 able leg., eitremely  variable  wart*  mil
 tunai. Thb method valktete*, Ihe measured
 proportion* oM"O. and O, for the fuel type,
 but the method doe* not delect •ample dUu'
     rewulllng  from leaks durlruj or aftet
 aampk rollerUon.  The method to applicable
 for aamptea collected downatream of moM
 lime  or  Umeatone flue !•*  desulfurtovtion
 unlu a* the CO, added or removed from the
 g*a ilrram to not  (trolllean* to relation u>
 Ihe total 
-------
               40 IM 0.. I (7-l-W
p..
                                                                        )
                  ••c!l iftauld be coMibVral In de.
      Lrrmlntna If • rHol b •opra**«ttc. I* . U
      the uM»»uml i-iafauuia urr nnirti town •
      oiiKti (Tnter  I ban the ecmpttence UB,H
j I   (vpetlUanof Uicb»lmiUnol>l«nllfc»mUv
                                       N «0 tak. TtwnriOT. MI Oral AIM
          UM a Md CO*
        UM mtruhllnn far f. m


                                                         N.-r 00

                                                         i a

                                                         CO,
    «? rant* of ill pn
   lot  the  r. tartar of
nvtBMr furl nUoi  The
    ratr relative to Che
CO. and H. I<*latent from Bectton « I
* > «> Into Bawrilon ) 1.
                                                                    I <•
                            613
                                                                                                                                       «. M. A**. A.
                                                                                                                                         1A
                                                                                                  0 Ml
                                                                                                      0B*ro
                                                                                                           o.» «coi
                                                                                                                           J  I
                                                                                        Mow: TTt*
                                                                           Iton tfuf« tanawa IhW
                                                                   all » aaedai theaaurc* ol O. and
                                                                    luri doe* not tamlaln vomtelito
                                                           aBMMinto of N. «aa do eokc o*m a* ataal fuf
                                                                   •» Vat Ihuac caon •ben amMwcte
                                                                     i of N. an loiaaul «i
                                                                                        • I  Orr Hohmiaw Vc%M. UM
                                                                                      1 I lo cajntteic Uw diy awfaruav •vhjM of
                                                                                                                          J I
                                                                                                lion ol Ihc umplr ilrrun • oonteied lo an

                                                                                                   O, and CO, ronrcnlnllonliI  Pcrlom-
                                                                                                     apKirtemtMMM and teat procedure* arc
                                                                                                    Idnt in rnMirc reliable dala.
                                                                                                1 Haaav aad Sf ••l(lv not lea* than
                                                                                                H percent of the i


                                                                                                  II  Meoaumacnl  flr
                                                                                                atnlpiiirnt rmulrcd lor Uta	
                                                                                                of Uw O,  or CO,  ai  DMtaiaa  Covramu
                                                                                       I.I  AnpHrmMlltr  Thai lacUBd at aiipll
                                                                                     cmbta IA thr drlcnataallnn of amfffu tO,\
                                                          fend cutnn dtoildc UtWl connUvllom bi
                                                          ii«h»luiM)  Irani  ilAllonur  Kurra  onlr
                                                          • hen •jmillrd vUltln Ihr ingutallmic
                                                           I 1 mnrtolc  *  (unpl*  !• conilnuiHHlV
                                                          rilnrLrd frun ihf rlflurnl itirtm m vat
  t I t On Anal ran An i
maw ronltoMMHaUi llw O> or CO, onmrnlra

•hall ocvi ihr owtaaole prrfanMnc* apoc
IIKalKHu ol aecllonvf A  IOWWH of rontiol
llnf Iht inalrwf I tow imtr end • dolor for
oVI»mJ»Jn« prufvr camplr Oo» rate tr«.
-------
               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  (C02) and oxygen
(0^) concentrations ind dry molecular weight  of  a  sample from a gas stream of
a rossil-futi combustion process.   The method^may  also be applicable to other
processes where it  has bten determined that compounds other thin CQ^t 0,, carbon
monoxide (CO), and nitrogen  (N-)  art  not  present in concentrations sufficient
to affect the results.

1.1.2  Other methods, as will  as modifications to the procedure described herein,
are also applicable for some or  all of the abovt 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 C02 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.
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 sampl ing; (2) single-point,  integrated sampling;
or (3) multi-point, integrated  sampling.  The-gas sample is  analyzed for percent
CO*, 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 Htisureuwnt Branch                           EMTIC TM-003
Technical Support  Division, OAQPS, EPA                            May 14,  1990
-------
EMTIC TM-003	EHT1C NSPS TEST HETHOO                       Page i


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, C02, CO,
and N., 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^, CO, and N^, to  remove  excess
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  Rite 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 Sag.   Any leak-free  plastic  (e.g.,  Tedlar, Mylar,  Teflon) or
plastic-coated  aluminum (e.g.,  aluminized 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,  HjO).  Allow to stand  for  10  minytes,   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.) H-O and allow to stand  overnight.  A deflated
bag  indicates a leak.

2.2.7  Pressure Gauaa.  A water-filled U-tube manometer..or equivalent, of about
30 cm (12  in.), for the flexible  bag  leak check.

2.2.S  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 Orsat or Fyrite type combustion gas  analyzer.   For  Orsat and
Fyrlte analyzer maintenance and  operation procedures, follow the instructions
recommended by  the  manufacturer,  unless other-wise specified herein.
-------
EHTIC TH-003	EMT1C NSPS TEST METHOD                      Page 3


3.  SINSLE-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.
                                                                      percent
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 CO* and percent CL.   Determine  the  percentage of the gas  that is N, and
CO by subtracting  the  sum of  the percent CO*  and  percent  0^ from 100 perc
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  Up  of the probe positioned it 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
CO,  and  percent Og 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  N2  and  CO
by  subtracting the sum of  the  percent CO? and  percent  02 from 100 percent.
Calculate  the  dry  molecular weight as indicated in Section 7.2.
-------
EMTIC TH-Q03 _ EMTIC NSPS TEST METHOD _   page  4


4.5  Rtptat  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 lb/lb-tnole) .  Average these three molecular weights, and  report
the results to the nearest 0.1 g/g-mole  (0.1  Ib/lb-mole) .

5.  MULTI-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 Qrsat
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:

S.I   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 thin 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 thi  next 4 minutts.

6.5  For the Orsat analyzer to pass the leak check,  two  conditions  must be (net:

6.5.1   The  liquid  level  1n  each pipette must  not fall below the bottom of the
           tubing during  this 4-minut§ inttrvil,
 6.5.2   The meniscus in the burette must not change by more than 0.2 ml during
 this 4-minuti  interval.

 6.6  If the analyzer fails 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 TH-003                EMTIC NSPS TEST METHOD                       Page  5

7.   CALCULATIONS
7.1  Nomenclature.
       Md - Dry molecular weight, g/g-mole (Ib/lb-mole).
     %L£>2 * Percent CO- by volume, dry basis,
      %02 - Percent Oj by volume, dry basis.
      %CO • Percent CO by volume, dry basis.
      %N2 • Percent Nj by volume, dry basis.
    0.280 • Molecular weight of Nj or CO, divided by 100.
    0.320 - Molecular weight of 02 divided by 100.
    0.440 - Molecular weight of C02 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) + O'.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 nay 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 Bags. International
     Journal of Air and Mater Pollution.  $:75-81.  1963.
2.   Conner, William 0.  and J.S. Nader.  Air Sampling with Plastic Bags. Journal
     of  the American Industrial Hygiene Association.  21:291-297.  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.  2fi:491-495. May 1976.
5.   Shigehara, R.T., R.M. Neullcht,  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 i ter/min





7. dev.a





a % dev.  - (Q -  Qavg)/Qavg x 100 (Must be s|10%|)
     Figure 3-3.   Sampling rate data.
-------
EPA METHOD 10
-------
        IrinsmiUid  LifHt Pulll|
      Biciicirttr Return Sifnai
                                                   a« at«e Zattcv '
                                                                                                          vvn B":t«3is»
                                       »,«,<\9 Qt«.jt
s

f
                                                                                                                                                     1
                                                                                                                                                     »
u
                                                                                                                                                    a



                                                                                                                                                    I
                                                                                                                                                    I

                                                                                                                                                    f




                                                                                                                                                    1
                                                                                                                                                    3


                                                                                                                                                    S
                                                                                                                                                    I
-------
 Pi. *C,
              A, MUH». IO
  ••!• Plulblr  Rag. TealBf, or  rqulvilrni.
 •ith • capacity oi eo u> »o lit*™ < i u> 3 n • i.
 Leak Lot Ihc bat In the laboratory brlorr
 inlng by evacuating b«g with • pump fol-
 lowed by • dry ta« meter. Whrn rvaruallon
 b  ootnpteU,  there  ihould  be  no  How
 through the meter.
  t.1.7 Pilot Tube. Type B, or equivalent. at-
 tached lo the probe ao Hut the aampllng
 rale can be  regulated proporUonal  lo Ihc
 ilaek  gai velocity when velocity b varying
 wtlh the time or • ample Iravene to con-
 ducted,
  1.1 Analyak* (Pwjure IO.H.
  Ill  Carbon llonoiMe Analyaer  Nondta
 pcralve infrared apatu-ometer. or equivalent,
 Thle Instrument ahouM  be  c»emorwtr»l*d.
 preferably br Uw manufacturer.  to meet or
eioMd  manufacturer'1 cnecilkaltoni  and
 that tocrlbed tn Into meUtad,
  t.l.l Drying  Tube,  To  contain  appraii-
 malely KM • of Mm «el.
  • II Calibration Oav Refer la cectlan II
  1.1.4  rnirr  Ai recommended br  KDIR
manufacturer.
  11 8 CO. Removal Tvibr To  contain ap-
prnlfanalcly MO i ol aacarlu.
  •.!.• Ice Water Bath. Fat awmrllc  and
dllcm gel lubea.
  B.1,7 Valte.  Needlr valvr, or equivalent, to
ad|uat flow rale
          *0 Ol Ch. I (?-l-l9 Edition)

  ft .1 II llalr Mrlrr, Rolunrl" or mul*Blrnl
In mruinfr (U flow ril» ol 0 In I 0 Illtr prt
mln *0 OJ6 rim) lliromh NDIB
  (.I.B Rmtrdrr (npdonall. To prn'Idr prr
m«jwnt rrrord of HIHH
                                             4, 1 Ckllbrallon (Iwn  Knaim oonccnu*
                                           lion or CO In nitrogen IN.» lor Inalrunwni
                                           •p«n; prrpurltlrd trmde ol Hi lor wro. uwt
                                           l*o MMIllmMl Mnccnlrmllon* cotmjwotflnf
                                           kpprailm*Lplr to 6O ocrcvnt uid 10 pemnl
                                           •p*n.  Trte (P*n  coiwpfitr*i>on  ihall  nol
                                           ricecd IB lime* the apfillobtc BMirce prr
                                           lormwwe  (tBiMlBrd. The c»l'brmtlon tmme»
                                           •hmll be certified br the maitufwiurer to be
                                           •llhln  il petcenl of  the vecltled
                                            • I «lk» Oel.  IndXsltnf trpe.  • lo II
                                           merti, dried *l ITS' C 1141' F> for 3 hour*
                                            1 1 AKariU. ComnwrcUllr •»lteble.
                                           7.
                                             7.1.1  ContlniKNU  flftmplln«  Set up Utt
                                           equipment •• •hawn In rlvun; IO- 1 nakbic
                                           nire all unimectlot» are leak Irce, Flaer UK
                                           probe lit the rlart it • Mmpllng point tnd
                                           purfe the •mplln* line, Cotmrct the ana-
                                           Ifier and bedn drmwlrw avnple Into the mn
                                           alner. Allow I mlnuUm for the BTMCIB U>
                                           •UbUta,  then record  the  analyser mdlnf
                                           a* required to* the tod proeedura. (See MC-
                                           Uon 1.1 and •> CO, oonlmt ol the •« roar
                                           be detennlned by urin« the Method t InU
                                           tnted am pie prootdunt, or br wdghbii Iht
                                           Mearlle CO.  remoral  tube and  compuUnf
                                           CO, ooneenUmllon  from  the |ai rolumt
                                           •mpled and Uw «ebjhl fmln of the lube.
                                             1,1.1 Inlefraled awnplln*  E*ani*ie IM
                                           npilMr bat Bet up the equipment a* jhovn
                                           In Figure  10  1 vlih Ihc bai dBVonnecWd
                                           F\»fr the probe In Ihr (lack and purir IM
                                          "tamptln* line Comwcl lite bat. making rurt
                                           thai all conmwtloni are lemk irrr Sample at
                                           a  rale propnnlonat to Ihr.  Hack Tflorllf
                                           CO, content of Ihe |u may br determined
                                           by  mint  the Melhod 1 Inlriraled aampl'
                                           procedure*, or br  •rtahlnf Ihe aocarlu CU<
                                           removal lube and rocnpulln* CO. roncentr*
                                                                                               EnvlronfB*nlol ftolecflon
linn fn.m Ihr IHH volume lampird tud llir
wi-lRhl mln »l llir Ilibr.
  1 2 < <) Amly.il.i A.W">hlr (l>r  apparaliK
•n shown In  F1|iitr  10 1. rKHbratf Ihr In
itriimrnt. and prrlurm nllvr-> irquUrd nprr
alloru M drurrlbrd In wrllon I Purfe ana
lyzrr  vllh  N. prior to  Introduction of  farh
•ample Dlrecl  Ihr umple itiram through
tnr bulrurnrnl for the le*t period, rrcord
ln« Ihr rewDnfi. Chrrk Ihr irro and  nmn
M«*" Mler Ihr lr«l lo anurr I hal any  drift
or  malfunction  to  detected. Record  Ihr
aamplr data on Table 10- 1,

•  Calibration
  Anemble   Ihr  apparalua imirdlng  to
FU  Tlir wmplr ron
       H KyMrm ilra-rlbril In Mrlhotl IDA.
        1 I ^ »n,l I 1. miy or «uvrt u an al
trrnalhc In tlir 'Mi t irl and aararltr tikpm

II. RINinoropA*
II. I  MrElroy. Prmrtk.Thc Inlerlrrh HDIR
   CO Analy>4-r, Prrnrnlrd  al  Illh  lielh
   nda Conlrrrnrr on All Pollution. Untvrr-
   illy or Caliromla, Berkeley. CA. April I.
   I no
\\1  Jacob*. M. n , (t •!.. ConUnuou* Oe-
   lermlrullon  ol Carbon  Honoilde  and
   Hydiorarboni In  Air by  a Modified In
   Irarrd Anal>«-r, J. Air Pollution Control
   Anocbulun  WH 110 |i«. Aufuat ItM
1 1.1  MSA  I.IRA Infrared da* and Liquid
   Analyter  Iruirucllon Donh, Mme Balely
   Appllancri Co., Technical Produru Dlrl
   Don, PHtabotfh, PA.
ll.l  Modrb  1I»A. 1I9A. and IDA Infrmred
   Aralytcn, Brcaman InAmmento. Inc.,
   Beckman  Inalruclkm  1115 -B,  Puller -
   Km, CA. October IM1.
Ill  Continuous CO  Monltorlnt  Syvtem.
   Model   AMI I. liilrrlech  Corp.,  Prince
   ton, NJ.
It!  UHOU   Infrared   Oa»   Analywn.
   Bendli  Corp., Ronceverle, WV

                 ADDIHD*
                                                                                                                                                           SPEOTRATIONS ron NDtR
                                                                                                                                                 CARBON MONOHDC AMM.VIEBS
                                                                                                    ouai
                                                    9 roJrulafloa

                                                      Concenlralkm of carbon mowiloe. Calm
                                                    late the concentration of carlnn monoilde
                                                    In the Black ualng Equation 101.



                                                                                     Bq. 10 I
                                                    Where:

                                                    (',„ ,nri  Ci>nrrntrallnn ul CO In alwk. upm
                                                       by viilntnr (Jry banl.M
                                                    (',,, HOI* Com rnlntlon al IT' meamirrd by
                                                       NDIH  tnilyv.ri. pimi  by volumr  al analyst* Jlvldril
                                                       by 100
                                                                                                                                                                       B I. H0-MB
                                             B. Oc/lnlfloiu of frtformumtt
                                            Horn*
                                                    The  minimum  and   mailmum
                                                  rmenl limit*.
                                             Owfpaf  Rlmrkal signal »hlrh to piopor-
                                           Uonal  to  Ihr meaduremrnl:  Intended  lor
                                           connection lo readout or dam procealng de-
                                           vim. Usually riprcBard a> millivolts or mil
                                           I lamp* full .vilr »l a f Ivrn Impedance.
                                             Full i< air  Thr maximum measuring limit
                                           lur • Riven ranyr.
                                             Winirnxm   dflTtaNr    tnallivtlf-Ttte
                                           imallrst  amount  
-------
Pi. M. App. A, M«4li. IOA

  4cnrae*— The litfi'iin of Mtvcmerrt.  be-
Ivevn • na«wur«d *»lue and the true value;
uwallp prpreavxt at ± percent of full acale.
  rime to M purernt fwpwite— The time In
tcr*«| fram a rt«p etiangc In the Input eon
omtraUan al the lartnm»n>l bilct to a read-
In* ot H percent of the ultimate
  Xlw  Ttine (W penmD-The Inlerral he
iwwm tnltU nafnrae Ume and lime to »
pvraent ••^••••i after a rtep incrcaie In the
Intel eonoanmUon.
  fall naM (M »cn*Mf>-The bilerval be-
IVMD Initial raapMM tte» and time to n
                afler a «tep dcei-eaie In the
  Z*r» DrVt— Th*  chao*e ID
ootpnt mvr a «Uied time period, uauall? 34
noon, of unadjusted cootbiuoui operation
•ban UM taput ennemtratlon b ano: uaual
IT expnaaMf a« pemmt foil acale.
  9fmm  ZW/T— The  chance In  Inrtnnoenl
output o»wr a «UI«d time period, umallr M
hoota, of unadjualed conUnooui operaLkm
•hen tlw Input rawantratlon !• a tUted
"Ttf*Jf value; ummll; eipnaavrd mm percent
fug acale
  JPmctffton — -~1TW WSffHB^ft  Of BCT^MfOOMfftll DB*
tvccn repealed nwaanreaienu of the awn*
OMmntratlon. cMpitaatil ai the aterai« de-
vtatlofi of the afettle reauiu from the mean.
  ITotac— Spootaneou*  derutllon*   from  a
mean output not cauacd by Input oonemtra-
                 maximum deviation  be-
tween an actual Instrument readlm and the
raading predicted b» a ctralfht line drawn
between upper and lover calibration point*
                             or  C*B*OM
                  Miom  in  CBmrrrno
                   nioa Moiirroaino Sra-
       I. MffHcohUtttanA Principle
  LI AppHcaAtHlf Thai method applla to
the nteaiuirrmefit of carbon monoiMe 
at petroleum refmerteB. Thto method mrntm
mm the referwnce inetnod In the relallte ae-
niracf  teat   for  noodtopemlve  Infrared
(rtDDt) COflonttnuoui emtaalon nonllorln*
•ntena  |
naii taMBil MI Ifinni Ilinav. flu atinrJuil iMiii
atlon of the mean teas*** blank vahHa.
  II  InUrfemamt.  Sulfur  omtdna. niuto
oikta. and  other aeM BW  ralerfen with
                                                                                             Hill U| TIN.
br u««nliM the •••jiliil am* Uiraugh an alaa-
Ime potaawum peiiaaiaiiiaitr atnibbtns a>
luUon. Carbon dkwlde  dan »fler prepara-
tion to avoid etoravrfe blank correction  The
•ample* In the TedJar ' bag *houM be (UMe
for at least I  month If the baa*  are leak-
free.

              2. Appomfaf

  2, / Sampling. The ammplln* tram ki *hown
in Plttirr lOA-l. and component  parts are
dtacuaacd below;
                                              ciiomioi
                                               net i*
                                              moil i»
lute  the endoraement or recommendation
for  me by the Environmental  Protection
                                                       L
                                                                                                     k^—ln** v*ivt
                                                                   cmiaiuic SMI in
                                                                      Wf INCI M
                                                                    figure  IOA-T.  Sampling
                                                                                              wool
                                       '•'.1  Prota.  8taliue*B  rteel.  rtiealhed
                                                or equivalent, equipped with a
                                                plug  to  remove  paniculate

                                       I '.2 Sample Ctnuflflonlnp Skitem. Three
                                     Otenburg-Bmllh Implnger*  connected  In
                                     ""ei with leak-free connection*.
                                                                                         Z.I.S P*mp. Leak-free pump with eUhileai
                                                                                        •teel mni T«non part* to lran*»ort "•™Pj«
                                                                                        •1 • How rale or MO ml/mln U> the fleiiwe
                                                                                        bag
                                                                                         IH  Sarpe TdaJt  Installed  between the
                                                                                        pump and the  rale meter U> eliminate the
                                                                                        pulsation effect of lh* P"mp on lh«  r«l*
                                                                                        meter.
                                       768
                                                                                                                              tan
-------
EPA METHOD 6C
-------
                                                                                          T
n «0. Ap». A,

  The aampllna: train In ui»mhlr<1 a.* slmain
In Figure •* 1. e«crpl Ih' iiot»roi«««'l b«b
birr  to not twinded  The probe miiM br
heated lo •  temperature lur'irkriil  In  pre
• rnl water eanrienaallon mm) mull Include  *
IIILer Irllher In Hack owl of alack, of bull.I
lo prrrent parliculale  enlralnmenl In  Iht
peroBidt tonptngera, TIM electric aupplr fix
the  probe heal ahauld be eonllniioui  and
•epwale *roB» tne limed  operation of  Ihe

  Adfuat I he timer »wiuri  to operate in the
"aa" poaNion Inmi 1 lo 4 mlnulci  oo •  I
hour repeating cwde or other cyrlc apertftrd
In Ihe applicable regulation  Other ttoaer se-
quence* MMV be aaed  wHh (fir rotricitan
that (he MW aampt* •otamc coMeded to be
  Add arid water  u. Ihe Unk  until the to»
ninger* and bufcWm are ravefetf al leaat
i*«-thlrdB nil theti length.  The  Imprngcra
•Ml bubMrr  tank nut be emend and pro-
tected Iran InWnae heal  and dJrcc* tun
Hght.  II fracatng amUllona ektet.  tne In
ptnger aolulron and Ihe water balh  muel be
protected,
  Nora aaj»pHn« mar br  rondurltd ran
Knianatfr If • taw  Hoar-rate laoiptc pump <»
u>  «• nl/mln  lor the  reagent volume* *
atrltara In Ihto anethadi  li  ward  Thrn Ihe
Ibnei iwltch to MM neceatarr  In addition, II
ihe aampte pump to dertinwf lor canalajM
rale lampllng. the rile meter  mar br deltl-
rdi. The total gaa  volume collected ahoutd be
 between 19 and «O lltera lor irw amount* ol
 BBfltplIng   reagent*  prearrllied  In   Ihto
 met had
  4.1 J l*ak Cheek  Procedure   The  l*«*
 check prot*du*« to Iht Mm* •• dacrlbed In
 If ethn« •. Bectlnn • 1.1.
  f I > Bv»pt* Collrvllon  Rerocd Itw Ini-
 tial dry ••• newt rndtnt. To brtln utn-
 pllna iKtottlnn Ihe lip ol the piobr  •• «hc
 •mmr*ln*  porrti   comwl Ihr probe  u> the
 flnl tanptnter  «* flltel i. •'«> xl*'1 lr» "<«'
 uid  Ihr  »«t»l>tr  pump Adjim  Ine umplc
                        l
                        bf
          40 Cm Cti. I (7.1-19 l«ll*«>

hli-|)S  in  lltls srrllilii |II3> lor  siMirviivr
nitis
  4 1  .lamplr Kn'utrny Tlir |«fiwrjiires fur
umnlr  rrrt»vrr» ItmiiMiur  mrKSiiirmrni,
prroilrtr lohiiloii. «IH| f«>. •tnorbrrt atr
llur wnr u l» MrllxnJ «A. HerlhMi « 1
  I I  itamplr Analy^li  Ariklril* of lite per
nildr Inplrwrr iohitlnw b Irw ume  •> In
Melhod i. 8ccll«n 41.
  44  QuaMIr Auuruirr <«*' Audll  Sun
ptn  Only alien ihli mcihod U mcd lot
^,^,-pji— delrrmlmiMm, obtain an  audit
MOVfe Mt u  directed In Bectlon  l.K ol
HMttMd  fl. Axialrie Ine  audit  kuapln ai
leMI  one* la* r*tir M d»»i ol (ample col
tertion, ajid report the raulta •• directed In
        44 ol  Hetnad • The UMJrK per
                      air>ea  tluUI per'onn
Ihe BiidH aimlr*aa II "»r» Uun on*  Mulpit
tuilummd UM aao«p«e  MMlr*> during Ihe
M dtn Miapikw prrtod, octi •ntJyii ahall
nerform UM W0I kmltna and Ul «udli rt
•ulU  •onll tot reported Acceptance  criteria
lor Ihc  •udU  rejBilU mtt the  Mine  u in
Method I
Inirlr
PI. *o,
                                                                                                                                                                     A. M«n,. tx:
                           llir
    »e thai Ihe tuner I* oprrallni a. Intend
ed. I e . In the "on" puuli«n lur tlir dralied
period and Ihe r.yrle rrpraU a» " 'jiilird
  Ourlna   tne   14 rwwi   rarnplina:  period.
in-ord the d»v «a* rwrirr Irmprralure one
lime between tOD a m and 11 OO a m., and
Ih* tjaromelrk- preuiirr
  At Ihr conelimloii of Ihr tun,  lurn nil Ihr
llmvi  and the  aamplr pump.  rrmi»r Ihe
IHOtar Irom Ihe utark. ami feccud Ihe  Dual
|U nrlrr lolumr r'adlrif fuiMliui  a Irak
rhn-k aa drartlbrd H> Srlliin «  I I  If • Irak
ll lourwl. Hold Ihr Irsl run III IINC |M«rrdurrs
•vrrplabfe La llir ArlnilnUIrir.ir  In  •(IJiitl
llir umple vuliimr fin Irlkair  Hr|H-al llir
  • I   Mctrrtn* Brctom.
  B I.I  Initial Cmllbralton  The Inllltl Mil
 Dnlkm lor Ihe MtUioK meterrna nMlem to
 ine ome ai tor kin hod •, Section S I I ,
  S I  1 PerUMttc Ckllbrktron  Cnccfe  Altn
 JO dari ol operallon ol the tnl train, ron
 duel  • c*JMM»ilon rhert a* to Section B I I
 abore. rieept lor the  loltovilna vkrUllona
 1 1 1 The leak  check to not to be condttrUd,
 ill three or morr ttmlulkMH ol Ihe drr •"
 meler mini be uaed. and 111 only two rnde
 prndent  rum need be  made  II Ihe ealibiB
 Han  factor does no* deviate by morr than ft
 percent from the  Initial calibration  factor
 determined bi Section S I.I, then  Ihe drr
 |U meter voliunei obtained durlnfl Hie teat
 term are acceptable and  u*c ol the  traJn
 can conllnix. II the canbrallan latlor de.l
 alei  br more Inan I percent, reeallbralr the
 meterinc mffUm mm In Section 6 I I, and lur
 Ihe rah-ulallofM lor Ilie preceding M da»i ol
 d«la  u*r the callbrallon fartiir I Initial or rr
 rillbrilkml  that   H*Ws  Ihe  »oarrr  (ax
 oolume tut each le»t inn Hie Hie laird rah
 brallun factor lor iu*rerdin« lr»l*.
   » 1 Tliemionieleri   Calibrate   Maiiu<
 mrrrurv  In |laat IhrrmunwIiTt InUlally *IM!
 al M) tUr Inlervab
   1 ] Holamcler.  The rutamrtrr nerd lift
 br calibrated, but iliouM br rleaiM-d and
 nialnlalned accurdliMi; U. llw maimlarlurcr'i
 liulrurtlona.
   S < Uaranirlrr  Calibrate acalnal k iurr
 rnir baromrlrr Inillally ana tl JU da> U»l«''
 «al^
   »S  Ilirliim I'rtrlHilial"- SnlillM.li  Sl»«
 tlmiUr  tin-  liallnni   ueiclllwrale  Milull'""
 •Cihui  M nil of  sianilaiil iiilfuili  ai l«t  '»
which IOO ml ol loo percent Impropanol has
orrn added.
4 Calrktaflom
  The nomefKl>tfir« and ralrulallan prore-
durea art  Ihe tame ai In Method aA vilh
IM lollmlni earvplloni:
p_  Inlltol baronrtric pinatue for Ihe tnl
   period, mm H«.
T. -Abaorule owlet lempeiaiur*  for  the
   teat pertodT *K.
1 CinuJtixi Male rVocrdare
  The emtoalon rale procedure, to the mo*
ai dnerlbed In Melhod «A. SecUon 1, eicept
thai the Uaier to needed and to operated aa
JuciloeJ In Ihto  metnod Onli  "hen  Ihto
method to vaed for cmnptlaon  determlna-
llom. peiforam the QA  audit analraca aa de
atrMied bi Beet Ion 4.4.
• BlMuwraa**
  The btblto«rap*iir to the aam aa deacrBwd
M Method *A, arctton 1, a-Mh the addition
of ihe loltovtna
  • I  Butler. Fianb  aV  J.B.  Knoll  JC
Bu««i  MR Mtdaetl. and W. Maaon  The
ColUtioraU*e Teat of Melnod «B. Twenty
Pour Hoar   nnalnto   of  BO,  and  CO,
JAPCA. Vol. II, No. II.OctobM IflU.


Mirnoa 1C  nemniaaTliM o* SviruB Ol
    OBiaa   bfiaaioa  Ftoai   Btmitommmt
   Boimrm llminumintTiL  AftLwum F»o-
   counl
I. 4ppHr»Mflf I ••* Pflmeifl*
  II  JpaflnMni r Thto method to aacittca
Mr to Ihe  detrmlnauon  ol wlfin dkaaUe
(W».l tmnecntratlarM bi conln>»Hd and toi-
tonUDlWO emtoalona Iroaa ftatlonaiy aotircn
onlr when aperifkd •NJdn Ua>
  1.1  Prmcmie. A «aa mil ..... tilr to
Ir eilnrtcd Iron  a Mack, and a portlom of
the aaaiiili to convered la aa taattnaaental
•nalran  for detetMinaUon of HO. caa eon
eentraUaB Mtaa? an »ttrae»o»»t IUV». oondto
prndte tofrared INDIRI, or fluoreacenee an
klnet  Perfomaamoe apecllleaUQna and leal
vroordurca are  provided  to  enaun reliable
Ua La
                                                                                                                                          mrnt srilem  pur  a  wrll dnlgned intern,
                                                                                                                                          Hit- minimum drimaub limit tlioukj be leai
                                                                                                                                          than 1 pr-rcenl ian
                                                                                                                                          J  Itrfimtliumi
                                                                                                                                           JI MeBBiiremnil  Kviirm.   The   total
                                                                                                                                          equipment required lor the detcnainallon
                                                                                                                                          of  gaB  ranmiirallim  Thr meaaurement
                                                                                                                                          iratem constil* ol il» fuliuwlng makw tub
                                                                                                                                          •yilenu
                                                                                                                                           1 I.I  Sample Interface. That portion ol a
                                                                                                                                          •rslem uard  for one or more of the follow
                                                                                                                                          Ing: aampkr  arqutolllnn, mranto tranapart,
                                                                                                                                          •ample condllhmuig. or prolectlon ol Ihe
                                                                                                                                          analvtrn Irum llw elfect* of the alack ef-
                                                                                                                                          fluent.
                                                                                                                                           1.1 1  Oaa  Analrter That portion of the
                                                                                                                                          araiem thai  arnm the IM  to be meaaured
                                                                                                                                          and generate* an output proportional lo III
                                                                                                                                          concentration.
                                                                                                                                           JIJ  Data Hecordrr. A (trip chart record
                                                                                                                                          er, anatog computer,  or digital rerrxder for
                                                                                                                                          rrcordlng rarmmrerneni data from Ihe ana
                                                                                                                                          Iriei output.
                                                                                                                                           11 Span The upper llmll of Ihc |ai con-
                                                                                                                                          cent ration meaavremenl range dtoplared on
                                                                                                                                          the data recorder,
                                                                                                                                           11 CaNbrallon Qai. A known concentra
                                                                                                                                          lion of a taa  In an appropriate dlluenl gaa.
                                                                                                                                           1.4 Analyser  Calibration  Error. The dif-
                                                                                                                                          ference between the gai conernlral Ion ri-
                                                                                                                                          hlbtted br Ihe gu analrwr and Ihc known
                                                                                                                                          foncenlrMion of Ihe raUbratlan gai when
                                                                                                                                          Ihc callbrallon gM to Introduced directIr la
                                                                                                                                          the analvaer.
                                                                                                                                           IB Sampling  Bratera  Wat  The differ
                                                                                                                                          cnce between the gaa concentraUoru eihlb
                                                                                                                                          Hed bv  the ror-aaurenimi  BrUem  »her>  a
                                                                                                                                          known  cancenlrallan ga* to Introduced al
                                                                                                                                          the outlet of the aaimpNog probe and when
                                                                                                                                          the aame gaa to Introduced dUectlr lo the

                                                                                                                                           ].• Zero Drill.  The difference  In  the
                                                                                                                                          measurement tratem output rtadtna  Irom
                                                                                                                                          Ihe IrriUal calibration reapero*  al the arm
                                                                                                                                          concentration le>el alter a Bated period of
                                                                                                                                          operation  during  which no uraKneduled
                                                                                                                                          maintenance, repair,  or  adtuatmenl  took
                                                                                                  1 I  Analr'kal  Hanac  The  analrtlcal
                                                                                                ranir to  determined br the tnalnMaenlal
                                                                                                aealcn PM thli method, a pot I km of lhe> an
                                                                                                Mrilcal range  to Belecteit  br chooalrai Ihe
                                                                                                Bpan ol Ihe monltorlnf irilefn The tpmn ol
                                                                                                ihe monllorlnf  aiBiem ahall br.  aelected
                                                                                                •urn that Ine pvtlulafll iraa concenlrallon
                                                                                                *qt>l»Bl*nl u> Ihr emtorton itandard to not
                                                                                                >m than » percent ol  Ihc apan  If al any
                                                                                                llnw duilnt a run the meuurcd IBB conren
                                                                                                daiiun eicectta Iht apan.  Ihr run iliall br
                                                                                                roiuidried Invalid
                                                                                                  11  Hrna(ll»IHr  Tlie inliitmum deLrrUblr
                                                                                                "inn drpenda on llir aJMlyllral raiigr, ai>aii.
                                                                                                ••Mt  alBiial Lu IM*LW  lallti  Ml  llir niraAiiir
                                             11  Calibration Drift  The  difference  bi
                                            Ihe  meaaurcracnt  ir*lem oulpul  reading
                                            from  Ihe Initial calibration rcMpana* at a
                                            mid range canbrallon  nlue after  a atated
                                            period ol operation during aihtcn no on
                                            arhrduted malnlenant*, repab, or adluat
                                            meiil Look, place.
                                             1 •  Hemponae Trme. The amount of time
                                            required fw the meaauf emenl »»atem to dto
                                            plar »S percent ol a ««i chanfe ta (aa con-
                                            rrnl ration on Itir data recordrr
                                             IB  Inlnlrrrnre  Chrrt A method lor de
                                            in-llna  analrlh-al lnirr(eie«cr« and eirra
                                            slvr littatrr, iliruiiili dlirrl romiiarUon ol gu
                                            riHH-riilrallinu  prnnlded br  Ihr mraaurr
                                            mriil sr^lrn, and br  a miidllied blrlhod •
                                            itdirrdiirr   H>r this   rlin-».  the  rnuulllrrt
                                          702
-------
n. M, App. A. nUtH  «C

Method  • aamplrs  Brr argnlrrd  si  Ihr
asmplr br PUB dtarhane trot
  I 10  Calibration C-rve A  irsuli •«• 	<
..Hematic method of nl.WUhln. Uir rrla
llitroihlp between Ib* anal|»r rrwoiur and
Ihe actual IBS ooncenlralkm Inlrodurrd lo
Ihe analraer
4  sreu.mwaf  SgHrm  Frr/omasrr Sprrt
/Icallomi
  I |  Amlntr Callhrallon Error  Lria than
i I percent of the span Iw  (lie  lero. mkt
range, and Ithjh range caJInrallun aaon

percrnl of Ihe ap»Q l« Ihe uro. and Bud a
high range calibration iases
  11  Zero Drtfl. Leas lhan  1I percenl of
Ihe apan over the period of each run.
  14  Calibrate*, Drill.  Irm lhan il per
rent ol the  apan over  Uir  period ol cacti

T»  Interference Chert  las   lhan tl
pereead ol Ihc modified Method • result for
                                           Ihr i|
                                           ,1,11
  • .I  Measurement ByHcoi. Anr aaeaaure-
nenl •ratrn for BO, lhal raeeto Ihe speclfl
OBlranj ol Uua Bart bod  A BehemaUrof an

figure «C I  The  uarnlhU aumvancmt of
the  meaaurnaent  irrten  an  Jeaviltaal
beta*
  111  Hwnptf Probe. Olssa. Malnlesa steel.
or equivalent, ol mffkhml  length lo  Ua
verse Ihe  aamplr  potnU.  The
probe ahall be healed lo prevent conocnaa
Uon
  6 II Sample Unt. Healed 4rafflctenl to
prevent  eondrnaaltoot  lUlnlea  steel  or
Teflon tubing, to transport Ihe sample CM
U the moMun? reowvai ifaum.
  B I » ftaBptc- Transport Lines. fUalnhtas
steel  or  Tenon tuMng. Lo trampurt  the
sample from Ihe motaturt lemoval iratcm
In Ihe sample pump, atmptr no* rale con
Irol and aample gaa amanlfold.
  Ill Calibration  Valve  AsacmMr    A
three ny valve asaetaWr. « equivalent, for
Mocfclag Ihe  aamplr gas flu*
DM caUbraUon gaaea lo Ihe
      i at Ihe outlet ol the sampling probe
             40 CFI Ch. I (7-1-V9
        |.(>i".»l III Uir AilnilnlMlBliir  Tlir ilr
          K'lliil»«i«  aiial»»er« Hial
   inruinr raiwiilrailiMM IMI •  mri limtla mtint
   ,11 . ...-1  bub «-4t, BiiBlrfrr  uperaled ar
   n»dlii| i« Urlhud 3A b lued to obUIn al
   nniltii>^aiu m»a»nr»mT«>l< and "3 I Ihe pol
   liiiuil/t-**> nwaAurrmrnta air turd lo opfr
   mlnr emlMlufti In unlU ol the ilandaid
     a I  I  Partkulalc  Filler. An  in alack, or
   lu>«lrd laitfWdenl l» pre»rol »"
   ulloiii oul ol >Uck fillrr The filler
   buroilllcal* or quarli llui  aioal,  or
   liber mat  AddMJonal flllen  al the Uriel or
      rl of  Ihe motaturr irmoraJ iratem and
       n  «hall be
   fabrkued of RkaierUt* that art noAreadlw
   to UM vac betna MBpled.
     » I V  BkBiple Ftatnp. A anfe-lree, purap, lo
   pull lite aaaBpic ca* through Ibe aiatcaa al a
   flofe  rale aulflrtnil lo  aalnlavlBt  Ihe  re
   apoiw Ibav ol  the meaaurenvrnt  iratem.
   The pump mm* br oooatrurted of anr i
   rial l»ai to laiojeacave lo the aaa bring i
  1.1.1  Moisture Removal BiMera A rtlrtg
evalor trpe condvuavr or vtmllar device le.g..
piiiB«sllon  drvert. to reaaov
conimuouslr from Ibe aample IBS
ojalnlaJnIng —fr^r*' contort  brli
nwirlrivam and Ihe aanple IB* The
lure itmuval •yawaa k not  nui'aaarv for
analrsera thai  can measure gas luammra
lion* on • Bet baam, lor I heat analraera. 11»
heal the saaiplr Une and all Interlace cart
pOnBRts IBJI to the Inlet ol the aiialvarr sulfl
rtentlv  lo prevent  rondeiuallon, and I II o*
termlne Ihc ajioWure corrfenl  and eorrrrt
Ihe oteaMied gas nmrenlrBlhana Ui a dri
           •ppraprlau meihathi. lubfrri u>
  111  Aampte  Plc«   Rate  Control.  A
•ampll fto« rate conlrol val.e and rotarar
ler, oil «prtvalrr»t. lo maintain  a ecawUnt
sampkng rate arlthbi 1C percenl.
         The leater  may elect lo Inatall a
              regulalor  lo  sa*lnta»n  Ihe
      • gaa manifold al a canatant prrarsurr
In orcfcr Lo protect Ihe analvMitil from
ovcrpresBHrmmUon,  and  lo
need f ir flaw nle ad»u*tjrnrrn
  1.10 Sample Oas Manifold  A i
gnnlfirid. Lo divert a portion of  the i
•mi auram to the analyaer, and the remain.
der  Ui  the tar pam dhKhgjge  vent.  The
iainpli>  ggg nmitlloM anouM asm tarJude
provWonv. for mtrmtudng caJUaraJLIan gaaea
ghraetlr la the analraer. The •anllorfi amr
be conatructed of anr material that b POD
reacUie to the gaa being anamlcil.
  1.1.IH  Ow An*lner  A If* or MDIR ab
•orpUeei  or ftaoreacence analFaer. lo deter
mine cootUMOoalr the SO, oonoenUaUoo to
the B»aw*e gaa stream  The analraer shall
awn Ihe atwIkaUe pcrlorauMiee spedfin-
Uons   br rrrardrd manuallr  11 thai Bllerna
liur u used, Ihe reading* »hall be obtained
al rquallr  ipaced Inler-rala  over Ihr dura
lion ol Ihe sampling run Vow sampling  run
duration* of teas lhan I hour, measurement*
al I mlnulc Intervals or a mlmmiUB of H
mraaurcmnila. «hlcheTer hi leas n*trlcll.e,
ahall  br obtained POr sampling run dura
(torn greater lhan I hour, measurements at
1 mlnulc  Interval* or  a minimum  of M
gifajurrmm'r aihlchevcr hi hcsa rcatrlcllve.
ahall be obtained.
  I.I  Mrthod •  Apparalus  and HeagenU.
The  apparatus and leggenU  deacrlbed In
Hrthod •. and ahoarn br Ihe acheraatk of
Ihe aampMm] tmoi In Figure iC 1, to  con
duct Ihe Interference check.
  • I  8Ot  Calibration Oaar*  The  csJmra
lion gaara for Ihe gas analvwr almll be BO,
In N. or BO. In air Allematrvelr. 8O./CO,.
BO./CK. or SO,/CO./CX  gas mlitura In Hi
•ay be uvd. For ftuuttateme baaed BtuUvm
era. the  O. and CO.  concenUaUons of the
rmlmratmn gaaes aa Introduced to Ihe  ana
Iner shall be Mlhln I percenl labaolulel O,
and I percenl < absolute I CO, ol Ihr O, and
Co, eorKenliallona ol Ihe cffluenl sampteB
as Intradueed la Ihr analyicr Ailemallvelr,
for niioiearence-bated analrten. uae  call
braltott Merrda of BO! In air and Ihe nomo
granhs provided br Ihe vendor to determine
the aunvrhlng correction factor ilhe efllu
erri  O, and  CO, concenlraltona  must be
knoantl. Uae three calibration gage* aa apecl
 Ikdbrloar:
  • II  High Range   Oaa   Concentration
«mdvalrnl lo t* to gg percent of llw apan.
  til Hid Range   aaa.   Coneenlralkm
equlvalenl lo M lo • percent of Ihc apan
  1*1  Zero das.  Concentration  of  less
lhan g.U percent of  Ine apa/v Purified sca-
 bhnu BUT may be uaed fat  the am* gaa by
paaatng  air  through  a  charcoal f flier,  or
 through one or aaare tmpfaigcn containing •
 solution ol 1 percent HiO>.
g m*m»mmuml Snttm Prr/armmmee  Tr§l
                                                                                                                 ft tO, A.p  A.
                                                                                                                                         *C
                                                                                                      I 1
        Alli-riiBllmr Nlimhrr 1  Us* ul r«ll
hralKm «BM> inn i««-|»«'*il •rc<»rt»n« la P*«
torol Nomuri I If Ihta alternative ii rliuaeii.
uMaln ••* mill urn •llh • annularlurerB
Inlfiwtrr  mil  lt>  r«rr«l I 1 percent ol the
la« tmtuf  wtiltln • month* talarr the emto
• km Inl  analrv rarh "I  Ihe ca,llbrallo«
•un In trlpllralr •»•«• Melbod •  €TIUth»»
1 In the BIMUgraphr dearrlnea procedures
and techniques that  mat be  !•"» *or  *'•'•
BJuiittB Record lh* mulu an • dal* *e*t
urr «C 4.
   Norm A calibration curve rttmWtahcd prior
 lo In* mnalrcrr nJlor«tlon rrrm ehrem nay
 be iaMil lo converl the •nalrwr iiwyutmr lo
 the mul««lrnl tai conrvmrBl Ion Introduced
 lo the aiulrwf  Ho*r>rr  Ihe aaBM raft ft
 Uan pforrdnrr limit br uant f« all rinuntl
 •nd  callbrtikni   mraaiiremenu   obtained
 diulnf Ihr Inl.
   • 1 1  Thr   knulrur  Hllbra,llon   error
 <-h«r» ihill br roruMerpd Inialld If Ihr IM
 rone ml rallun irc arllon, and rrpcal
704
                                                                                                705
-------
 ft. M. Afr». A. fcUit. AC

 Ihe  inalrrer rallbrallon t-tn.i • ln-rk  until
 arrrplibtr performance Is •rliirvrtl
  • I  Sampling  SyMem  Illax  I In-, k  |Vr
 lorot Ihe Buitpling irilem blu rliri'k by lit
 traducing rallbratlon gasr* al Ihr ctllbr*
 lion valve Installed al tiir outlet ol Ihr uun
 pllng probe  A UM-O gav and erfftwr flu  mht
 ruigr of high ran** |u.  •liirlimvi  niuai
 rloarly approilntatea I In- tlfhtelil  rmtren
 irmllona. ihall br uatd for Dili > lirra u lul
 low.
  • «.I  Introduce  lh» upacalr  calibration
 gai.  wid  record Ihr |U ranrrnlration dto-
 played by Ihe analyzer an * form timltcr to
 Pta-ure- tC-t. Then  Introduce  rero gu. and
 record Ihe CHI concentration dlaptayrd  by
 Ihe  analyser. Durlm Ute campling *y*um
             operate  the  crUrm  al  the
            illna1 nil*.  and make nn adluxi-
       U» the  tactauieiMni  ayttrai  other
 than I hoar orri-aiti-y (A achieve proper caJl
 oration gki flow rala at Ihc analywr. Alter
 natejy Introduce llie utio and Mjiarale gMaa
 until a  atcMe revpanar  b achieved*.  The
 bnMjr ahall detcmlnr Ihe   meaiurrmcnt
 lyttein rrapan*r time by obaervtng the Urn**
 rn]ulr«1  lo  •rhtrvt • •table  miim*ae lo.
 both Uw »rro uid uoaralr |un Note llw
 lonaYr of Ihc  durtna
 Ihe kaMlBl fleM teat on »  parlleuhMr aowrcc
 r*trtofr  Hetaln  Ihe  rmilim. and  rcfiort
 itvn*  with each  l*ml  perlorned  on  lhal
 anorec cMevorf.
  If  an  tnlfilttmct rheck  to  belnc  Oft
 mraMil.  aa»f•»•••• ronlalnlnc I percent  llt<>,  and dry
>a* m-trr> a* ihovn In Plpure W.' 1 fniilall
in* auBplliM t'Bln lo Mtialn * ounplr •! the
mvaAiiirntenl  •yttrm  ftafiif>lr  by pace 4la
rhtrcr  *enl  Hfrord  Ilir  lnill»l  diy laa
tmru-i rradim
m  ti r ,  * IO
  'I'lir *ain
xamr a.v fui
          40 CFt  Ch  I (7-1-19 fdilion)
irlliif iilniir II Hi i (h si cn< k.Mi
•mi bruin uniitliiii it ilu Mm
dufiiig  Ihr  &Amr>lfiig  syhf*"i
Maintain constant lair >am|il
      tl i durlrm Ihr  e nllrc  n
      limr prr run ihcfl br Hi
Mrlliod  • plm  Ivlrr thr synli-m rriimnir
llnw. KOI rarh "in uir only ihov mraaurr
nvrnu obtalnnl iliri  l»U-r irxKmar Km* ol
the ntcaiutrinm) •rttetn hai tlkpanl, lo de
iermlne the avrra^e rffnient concenlrBllan,
If an fnterferenrr check to being perfotmrd,
opm the Oo« control valve on Ihr modlftrd
Method  • ttaln rancvrrenl  *llh  thr Initi-
ation of lite kkimmnt period, and adHisl Ihe
flo* lo I liter pet oilnolr I t I* prrcrnl I,
  cffofi: tl m pump to not un*d in the modi.
lied Method * Urnln. caution ahouM br rirr-
ctard  In  •AkajUha  the Oo»  rtlr linr*
oirrpreaawrtoailDn  of the  (mplnccn  m*r
i.a>»« Inakaar bi Ihe  kBpfcnacv train, result-
ln« In portUvely Maaid raulU)
  1 • Zero and C^NbraUon Dtllt Trmia. Im.
rordlately praeedtn* ami lolloailni each  run.
or  If  adluMlaBenla arc  m coami  for  Ihe
•eaaurcfacnl •>•<€•  dMHm (he run. repeM
the •tmpHni ivMcai Mac check procedure
deacrlhed In fiectlon  t « rMakc no adtucl-
nmU to the  meaMirenent lyMem until
after  Ih*  drill  check*  are comptetrd.)
Record and anatnrr  * ratMNWei on a form
Umllar to Pkfure *C •
  t.t I  II either the aero or upatale callbra
lion value eiecedk thr akiBpilna; •!•!••  Maj
•prclllCBllon, thru the run to conatdrml in-
valid Hrpnt both the analyapr calibration
error check procedure tBmlon • Ji and the
•anpllnc lyatcm blai check procedure «fjre-
llofi • t » belore repeating the run,
  1,*.I  If both Ihe aero and Mfavalc callbra-
lion valuca are vlthln the laaiplhn •yatem
fata* apedllcailaa,  then  uat the average of
the InltlaJ and final bto* chock nlua to cal-
culate Ihc (a* ooncentraUon lot the nm. If
Ihe atro or Mpmtsaje aaMbratMn drift value
e. cento In* drift IbaMa tmtrtt on Ihr differ
ence  btl»r»n  Uw amnllng  lyatem  btoa
check  itanonam kMMedtalely before  and
after the run, repeat  both the analyaer cali-
bration error chock procedure (Section • ti
and (he aBiafiltin  cyatetm bla* check man
dure  iSn-Uon «4i  before conduct In* addl-
llonal ntna
  1» Inlcrferenot Check  III prrlurniedl.
After completing the run, record Ihe final
dry Ifti meter reading, meter trmpr««lurr
and barontelrlc preaiiire. Recover and ana-
>rtf the content* of the mldgcl Implngm.
and drtermlne Ihr tK>> au murrntralkm
using (hr prorcdurea of Method t  ill ta IUM
nnraaary  lo analyze   EfA urilmmaiM-r
•udll lamtilrx lor Mr I hud * I llrirrminr Ilir
•vrrM* cai runrrntrallon rilnbltril by  tlir
analyzer tot  Ilir riin  M tlir iftn rtMii-rntr*
                                                           oeiMonlol PfOloctUn Aljmtcf
lliHi.1 fiffivldi'd  by Ihr  analyier and  Ilii*
mudlllrd MrlliiKl  8 «lhl«lrrl
• fmifnon Cafrvlafron
  The av*ragr gai efflurnt cnncrnlrallon Is
dtlermlnrd from Ihc averkgr gai ronrenlra
Uon dtoplayrd by  Ihc gai analyiri. and b
adlusted for the arro and upacalr aampllng
•palnn bias checkj, a* determined in accord
anre vllh Herllon  II The arerage gar eon
cenlratlon dtoptoyed by Ihr, analyier may br
drUrmbMMl by Integration of the area undrr
Ihe curve for chart recorder*, or by averag-
ing all of Ihe * I fluent mramrrntrnu Alter
natively. Ihe  average my  be  calrulaled
from  reeaavreraenui  recorded  at equally
                                                                   Where
                                                                                                                       App  A. M.M,.
                                Eq «C
                                                                   ('•_   Eflliirril na.1 fMirrnlrallon, dry bail*.
                                                                      •mm
                                                                      pprn,
                                                                      prn,
                                                                   C    Avrragi- iu, runccntrallon Indmied by
               ,            n
    gai analyzer, dry baato. pnat.
                                                                      gai analyzer, dry baato. pnat.
                                                                   ( . - Average ul Initial and final iy*t*m call
                                                                      oration Mai rheck rnma»i.» for the *ero
                              Inlervato over the entire duration of
                       Ihe run. rot ammpilng  nin owmtloM of leal
                       than  I hour. meuureiaenU at I ftilnule In
                       tervato or a minimum  of M ovraaurrmenii.
                       •Mr he re r to lfo> rcatrlrtlve,  chmll be uard
                       Por •ampllng run durallona greater than I
                       hour. memnrrmenU «l 1  mhiulr hilervato
                       or a mlntraum of ag nwaaurenienui, Bhtch
                       ever to lea« realrfcllve.  ahall be ua»d. Calcu-
                       late  Ihc effluent gal  concenlratlon inlng
                       Equation *C I.
   ••«. §•*"**
C.     Average <>l tnlitoj and  final lyMem
   callbrailiin blai cheek roponan for the
   upBCatr evllbrellOR car, pom.
C!_ -  Actual  concciMratlon of Ihe  upacale.
   callbrallni> ga», ppm
t.
                                              I. TraccBtMllly Protoct^ lor  ErtaMtohlng
                                            True Coorrntr«llon» of Quev Uatd for C«ll
                                            braHom and  AudlU of Cundnuow  Source
                                            Emualon Monllori  Protocol Number I US
                                            Environmental Protection Agency. Quality
                                            Aaurure   t)ivl*lun.  Meaearch  Triangle
                                            i^tk. He. June irir
                                              1. Wnllln.  frier R  and  J.  W.  &ra«n
                                            Method* lor Col feeling and Analysing Ou
                                            Cylinder Bamplei Hourcc Bvaluallon Socle
                                            ly NewtleUe,  Jillft II. Beplcmber
-------
   ft, tO, Ap*. A. M*Mi. 6C
            40 CFI  Cfc. I (7-1-19 Edition)
Environmental Protection Ag«nnllllr*tian
                                                                                                  TrH prfB
                                                                                                                                               Run numiirr
 Dilc
                                                                                                                                                   cri
                                                                                                                                                   i
                                                                                                                                                   al
                                                                                                                  Sntara
                                                                                                                 c^>»*u
                                                                                                                                                                                   tMI
                                                                                                      ( or Nitvonm
                                                                   IMI Pkoa 8i*tiov«av Boucc
                                                                                                  OBIM BBIM
                                                                                                    I 1  Prlnclplr  A f r«b umpVr la collect*-*
                                                                                                 In ui rtHiwu^i  fUMk rontMlnlnc •
                                                                                                 •uirurto  meM hrrfracrn iwromhle
                                                                                                 •olulton. and inr nllro«rn omUin. rin-pt ni
                                                                                                 limn  i>» Mr  mtt mruuird rnlorlinclrlrally
                                                                                                 lultil  (hi- ulirnwltfbullnnlr arid illiSi pto
                                                                                                 rrdmr
                                                                                                    I 2  AI>I>I>< jblllly  Tli la  mrlliud  In
                                                                                                 Mr in llir mrunrnnfnl  o| mirugrn
                                                                                                 rriiiltrU irmn !ilailonary Miurivi, Ttlr  fatiir
                                                                                                 «>l III. mriluMt li»-v lH>i-n nj ac
                                           rrplablr •llrrmlivra, >ub)m to appfoval of
                                           Ihr A<1nilnLMi»n uiU rqiilppi^l with  an In Hack of  mil
                                           ituk  Hlli-r In rrmuirr iwrllrulttr mallei i*
                                       708
                                                                                                                                          109
-------
EPA METHOD 7E
-------
                                                   40 CM O. I <7-l-«t l«fhjti)
   Jiiea  eeroMI cnnmMrallon In P|NO,/ml   arquUrd dal* ftound nil Ilium •«l«-i llnal
   > oat tort* the rum Ihraua'i trio Ikfiu •   rak-ulaltan.
     4h curve Iftrawah Ihe point* The tune     a I  fuwml* ««iu_» n. _ —  -  r-m. j .  .
                ^^~   _  u                  • •  •^^"•••i *"•*•••*, mr na*M, ».iwiM_ieo

                U^et^rT^"^!,,?   ^.^-^C—"••— H"" - '" Method

                                            • I  Total M MO.

                	retaining al fmaBT
                 Havre heiond llul of the
                                                                                                                                                    n.«o.
                                         M*l
                                                -HI* 18  Bl
                                                                           IB I
 «TST±±r^ rT-rtTrr^Tu..^' """    ,* ' "—"—*•- n"^» Prepar.,ta. ju,
 ine !•• romponenl rjelni meMiiied           alrari  Cilibrallon  Einv   and
                                          Bratra* Bla* f."nert   Pbllo* Smion,
                                          through • 4 0| Method §T
   aanre M Method *C, aecUam 4 I Irirnnh    * ' MU>  *°  *°

 • dMMmlu o*d •ewml*                  UMliht   HO.  ooarantralloii " ^ms&t

 _jj .^frr^L ?!Mf*  *•'. •*"-"•   ^HteHtrr^rru^r.^^
 OMB*•*•!••• lor HO. that BMMaUM anecUl    i> HO  J.  MrU
                                                                                                                               (iyjC       Brf§Wt€JiOB of 0BaH^^tal ffftMiY U^fl a^fffffffl'
                                                                                            • III
                  it.l.l IfuiiBth •.!.». and

  lit  HO. !• HO Cotreerter Ttmt pottton
 jf UM HBUMI UM« IHBUIJI UM  "
 oiMe IHO.» hi UM BMMPB, tm
                                                                                            MUI4HO)  «D Hpb lo HO Mmtrwt k nol  K»M th»e iiiMtud to
                                                                                            ii ....... «i| H dua on  pi» b ba. UMB t prnrnt of the total HO
                                                             the
                                                       	OBlfl
                                              i  obtained alter  ivtee UM

                                              d. U» dettrMii'M the areraae eMlnent

                                           It Xfta  and  CaUkraUan  Drill  Tot
                                         PtollM aenlon 1 « of Method «C
                                         • tmtuiom CWrBlarioB
                                                                                                                                           « bMtatraphf of Mrlhod «c
                                            IMOB  • - D*TBmMio«iMo:  D*  SinmBic
                                            Ana Mm COB SOLT**  DIOIIBB  lOiia
                                                      fjliiioaiaiv I
                                   •c.   i mi
  Mrthn.il for  Detei
           uumr
  I tVnloiilnei A«*ncr. He
Phrk  HC. Journal of UM
           I Of tBBMdBBB OMCtlBB tl.
  •J raH»,t)uu oa* OarMotraUoa ferHV    II
                     •J  of  MHlMii K.  Me lor the
                                                                  a* Method «C.
                                                 11 I.I I I. andl I I
                                           III  HO.I«MOOon«*ff«*f AdBVfcolhal
                                                                  to I HO.) to UM
tav Method r and ctMfM* an t> cement POT
'"•••»« »ah»«a !• !• peranM lar •• pan.
bM HinHMiii  lahiriilHii  lo The Homed.  Drill, CaMbratian Drill, and I
•TA. March Ml.  I MM  HH, Intnltrrne* tn  Bam I1 a* Method dC, Orrtlon* t.l IhroMh
MethodHCotMITD.                        I*
  • Q*BM|  Amurwwr Handbook lor  Air    II  Interfereno*  ftflBjianec  The  output
Pollution  MeBovremenl  armltmf  Volume  frvponee ol  the •f»*unnu.i»i ivatem to •
              oullw Irlaildt. aad hi UM
        of other  aarUcutaU BMllm and
•wlfar dteiMe eouMoB* Iroai  mtulmmi i
otMrcw. CMlBhonlhw laU how otMvn Uial

method  an •«•  ayitlB¥*MI/cuMr rwter
10 U > !•  ' paurKbj/nttrt looll lor wUiu Irt
  • 1 InUrrnrnR
•fnlnnw g^^^^^
prto. lo H* brMM we In UM IkM Theml
tn. rechor* Ihe oMBMiiBMin nnteai U  oildr and II •*/••<• N H  • •>/«•» lor
rhanfca on  nade hi Ihe tnaUwrnKlion  ulfur dto'lde Ho upprr Itouu hate been m
thai oautd aHei Ihe InUtlrrrm leoponM  laMlahed rtaoril on iheorrUeal  CBtralaUon*
<' I . chamtoi In Ihe aa* drietrlari C otMturl  (or MB mlllrVrra ol } ueioirt hrdio*en per
Ih* BM\«ifutitu ilfvmim  In aorofdaivr  oitldr •olulbm  Ihe  uppei  oonmunitlon
allh Becunt, f « of Method M               limit lot luilui dloilde In a I •  m" 11*1 II •>
                                      730
                                                                                                                                731
-------
EPA METHOD 25A
-------
   . tt, At*. A. M*ffc. 7M
                                                    40 CF« Ck,
 Mtt» t*«*l
                   i •*• al the calibration   cxllbnlkm aa> Thr an-raav (hall I
        	_ __*^. *4|uat Uw analrm output   mined by  (hr Inlranltan of Uw output r»
to Uw appropriate leww. II nrnmmrr. CM   aOrtOni o*»r Ih*  period apeelifed In thr M>
                            lor Uw !»••   ptlcaMe nvutallon
                       i baaed on a Ibmr
         Ifcw eetaarii Uw aero and  hbjh-
                Tnen Mradonr it>* trnl   wbM •^iw.Uon »A I
                                             If raulu we required bi ICVM el PPN» M
                 ror tomtnrl and aild-w»l
                 and determine Uw dMIpr
               Uw awaaurtiBcnl litcai rc-
                                                            rvllon M cvrtion.
                         hMi I pnwnt «f
                                  II «t.
                   to  uw  n*uhw
             etiMt BCttodiol praotM Inter
                  Uw la* anted. |*M*».
            aAcr both Uw aero
              If Uw drill ralun euved Uw   cam. ajrf M analraer aei to I
                        r the  loat raaolu   atwnrpilnrt band I Tnc oanamtraUon hi ••-
                  i and rrpial the taal fol-   prowwl to Una* of propane tor other appro-
                    to  Uw  imjwumiwii*   prtalc organic calRmUon •*•» or hi temw ol
                      reeallbrau Uw tat   cvrtnn.
                    H In Serum • 4 and     | 1  ntnHpw  A «aa wMVlr to
                     I bath atto of «inn»   Iron  Uw  aoaree tnrovali  a htalc
        i U«. data ortcrnMnrd prior to the   line. It im«wj»ii  and «laa> flbR fitter to a
           and data drtormlnrd  folloa'lna   nondwornrn bifrarvd analyan iNDlHt. Re-
lha taat period)                            mHa  are reported • volwiw conettM ration
• orffHf Ctonmlrmtlo* CcLlrUaflou       rqulwawnto of  Uw cajlbrallon  ••• or
  D»iHiw.lm Ihe B*rraie organic concenlra-
             ol Ptvnr a* (kropw or othrr
                                         caibon rqultalrnla.
                                         J
                                       944
 II  PrtorltaJt,  Praanir* and
*Wlwd anc
        vtUiMibv
itet »»r« BK lo mtU-
-------
PI. MlAftoa. A.
                    ISA
                                               40 CM Ch.
                                                                          )
                                                                                                                                     PI. «0.
                                                                                                                                                          ISA
                         *r m*rvmm.*^mm"  »«fn.iiH«  for affected MMJrcv catofloclee lii
                         no* UeiBB •  Ihe applicable pan ol Ihe regulation* Toe
                                      epan value to otaMtohed In In* applicable
                                      reiulailon arid to unialir I & 10 1 & llnvrv it*
                   _                  applteabMmitoalun llmjl  If no loan value to

   -^^^^£irt^  ssrr±r«::s^s£^£
                                      aanTtnimx. Uw apan value  eltoutd cure
                 Ala, .,-.." /-^__,J.  "Bond lo 14* peveenl o| Ihe recorder icale.
            TIM oonoanu^Llr^r^    " C^"""0" °"» * ••">-•» eonewira
           i-"—srjKs..  ;s^^srairrrs
                      •i or B ma 01  aMa*a»aa»*i«l araua*  napmiee  lo a arm
ii  -MA.  A „..».,.,. „,«**  ±^'±^0£^"E^.nfctn:
                                 **•    «.» OUftaraUon Drill. The different* hi
                                                                                      i |  Orcanlc ConottMraUon  Analrecr,  A    • I  Puel  A 4O percent H./M pen*** He
                                                                                                      ran IP1A) eapohto of  or M percent H./M percent N. aaa I
                                                                                                       UM aparlflcaliam In  to reeoatonende* to avoid an oiyavn i _
                                                                                   into eaeUMHl,                            atom effect  thai  leportcoly  ootwre  when
                                                                                     l.t  neamlr Prone  nielnVa*  aucl.  or  omen caneenirailaB vartoi alcnUleanUy

                                                                                   nolee ahaU be t OMB h> ittoaniw of aamiler    4 t  Zero Oa> Hlch puiny air Mlh teae
                                                                                   MM) totalled al HI. H, and U.I pcrnml of  lhan a I part* 9ft teUUan br mlietoie (ppaivl
                                                                                   lh* cejajvajenl ala«-fc daMaeMr, AMcmallvc-  of onianle  natertal  (propane  or
                                                                                                                     ~ an  eoulvalenli or kai lhan • I guinea:!
                                                                                   thai a Caa eaeaate to BoUectoi Iraea Ihe cm-  anao value, •ttlchcvn Ii |r*al«.
                                                                                                                    •LMb    4 J  LAV level Cainbrallon ON- An oraantc
                                                                                                                          caiavratlom aai wlih a ooncvnUaUoo <
                                                                                     I.I  flwepM  UM.   auMeai  eleel  or  lent lo M la IB pcrecnl «f UM
                                                                                   TafleA* tabbaej lo tranaport UM amaolc iae  epan valun
                                                                                   M UM kJaalvaer The aeaapte Une vhowld be    4.4  Mid level Calibration Oa>  An >
                                                                                          U nooeeaary,  lo  puna*  oomawiioB-  caJtbvatfcHi >ai »ilh a i
                                                                                                                          ami lo «• lo AS pertem af UM appHraatr

                                                                                                                            4.1  Hkjh tevei CaHbtaUon OM An organ
                                                                                                                  mccoi-  Ic ckUbraUon  eai  aUn  a ooBoeaUailon
                                                                                                                          •aulvaleM U> •• to M percent of UM appll
                                                                                                                  la UM  cable epan value.
                                                                                                                                      •I Sultm rVi/toiaMaof Sptcl

                                                                                                                            11  Zero Drill. Lam lhan tl ptronu of
                                                                                                                          the epmn ralue.
                                                                                                                            •.I  CaoDnilon Drill. Leva lhan  i) per
                                                                                                                 —tfjf.ifr  cent ol apoj> value.
                                                                                                                 ^,1 ™    t.l  (aaUbralun Error Leva lhan  11 per
                                                                                                                    mmt  cent ol UM cattbrukei fa* value
                                                                                                                     in-  41. fnUtl Pnrparahou
                                                                                                        Hot*. Thto eaeUiod    a |  aetontem of SMBpllaa Slta The taea
                                                                                                           ••jiloitM area*,  tion «f UK •aMptbw atlc to eeaeraft
                                                                                                                      •n  fted by UM -rP"r«%>- rt«ulaUan or |
                                                                                                                          ol Uw lev*. !.«., fihaiMI aucfc. featM Une. vtc
                                                                                                eadOOwrOaK*             The uuopte port ttuiU tee totaled al toa« 11
                                                                                              I far caiavfattaeax fuel  and GO ••  aMfen or 1 couivale.nl
                                                                                           a* ill noniivitl  an eonlaJom In  of ir<« aaa dtochan» ila UM i
                                                                                           •AT ill lewHMii  are dpuaian. m    ^  goo*** at aejaple Probe InaUII UM
                                                                                                                     , >.  aMBBte piiitot ao that UM ptejbe to eeotrmllr
                                                                                                               •  ihacd hi  localM bi the uact, pfev. «  dnrt and to
                                                                                    •afavoeje •!  AdonMeaaMF. UM OMaufiic-  eeaktl UfhUy al the Mack port oonnertkuj.
                                                                                    turn tf UM crllndw ehotild orovtdc a (IK  «"Mc>fttn
                                                                                            I ehell Uf« lor oach OkUbraUan |aa  "*• *•_ «"«
                                                                                                                           k«iwurccncnl  mint fa
                                                                                       	ora^UM^ToBIWBDUrroto^lM  '•««*""• ejmieti mamdlOtia IB i
                                                                                   OBrUJMeTveiuTl'tarcaa^rattaMtw^iiai  "*• •»*"* toHrrfecr ind UM area** analyr
                                                                                   IM*  avanaUy avaUabte tl*. omnfce !•>  •»i*****'"V"'**"lloef**le  „»„._,  .„
                                                                                   la*n> I and If oenM b, MfeuMl aUma     "* •«*-«'»  f TL^'.^S^.J!'
                                                                                   Uv«  OMtbotto tor pvaparlM eaUbrmUor. lee  •*1^*"PiJ'•«* ^ J^J^S?!6!/'^!!"
                                                                                   —1,1,..-- OM* aa flkiUon enlaaat. B«r lav  tr»Uor»  Pot huh cnmotojimioaa of onjan-
                                                                                   ^^^^^^^^* ^^^™ ^* ^BilW^^Bl *P^^^^^^ ^^*r ^*  ^^       at mu^ ,M. kk.i BMlBi^^B ^M fWMB]A2M|
                                                                                   UM>| ortUi Mh» •iM^nvai of the AdBaa^aUa-  Ha  1 > I a perecm ov VORIOIB ^ m»*^nei
                                                                                   ——  -«« •"•"• «ew»w»«- •••«         •   ModMleaWon* u> OMBII iiMiainnlr avalteblr'
                                                                                     Calibrmuon MOB> ueua(>» oanatM ol pto   analnere  are  neraawy  One  erraalert
                                                                                   I^MTaU^^SSTand ,*?Z*~£«  —•»•* •« «.«*««* —-*<•««"» «• f «»
                                                                                   to leroM ol the apan value. Orcanlc caa-
                                                                                   PoiuMto other lhan nropane can be uaed t<*
                                                                                   lo*tn« UM above euldcllnea and Matin* U«
                                                                                   •PproprtaM eorrotUone lor uaiiiiiMl facbr.
                                                                                                                                                 U UM analran
                                                                                                                         ereaw the OBK u( Ihe
                                                                                                                         lrtrou«h the uat ol a
                                                                                                                         aunptc capuiarr  Direct
                                                                                                                         Bwauirencni ol oreuitc oBe»enl»mUnti to
                                                                                                                         nertMrr muldrraitan a>heo
                                                                                                                         anr momricallon tiatvn
                                                                                                                           • •  Callbralton biw T«M.
                                                                                     • Mention of Hade namri or *p*cl(tr pro!     _    	         	
                                                                                    m;U doea not oomlNuU cndonenitnl br ll«  pilor to ihr l«l eerUa. ivHhln J noure or
                                                                                               I Protection Aaciic*.           tlx mi+i\ of HM- l«i r Inlraduee *f» cat Uid


                                                                                                                       043
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