DEECO Inc.

3404 Lake Woodard Road

Raleigh, NC 27604

(919) 250-0285 (ph); (919) 250-1835 (Fax) www.deeco.com

REPORT NO: 042110-2526

PROJECT: 10-2526

DATE: May 7, 2010

TYPE: Emission Test Report

U.S. EPA Information Collection Request

for

Hydrogen Chloride Emissions

from

Portland Cement Manufacturing Facilities

Holcim (Texas) LP

Midlothian, Texas

AUTHOR: Scott Steinsberger, Ph.D.

TEST DATE: April 30, 2010

FIELD TEAM: Josh Fox, John Martin, and Scott Steinsberger

PREPARED FOR: Holcim (US), Inc.

201 Jones Road

Waltham, Massachusetts 02451
i

TABLE OF CONTENTS

Section Page

1. INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

2. SUMMARY OF RESULTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

3. SAMPLING AND ANALYTICAL PROCEDURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

3.1 EPA Method 1 and 2 - Stack Gas Volumetric Flow Rate Determination . . . . . . . 7

3.2 EPA Method 4 - Stack Gas Moisture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

3.3 EPA Method 3A - Stack Gas Oxygen and Carbon Dioxide . . . . . . . . . . . . . . . . . 9

3.3.1 Gas Sampling System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

3.3.2 Oxygen and Carbon Dioxide Monitor . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

3.3.3 Data Acquisition System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

3.3.4 Calibration Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

3.4 EPA Method 321 - Stack Gas Hydrogen Chloride . . . . . . . . . . . . . . . . . . . . . . . 11

4. QA/QC PROCEDURES AND RESULTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

4.1 Sampling Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

4.1.1 Manual Sampling Equipment Calibrations . . . . . . . . . . . . . . . . . . . . . . . 14

4.2 Analytical QA/QC Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

Appendix A - Emission Summary Sheets 

Appendix B - Field Sampling Data Sheets

Appendix C - Continuous Emission Monitoring Results

Appendix D - FTIR Data

Appendix E - Equipment Calibration Data Sheets and Calibration Gas Certificates of

Analysis

Appendix F - Test Participants
ii

LIST OF TABLES

Table No. Page

TABLE 1.1 SUMMARY OF HYDROGEN CHLORIDE EMISSIONS; HOLCIM (TEXAS)

LP MIDLOTHIAN, TEXAS FACILITY; APRIL 30, 2010 . . . . . . . . . . . . . . . . . 3

TABLE 1.2 SUMMARY OF SAMPLING AND ANALYTICAL PROTOCOLS FOR 

HOLCIM (TEXAS) LP MIDLOTHIAN, TEXAS FACILITY . . . . . . . . . . . . . . . 4

TABLE 2.1 HYDROGEN CHLORIDE EMISSION TEST RESULTS, HOLCIM (TEXAS)

LP MIDLOTHIAN, TEXAS FACILITY; RAW MILL ON CONDITION; APRIL

30, 2010 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

TABLE 2.2 HYDROGEN CHLORIDE EMISSION TEST RESULTS, HOLCIM (TEXAS) LP

MIDLOTHIAN, TEXAS FACILITY; RAW MILL OFF CONDITION; APRIL 30,

2010 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

TABLE 3.1 HYDROGEN CHLORIDE ANALYTE SPIKING TEST RESULTS, HOLCIM

(TEXAS) LP MIDLOTHIAN, TEXAS FACILITY; RAW MILL ON

CONDITION; APRIL 30, 2010 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

TABLE 3.2 HYDROGEN CHLORIDE ANALYTE SPIKING TEST RESULTS, HOLCIM

(TEXAS) LP MIDLOTHIAN, TEXAS FACILITY; RAW MILL OFF

CONDITION; APRIL 30, 2010 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

LIST OF FIGURE

Figure No. Page

Figure 3.1 Schematic of the Main Kiln stack. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
1

1. INTRODUCTION

The U.S. Environmental Protection Agency (EPA), Office of Air Quality Planning and

Standards (OAQPS) issued an Information Collection Request (ICR) to Holcim (US), Inc (Holcim).

Under the authority of Section 114 of the Clean Air Act (CAA), the EPA requested information on

hydrogen chloride (HCl) emissions from nonhazardous waste-burning kilns at Portland cement

manufacturing facilities. The request was in response to comments from Portland cement industry

members and its trade association to EPA’s proposal to amend the national emission standards for

hazardous air pollutants for Portland cement manufacturing (74 FR 21136 (May 6, 2009)).

Holcim retained DEECO Inc. (DEECO) to conduct the required emissions testing. Testing

for HCl was conducted in accordance with EPA Method 321 - Measurement of Gaseous Hydrogen

Chloride Emissions At Portland Cement Kilns by Fourier Transform Infrared (FTIR) Spectroscopy.

The Holcim facility in Midlothian, TX (1800 Dove Lane, Midlothian, TX 76065) has been

one of the Portland cement manufacturing facilities selected as part of the ICR. Holcim operates a

dry process kiln system at this facility. 

The Midlothian Plant's Portland cement manufacturing process involves raw materials

acquisition and handling, kiln feed preparation, pyro-processing, and finished cement grinding and

loading. Each of the Midlothian Plant's Line 1 and Line 2 pyro-processing systems consist of a fourstage preheated precalciner system (Emission Point Numbers [EPNs] 7 and 65). Both lines have a

bypass system to control the quantity of alkali and sulfur since the nature of the raw materials

requires that alkali and sulfur be removed to control the quality of the clinker. Water spray

conditioning towers designed to cool gases are located in the ducting between the preheaters and the

raw mills. When the mill systems are not operational, the spray towers protect the main baghouses

from high temperatures. The spray towers are not used when the mill systems are operational. 

Testing was performed at the stack under two conditions, Raw Mill On and Raw Mill Off,

on April 30th, 2010

Sampling was conducted by personnel from DEECO, Inc. of Raleigh, North Carolina.

Emission measurements were conducted simultaneously at the Main Kiln Stack for temperature,

volumetric flow rate, dry gas molecular weight, moisture, and hydrogen chloride. A summary of the

sampling and analytical methods are presented in Table 1.2.

All questions regarding sampling and analytical data should be directed to Dr. Scott

Steinsberger of DEECO at (800) 733-3261. The field sampling was completed by Josh Fox, John

Martin, and Scott Steinsberger of DEECO. 

The remainder of this document summarizes the results, procedures and quality control

measures followed for this program. Section 2 contains tabulated air emission results for each

parameter of interest. Section 3 summarizes the air emission sampling and analytical procedures

performed by DEECO, with a brief description and/or reference to the applicable methodologies.

Section 4 discusses the basic quality control elements in place for this program to assure the

collection of representative, accurate air emission data.
2

The appendices provided in this document contain all of the necessary information to verify

the reported results. Included as Appendices are: A - Emission Summary Sheets; B - Field Sampling

Data Sheets; C - Continuous Emission Monitoring Results; D - FTIR Data; E - Equipment

Calibration Data Sheets and Calibration Gas Certificates of Analysis; F - Test Participants.
3

TABLE 1.1 SUMMARY OF HYDROGEN CHLORIDE EMISSIONS; HOLCIM (TEXAS)

LP MIDLOTHIAN, TEXAS FACILITY; APRIL 30, 2010

Test Parameter Raw Mill On Raw Mill Off

Hydrogen Chloride Emissions (ppm at 7% oxygen) <0.42 <0.45
4

TABLE 1.2 SUMMARY OF SAMPLING AND ANALYTICAL PROTOCOLS FOR HOLCIM (TEXAS) 

TEXAS FACILITY

Location and Frequency Test Parameter Sampling Method Sampling Procedure Analysis Method 

Kiln Main Stack Volumetric Flow Rate EPA Method 1 and 2

with s-type pitot 

Velocity traverse with

pitot for delta p

EPA Method 2 

Oxygen and Carbon Dioxide

EPA Method 3A Continuous;

extractive sample

EPA Method 3A 

Stack Gas Moisture EPA Method 4 Integrated sampling with

condensation

EPA Method 4 

Hydrogen Chloride EPA Method 321 Continuous;

extractive sample

EPA Method 321 
5

2. SUMMARY OF RESULTS

Emissions sampling was conducted at the Holcim (Texas) LP facility located in Midlothian,

Texas. Sampling was conducted for stack gas HCl according to EPA Method 321. Concurrently,

sampling was conducted for stack gas volumetric flow (EPA Method 1 and 2), stack gas oxygen and

carbon dioxide (EPA Method 3A) and stack gas moisture (EPA Method 4). Testing was conducted

under two conditions; Raw Mill On and Raw Mill Off.

The emissions results are summarized in Tables 3.1 and 3.2, respectively for the Raw Mill

On and Raw Mill Off conditions.
6

TABLE 2.1 HYDROGEN CHLORIDE EMISSION TEST RESULTS, HOLCIM (TEXAS)

LP MIDLOTHIAN, TEXAS FACILITY; RAW MILL ON CONDITION;

APRIL 30, 2010

Test Parameter Run 1 Run 2 Run 3 Average

Time 08:35-09:35 10:05-11:05 11:32-12:32 ----

Stack Gas Temperature (EF) 138 137 137 137

Stack Gas Moisture 18.3% 17.9% 17.9% 18.0%

Volumetric Flowrate

 actual cfm

 dry standard cfm

467,100

332,800

464,400

333,100

460,600

330,300

464,100

332,100

Oxygen Content 12.7% 12.8% 13.1% 12.9%

Hydrogen Chloride Emissions

 Concentration, ppmby volume, wet basis

 Concentration, ppmby volume, dry basis

 Concentration, ppm at 7% oxygen

<0.20

<0.24

<0.42

<0.20

<0.24

<0.42

<0.20

<0.24

<0.43

<0.20

<0.24

<0.42

TABLE 2.2 HYDROGEN CHLORIDE EMISSION TEST RESULTS, HOLCIM (TEXAS)

LP MIDLOTHIAN, TEXAS FACILITY; RAW MILL OFF CONDITION;

APRIL 30, 2010

Test Parameter Run 4 Run 5 Run 6 Average

Time 15:02-16:02 16:30-17:30 17:58-18:58 ----

Stack Gas Temperature (EF) 137 134 137 136

Stack Gas Moisture 17.2% 17.0% 17.9% 17.4%

Volumetric Flowrate

 actual cfm

 dry standard cfm

450,200

325,500

449,600

327.600

424,000

304,100

441,300

319,100

Oxygen Content 13.6% 13.7% 12.6% 13.3%

Hydrogen Chloride Emissions

 Concentration, ppmby volume, wet basis

 Concentration, ppmby volume, dry basis

 Concentration, ppm at 7% oxygen

<0.20

<0.24

<0.46

<0.20

<0.24

<0.47

<0.20

<0.24

<0.41

<0.20

<0.24

<0.45
7

3. SAMPLING AND ANALYTICAL PROCEDURES

Table 1.2 presents a summary of the overall sampling and analytical protocols used for the

Information Collection Request (ICR) test program for the Line 2 Main Kiln stack at Holcim (Texas)

LP Midlothian, TX facility. All sampling and analytical methods employed for this test program

were performed in accordance with the procedures outlined in the Reference Test Methods contained

in the Code of Federal Regulations, Title 40, Part 60, Appendix A (40 CFR 60, Appendix A) and

40 CFR 63, Appendix A.

3.1 EPA Method 1 and 2 - Stack Gas Volumetric Flow Rate Determination

The Main Kiln stack was a round vertical duct with an inside diameter of 164.063 inches.

The sampling ports were located on the Kiln stack over 7.5 duct diameters above the nearest

disturbance, and more than two duct diameters below the stack discharge. This location meets the

minimum specifications for selection of a measurement site as outlined in EPA Method 1 (see

Appendix B). A schematic of the Main Kiln stack is shown in Figure 3.1.

An 6-point velocity traverse in each of two perpendicular directions was made at each

sampling location using a type-S pitot tube in accordance with EPA Method 2. Gas temperatures

were measured using calibrated Type K thermocouples and digital readout devices.

Dry gas molecular weight was determined using the oxygen and carbon dioxide

measurements following EPA Method 3A employing oxygen and carbon dioxide monitors. Stack

gas moisture was measured in accordance with EPA Method 4 procedures.

3.2 EPA Method 4 - Stack Gas Moisture

The moisture content of the flue gas was determined using the methodology described in

EPA Method 4. Based on this method, a known volume of particulate-free gas was pulled through

a chilled impinger train. The weight of each impinger was determined gravimetrically before and

after sampling. The weight increase in each impinger was then related to the volume of gas sampled

to calculate the moisture content.

During this test, the moisture content of the flue gas was determined simultaneously with the

Methods 3A and 321 sampling.

9

3.3 EPA Method 3A - Stack Gas Oxygen and Carbon Dioxide

A CEM system was used for determining the flue gas molecular weight and stack gas oxygen

content on the Main Kiln stack. 

The extractive monitors require that the effluent gas sample be filtered and maintained above

condensation temperature, or conditioned to eliminate any possible interference (i.e., water vapor

and particulate matter), before being transported and delivered to each analyzer. All components of

the sampling system which contact the sample are either of glass, stainless steel, or Teflon. A heated

sampling probe with heated out-of-stack particulate filter, heated sample lines, an ice water-cooled

condenser, a sample pump, and a gas distribution manifold are used to deliver a representative

sample of flue gas to each of the analyzers. Details of the major components of the measurement

system are presented below.

3.3.1 Gas Sampling System

The gas sample was extracted from the stack through a glass lined probe and filter heated to

at least 356E F in an enclosure custom built for these test procedures. This heated enclosure was

equipped with heated glass-lined probe that allowed three traverse points on the line at 0.4, 1.2, and

2.0 meters from the stack wall be sampled equally during each test. The glass filter holder had a

teflon frit supporting a quartz fiber filter. Outflow of gas from the heated filter enclosure was

conveyed using a heat-traced Teflon sample line also maintained at least at 356EF. The heated line

was connected directly to the FTIR sample cell. A sample pump in a DEECO proprietary chillertype gas conditioner system was used to pull the gas sample through the system. The gas conditioner

system was also used to remove moisture from the gas sample prior to introduction to the

oxygen/carbon dioxide analyzer.

3.3.2 Oxygen and Carbon Dioxide Monitor

A CAI Model 200 O2/CO2 analyzer was used to measure the oxygen and carbon dioxide

concentrations. The oxygen concentrations are were measured using the paramagnetic technique.

Because of its sp3 electron orbital distribution, an oxygen molecule has an unpaired electron and

hence displays a magnetic orientation. Since other elements that display this magnetic phenomenon

are not common gasses at normal temperatures, the paramagnetic measurement technique is virtually

specific for oxygen. The sample gas flows through a detection cell located in a very strong magnetic

field. The magnetic nature of the oxygen causes the oxygen to move to one side of the detection cell,

inducing a pressure differential proportional to the oxygen concentration in the detector cell. The

analyzer measures this pressure differential, converts the pressure differential to an electrical signal,

and sends the results as output.

The carbon dioxide concentrations were measured using a single-beam photometric system

with a micro flow sensor detector. The micro flow detector is a sealed unit filled with carbon dioxide.

The instrument consists of an infrared light source, a chopper, a measuring cell and a micro flow
10

detector filled with carbon dioxide. The infrared light emitted backward is reflected by a reflecting

surface and is added to the infrared light emitted forward. Arranged between the infrared light source

and the measuring cell is a chopper blade which rotates to modulate the infrared light beam at regular

frequency. The modulated infrared light beam thus formed passes through the measuring cell filled

with a sample gas where the light energy is partially absorbed or attenuated before it reaches the front

chamber of the detector. Both the front and rear chambers of the detector are filled with the gas

component to be measured. The infrared light energy is partially absorbed in the front chamber and

residual light is absorbed in the rear chamber, thereby increasing the pressure in both chambers.

Since the detector is designed to produce a pressure difference between the front and rear chambers,

a slight gas flow is produced through a path connecting these chambers with each other. This slight

flow is converted into an AC electrical signal by a micro flow sensor.

3.3.3 Data Acquisition System

Data were recorded on two separate devices. A hard copy was obtained using a Molytek 2702

strip chart recorder. Data was also recorded to the hard disk of an IBM compatible computer utilizing

the serial output of the Molytek recorder in conjunction with custom software developed by DEECO

Engineers. Data for each of the analyzers was sampled each two seconds with a one minute average

being written to disk. Data was further averaged over the test period and corrected for calibration

error and drift using a spreadsheet program.

3.3.4 Calibration Procedures

Calibration procedures were performed in accordance with EPA methodology. Analyzers

were calibrated before and after each test and a calibration check was done between each test run.

The pretest calibrations consisted of the following steps:

C Internal (direct) calibration of each analyzer to adjust calibration and

check linearity.

C External (through the entire sampling system) calibration to check the

system bias on zero and span gases.

The post test calibration consisted of an external system bias calibration check

Each analyzer was calibrated using a certified zero and span (mid or high range) gas. Zero

and span gases were directed to each analyzer through the appropriate plumbing, the calibration gas

flow rates were adjusted to the correct flow rate and the analyzer was adjusted with the appropriate

span pot.

After the analyzer was properly adjusted the linearity was checked using a low and high range

calibration gas. The maximum allowable limit for linearity is 2% of the analyzer range. All analyzers
11

were shown to be linear within these limits.

The external calibration bias check was performed by placing the CEM system in sampling

mode and injecting a zero and span gas into the sample line at the probe exit. This check shows if

there is any sampling system related bias, and also serves as a check of the integrity of the sample

line. 

DEECO used EPA Protocol and/or ±2% NIST Traceable gases for calibration as required by the

various reference methods employed in this test program. Calibration gases were selected from

previous experience with similar sources and/or from information obtained from the facility engineer

prior to sampling. In some cases if the gases that were selected were out of the optimum range of

operation then no significant impact of data quality is expected due to the linear nature of the

analyzers that were used.

No audit gases were available from federal or state agency.

At the completion of the pretest calibration routine, the CEM system was ready for operation.

No further adjustments of sample flow rates, analyzer zero or span adjustments, or other critical CEM

operating parameters were made until testing and post test calibration were complete.

At the completion for each test run, calibration gases were used to check between test runs.

A zero and the upscale calibration gas closest to the actual emission concentrations were used for the

pretest and post test calibrations.

3.4 EPA Method 321 - Stack Gas Hydrogen Chloride

The sampling system described above was used to convey the gas sample to the FTIR sample

cells. The FTIR sample cell was maintained at 356EF. The sample cell was connected to a MIDAC

Corporation I-series Fourier Transform Infrared Spectrometer and Detector.

The FTIR spectrometer measures vapor phase organic or inorganic compounds which absorb

energy in the mid-infrared spectral region, about 400 to 4000 cm-1 (25 to 2.5 μm). Continuous

measurement is made by matching sample absorbance bands with bands in reference spectra, and

comparing sample band intensities with reference band intensities.

The principle limitation to FTIR spectroscopy are the presence of interfering compounds that

also absorb energy in the mid-infrared spectral region. In a cement kiln stack gas matrix, water vapor

(H2O) and carbon dioxide (CO2) are the primary interferents that must be incorporated into the

identification and quantitation method.

The FTIR software performs the computation for a single compound by subtracting all the

other compounds (interferants and target) from the absorbance spectra and quantifies the single

compound based on the remain absorbance. The FTIR software provides a Standard Error
12

Calculation (SEC) value that is an indication of how well the identification and quantitation has been

performed. A high SEC indicates that other interferants have not been accounted for in the analysis

method, and a low SEC is indicative of greater confidence measurement. 

The instrument was operated with a resolution of 0.5 cm-1 with 4x zero filling. Beer-Norton

Medium apodization was used with amplitude phase correction. Five analytical regions were used for

HCl; 2748.85 - 2754.20 cm-1, 2772.80 - 2776.80 cm-1, 2795.80 - 2800.20 cm-1, 2818.80 - 2822.7 cm-1,

2840.8 - 2845.7 cm-1, 2962.50 - 2964.0 cm-1, and 2997.0 - 2998.60 cm-1. These regions were found

to provide the lowest SEC values for this stack gas matrix. 

With this system at the 0.2 ppm detection limit required in the ICR, a Maximum Analytical

Uncertainty (MAU) of 0.15 ppm at cell conditions was calculated. The ICR request that the detection

limit be calculated according to Method 321. However, Method 321 does not have provisions for

calculating a detection limit. The method has the analyst specify the detection limit and then

determine if the data quality of the analytical system meets calculated criteria based on the desired

detection limit. The MAU of 0.15 ppm is less than the 0.2 ppm required detection limit, indicating

that the FTIR system is suitable for measurement at this level.

Analyte spiking was conducted before and after each sampling run according to Method 321.

The results are summarized in Tables 3.1 and 3.2. All analyte spike recoveries were within the

required 70-130% and the pre and post test CTS calibration checks were within the 5% required .

It was apparent that higher spike recoveries were obtained with higher levels of native HCl.

 
13

TABLE 3.1 HYDROGEN CHLORIDE ANALYTE SPIKING TEST RESULTS, HOLCIM

(TEXAS) LP MIDLOTHIAN, TEXAS FACILITY; RAW MILL ON

CONDITION; APRIL 30, 2010

Test Parameter Pre Run 1 Post Run 1 Post Run 2 Post Run 3

Time 08:03-08:27 09:36-10:01 11:06-11:28 13:34-13:58

HCl Spike Direct (ppm) 20.47

SF6 Tracer Direct (ppm) 10.90

Total HCl (spike plus native ppm) 2.250 1.862 1.736 1.674

Average Native HCl (ppm) 0.526 0.001 0.031 0.000

SF6 Tracer Diluted (ppm) 1.084 1.009 0.999 0.964

HCl Analyte Spike Recovery 87.4% 98.3% 91.1% 92.6%

Ethylene CTS Error 0.45% -0.07% -0.37% -0.65%

TABLE 3.2 HYDROGEN CHLORIDE ANALYTE SPIKING TEST RESULTS, HOLCIM

(TEXAS) LP MIDLOTHIAN, TEXAS FACILITY; RAW MILL OFF

CONDITION; APRIL 30, 2010

Test Parameter Pre Run 4 Post Run 4 Post Run 5 Post Run 6

Time 14:33-14:54 16:04-16:26 17:31-17:54 18:56-19:15

HCl Spike Direct (ppm) 20.47

SF6 Tracer Direct (ppm) 10.90

Total HCl (spike plus native ppm) 1.587 1.578 1.437 1.432

Average Native HCl (ppm) 0.000 0.000 0.000 0.000

SF6 Tracer Diluted (ppm) 0.988 0.983 0.976 0.985

HCl Analyte Spike Recovery 85.6% 85.6% 78.5% 77.5%

Ethylene CTS Error 0.33% -0.07% -0.08% 0.15%
14

4. QA/QC PROCEDURES AND RESULTS

The objective of a quality assurance/quality control (QA/QC) program is to assure that the

precision and accuracy of all environmental data generated by DEECO for clients are commensurate

with data quality objectives (DQO's). DQO's are based on a common understanding of the intended

end use(s) of the data, the measurement process, and the availability of resources. Once DQO's are

established, formally or informally, QC protocol can be defined for the measurements.

In this project, the final data user will be Holcim. The data quality objectives in this project

are to generate scientifically sound data to be used for compliance purposes.

4.1 Sampling Equipment

All of the sampling equipment used was calibrated according to the procedures outlined in the

Quality Assurance Handbook for Air Pollution Measurement Systems, Volume III, EPA-600/4-77-

027b.

4.1.1 Manual Sampling Equipment Calibrations

For sampling Methods 1, 2, and 4 the procedures and equipment used to measure stack gas

velocity and temperature measurements and the metering system used to maintain constant rate

sampling conditions and to determine the sample gas volume were subjected to pretest and posttest

calibrations and/or inspections as required by the appropriate EPA methods. 

Barometer - Barometric pressure values were obtained from a calibrated barometer, verified by

phone call to a local airport, and corrected for elevation to sample port level (0.01 inches Hg per 10

ft. elevation).

Pitot Tubes - Each pitot tube used in sampling meets the design specifications for type-S pitot tubes

in EPA Method 2. Therefore, a maximum value baseline coefficient (Cp) of 0.84 is assigned to each

pitot tube. Calibration by the manufacturer for pitot face-opening alignment included measuring the

external tubing diameter (dimension Dt), the base-to-opening plane distance (dimensions Pa and Pb),

and the face opening misalignment angles, with all terms as described in EPA Method 2. Pitot tubes

were visually inspected for structural integrity at the completion of each test. Inspection sheets for

pitot tubes are included in Appendix E.

Calibration Meter and Metering System - The secondary reference meter equipment arrangement

for calibration is shown in Figure 5.7 of EPA Method 5. The prescribed procedures were followed.

A wet test meter with a 1 ft3

/rev capacity and + 1 percent accuracy is used as the primary calibrant.

The dry gas meter's pump is run for a minimum of 5 minutes at a flow rate of 0.35 cfm to condition

the interior surface of the wet test meter. Leak checks are performed and if satisfactory, triplicate runs

at each of no less than five different flow rates are done. A calibration curve is prepared and the

meter is recalibrated after 200 hours of operation or annually, whichever comes first.
15

The calibration set-up for the dry gas metering system using the secondary reference meter

in lieu of the wet test meter is given in Figure 5.5 of EPA Method 5. A leak check of the metering

system before calibration was performed as shown in Figure 5.4 of EPA Method 5. The metering

systems's pump is operated for 5 minutes at an orifice manometer setting of 0.5 inches H20 to heat

up the pump and system to stabilize the meter inlet and outlet temperatures. Values for the orifice

setting (delta H), wet test meter volume (Vw

), corresponding dry test meter volume (Vd), dry test

meter inlet and outlet gas temperatures (tdi and tdn), and time are recorded for the initial calibration.

Then the ratio of the wet test meter to the dry test meter (gamma) and the orifice pressure differential

that equates to 0.75 cfm at standard conditions (delta H@) are calculated. 

A post-test meter calibration was made on the dry gas meter used during the test to check its

accuracy against the pre-test calibration. This post-test calibration check was made using the average

orifice setting obtained during each test run and setting the vacuum at the maximum value obtained

during each test run. These test runs were made against DEECO's secondary reference dry gas meter

which was calibrated against a wet test meter. The calibration data sheets for the dry gas meters are

included in Appendix E.

Thermocouples and Digital Indicators - Thermocouples were calibrated by comparing them against

an ASTM-3F mercury-in-glass thermometer at approximately 32EF (ice water), ambient temperature,

and at approximately 220EF. Each thermocouple was calibrated against temperature ranges to which

it is typically exposed during test conditions, and they agreed within 1.5 percent (expressed in ER)

of the reference thermometer throughout the entire calibration range. Also, thermocouples were

checked at ambient temperature at the test site to verify calibration. The calibration data sheets for

the thermocouples are included in Appendix E.

Pretest and Posttest Leak Checks of Sampling Trains - Each Method 4 sampling train was

subjected to pretest leak checks and posttest leak checks. For all sampling runs the posttest leak

checks were acceptable (less than 4% of the sampling rate at the highest vacuum recorded during the

test run).

4.2 Analytical QA/QC Results

Analytical measurements of precision and accuracy were made on stack gas samples, and are

summarized in a separate report.