Mr. Shawn Jennings July 23, 2010 

E. H. & S. Specialist 

P.O. Box 159 

Grant Town, WV 26574 

Subject: Utility MACT ICR Testing Quality Assurance Project Plan; 

American Bituminous Power Partners; Grant Town Station; 

Grant Town, West Virginia; 

 Avogadro Environmental Corporation Project No. 10-7091

Dear Mr. Jennings: 

Attached please find the Utility MACT ICR Testing Quality Assurance Project Plan for the proposed 

testing at the above referenced facility and source. 

Avogadro looks forward to working with you during this project. Please feel free to contact me or 

Tom Mattei if there are any questions or comments. 

Sincerely, 

Janeen D. Maruskanic 

Air Quality Scientist

F:\2010 Projects\2010 projects\American Bituminous ICR MACT 10-7091\QAPP\final American Bituminous QAPP.doc 
 

 

QUALITY ASSURANCE PROJECT PLAN 

FOR 

UTILITY MACT ICR TESTING OF THE AMERICAN BITUMINOUS POWER PARTNERS 

GRANT TOWN STATION COAL FIRED BOILERS 

AMERICAN BITUMINOUS POWER PARTNERS 

GRANT TOWN STATION 

GRANT TOWN, WEST VIRGINIA 

Prepared for:

AMERICAN BITUMINOUS POWER PARTNERS 

P.O. Box 159 

Grant Town, WV 26574 

Attn: Mr. Shawn Jennings 

Prepared by:

AVOGADRO ENVIRONMENTAL CORPORATION 

1350 Sullivan Trail, Suite A 

Easton, PA 18040 

Attn: Mr. Thomas Mattei 

Avogadro Environmental Corporation Project No. 10-7091

July 23, 2010 
 

TABLE OF CONTENTS Page No.

1.0 PROJECT OVERVIEW / BACKGROUND INFORMATION 1 

 1.1 INTRODUCTION 1 

 1.2 PROGRAM RESPONSIBLE PARTIES 1 

 1.3 TENTATIVE TEST SCHEDULE 2 

 1.4 KEY PERSONNEL 3 

2.0 SOURCE INFORMATION 4 

 2.1 FACILITY AND PROCESS DESCRIPTION 4 

 2.2 PROCESS DATA 4 

3.0 SAMPLING LOCATIONS 5 

4.0 TEST PROGRAM AND METHODS 6 

 4.1 TECHNICAL APPROACH 6 

 4.2 SUMMARY 6 

 4.3 VELOCITY AND VOLUMETRIC FLOW RATE MEASUREMENT 7 

 4.4 SULFUR DIOXIDE, CARBON DIOXIDE, CARBON MONOXIDE, OXYGEN, 

NITROGEN OXIDES, TOTAL HYDROCARBONS AND METHANE 

MEASUREMENT 8 

 4.5 HYDROGEN CHLORIDE, HYDROGEN FLUORIDE, HYDROGEN CYANIDE 

AND MOISTURE MEASUREMENT 11 

 4.6 PARTICULATE MATTER, MULTI-METALS AND MOISTURE 

MEASUREMENT 14 

 4.7 MERCURY MEASUREMENT 17 

 4.8 PARTICULATE MATTER LESS THAN 2.5 MICRONS AND MOISTURE 

MEASUREMENT 19 

 4.9 FORMALDEHYDE MEASUREMENT 22 

5.0 QUALITY ASSURANCE / QUALITY CONTROL INFORMATION 25 

5.1 TEST EQUIPMENT AND INSTRUMENTATION 25 

 5.2 CALIBRATION AND HANDLING OF TEST EQUIPMENT AND 

INSTRUMENTATION 26 

 5.3 DATA COLLECTION AND MANAGEMENT 28 

6.0 EMISSIONS TEST REPORT 33 

 
 

TABLES

TABLE 1: TENTATIVE SCHEDULE 2 

TABLE 2: SAMPLING LOCATIONS SUMMARY 5 

TABLE 3: TEST PARAMETERS AND METHODS 6 

TABLE 4: REAL-TIME INSTRUMENTATION SUMMARY 9 

TABLE 5: REFERENCE METHOD TRAVERSE POINT DETERMINATION CRITERIA 10 

TABLE 6: REAL-TIME INSTRUMENTATION FIELD QA PROCEDURES SUMMARY 11 

TABLE 7: SUMMARY OF MULTI-METALS DETECTION LIMITS 15 

ATTACHMENTS

1 EXAMPLE CALCULATIONS 

2 FIELD DATA SHEETS AND CHAIN OF CUSTODY FORM 
 1

1.0 PROJECT OVERVIEW / BACKGROUND INFORMATION 

 1.1 INTRODUCTION

An emissions test program will be performed at the common outlet of the two coal fired 

boilers at the AMERICAN BITUMINOUS POWER PARTNERS, GRANT TOWN 

STATION (American Bituminous) facility in Grant Town, West Virginia. The purpose 

of this test program is to comply with the USEPA’s Electrical Utilities Maximum 

Achievable Control Technology (MACT) Information Collection Request (ICR). 

 

AVOGADRO ENVIRONMENTAL CORPORATION (Avogadro) has been retained 

by American Bituminous to perform the emission testing for the boilers. Avogadro has 

prepared this Quality Assurance Project Plan and will perform the emissions testing 

program in accordance with this document. This plan describes the source, the sampling 

locations, the technical approach, test methods, quality assurance items and all other 

details pertaining to the evaluation. 

 1.2 PROGRAM RESPONSIBLE PARTIES 

 

 Site Address: Contact: 

American Bituminous Power Partners Mr. Shawn Jennings 

Grant Town Station Telephone: 304-278-6103 

Grant Town, WV 26574 

 

 Corporate Address: Contact:

American Bituminous Power Partners Mr. Shawn Jennings 

P.O. Box 159 Telephone: 304-278-6103 

Grant Town, WV 26574 

 

 Test Firm: Contact:

Avogadro Environmental Corporation Mr. Thomas Mattei 

 1350 Sullivan Trail, Suite A Telephone: 610-559-8776 x 103 

 Easton, PA 18040 Fax: 610-559-8913 
 2

1.3 TENTATIVE TEST SCHEDULE 

TABLE 1: TENTATIVE SCHEDULE 

Day Weekday parameter Runs 

0 Monday Set-up 

1 Tuesday Particulate matter, metals and Hg 1&2 

Particulate matter, metals and Hg 3 2 Wednesday SO2, NOX, and HCl/HF/HCN 1 

3 Thursday SO2, NOX, and HCl/HF/HCN 2&3 

4 Friday Demobilize 
1.4 KEY PERSONNEL 
 4

2.0 SOURCE INFORMATION 

2.1 FACILITY AND PROCESS DESCRIPTION 

American Bituminous operates a coal refuse fired power plant in Grant Town, West 

Virginia referred to as the Grant Town Station. 

The Grant Town Station generates electricity with the steam supplied from two 

circulating fluidized bed combustion (CFB) boilers with a maximum rating of 551.9 

MMBtu/hr each. The primary fuel is coal refuse supplemented with pond fines. Natural 

gas is used as a startup fuel. 

Limestone is injected directly into the furnace combustor for control of sulfur dioxide 

emissions. High fluidization velocities promote circulation of solids which provides more 

efficient combustion, emissions control, and heat transfer. Employing limestone as the 

sorbent material in the fluidized bed removes sulfur dioxide (SO2) at an efficiency of 90 

to 94.8%. The addition of limestone to the coal refuse at the combustion chamber is 

integral to the design and operation of the CFB boilers. Once the sulfurization process 

has occurred, the remaining calcium sulfate is removed from the boiler in the bottom ash 

and fly ash streams. 

Gases and particulate matter (PM) produced from combustion then move through a hot 

cyclone where heavy particles and ash are separated from the fine particulate hot exhaust 

gas. The hot exhaust gases then pass through a baghouse for capture of fine particulates. 

Both boiler units discharge through a common stack. 

The CFB boiler technology produces lower levels of nitrogen oxides (NOx) than other 

combustion technologies. The CFB boilers operate at a relatively low temperature in the 

combustion zone producing less thermal NOx. 

2.2 PROCESS OPERATING DATA 

During a 30 day period that will include emissions testing and fuel analysis reporting, the 

following process information will be collected: total heat input; feed rate (if available); 

steam output; gross electric output; net electric output; emissions control devices in use 

during the test; control device operating or monitoring parameters (including, as 

appropriate to the control device, flue gas flow rate, pressure drop, scrubber liquor pH, 

scrubber liquor flow rate, sorbent type and sorbent injection rate), and process parameters 

(such as oxygen). These data will be averaged daily and included in the final report. 
 5

3.0 SAMPLING LOCATIONS 

Sample locations will be verified in the field to conform to USEPA Method 1. 

Acceptable cyclonic flow conditions will be confirmed prior to testing using USEPA 

Method 1, Section 11.4. 

TABLE 2: SAMPLING LOCATIONS SUMMARY 

Distance from nearest flow disturbance Sampling 

Location Stack ID Downstream 

EPA “B” 

Upstream 

EPA “A” 

Number of 

Traverse Points 

Outlet 139.5 

inches 

>93 feet 

(>8 duct diameters) 

>23.25 feet 

(>2 duct diameters) 

Twelve 

(three per port) 
 6

4.0 TEST PROGRAM AND METHODS 

4.1 TECHNICAL APPROACH 

The facility will correct daily averages from 30 days of CEM data in lieu of conducting a 

NOx and SO2 stack test. In order to correlate these emissions with other stack test 

emissions, a portion of the CEMS data will contain emissions data collected during this 

ICR test. The CEM meets the requirements of Title 40, Code of Federal Regulations, Part 

60, (40 CFR 60), Appendix B, Performance Specification 2 and ongoing QA/QC 

requirements of 40 CFR Part 75. 

4.2 SUMMARY 

The proposed emissions test program will be performed for the parameters specified in 

Table 4. Three, test runs for the listed parameters will be conducted. All test methods 

proposed for this compliance program conform to 40 CFR 60, Appendix A test 

procedures or those specified by the USEPA. 

TABLE 3: TEST PARAMETERS AND METHODS 

Parameters 

USEPA Test 

Method 

Duration 

(minutes) Reporting Units In-Stack Detection Limit 

acfm --- 

Velocity / Volumetric Flowrate scfm --- USEPA Methods 

1 & 2 60-240 

dscfm --- 

Carbon Dioxide (CO2) / 

Oxygen (O2) 

USEPA Method 

3A 60-240 %, dry basis 0.1 

Moisture USEPA Method 

4 60-240 % 0.02 

ppmvd --- 

Sulfur Dioxide (SO2) Plant CEMS 60 ppmvd @ 7% O2 --- 

lb/MMBTU --- 

ppmvd --- 

Nitrogen Oxides (NOx) Plant CEMS 60 ppmvd @ 7% O2 --- 

lb/MMBTU --- 

ppmvd 1.0 

Carbon Monoxide (CO) ppmvd @ 7% O2 0.001 USEPA Method 

10 

120 

lb/MMBTU 1.1 

ppmvd 0.4 

ppmvd @ 7% O2 0.4 Total Hydrocarbons (THC) as 

propane 

USEPA Method 

25A 

120 

lb/MMBTU 0.0007

 
 7

 

TABLE 3: TEST PARAMETERS AND METHODS (CONTINUED)

 

Parameters 

USEPA Test 

Method 

Duration 

(minutes) Reporting Units In-Stack Detection Limit 

ppmvd 1.7 

Methane ppmvd @ 7% O2 1.9 USEPA Method 

18 

120 

lb/MMBTU 0.001

lb/MMBTU (HCl) 0.0005

lb/MMBTU (HCN) 0.0001

Hydrogen Chloride (HCl), 

Hydrogen Cyanide (HCN) and 

Hydrogen Fluoride (HF) 

USEPA Method 

26A / CTM-033 60 

lb/MMBTU (HF) 0.0003

Suspended Particulate Matter / 

Multi-Metals 

USEPA Method 

29 240 lb/MMBTU See Section 4.6 

lb/MMBTU 

(filterable) 0.00006

Particulate Matter less than 2.5 

Microns (PM2.5)) 

USEPA OTM27 and USEPA 

OTM-028 

240 

lb/MMBTU 

(condensable) 0.0005

Mercury (Hg) USEPA Method 

30B 120 lb/MMBTU 2.20E-09 

ppmvd @ 7% O2 3.2 Formaldehyde USEPA Method 

320 120 

lb/MMBTU 0.006

4.3 VELOCITY AND VOLUMETRIC FLOW RATE MEASUREMENT 

SUMMARY: The outlet volumetric flow rate for each test run will be determined in 

accordance with USEPA Methods 1 and 2. Simultaneously, USEPA Methods 3A and 4 

will be conducted to quantify the oxygen, carbon dioxide and moisture content of the 

exhaust gas. 

CALIBRATION: Pitot tubes will be calibrated in accordance with USEPA Method 2. 

All new pitot tubes or those meeting the dimensions of USEPA Method 2, section 6.1, are 

assigned a baseline coefficient of 0.84, per section 10.1 of this method. All other pitot 

tubes are calibrated to establish the specific coefficient. A pitot tube coefficient of 0.99 is 

assigned to each standard pitot tube. 

DETECTION LIMITS: The lower detection limit for the pitot tube/manometer 

measurement system is 0.01 inches of water. 

OPERATING RANGE: The water manometer has a range up to 10 inches with 0.01 

increments. 
 8

PRINCIPLE OF OPERATION: The total stack or duct pressure is a combination of 

the static and the velocity pressure. The velocity pressure is also referred to as the delta 

P, which is equal to the total pressure minus the static pressure. 

 When a type S-pitot tube is connected to a water manometer, the total pressure and the static 

pressure are measured to yield the velocity pressure. The volumetric gas flow in a stack or 

duct is equal to the area times the velocity. 

4.4 CARBON DIOXIDE, CARBON MONOXIDE, OXYGEN, TOTAL 

HYDROCARBONS AND METHANE MEASUREMENT 

SUMMARY: Stack concentrations of carbon monoxide (CO), carbon dioxide (CO2), 

oxygen (O2) and total hydrocarbons (THC as methane), will be continuously sampled and 

analyzed with Avogadro’s real-time monitoring system (RTMS). Methane will sampled 

using Tedlar bags and analyzed via USEPA Method 18. 

SAMPLE SYSTEM DESCRIPTION: The RTMS is fully extractive, conforms to 

USEPA Method 7E and consists of a sampling interface system (SIS), an instrument 

control panel, and instruments. The SIS consists of a stainless steel probe with a 

calibration tee, a heated sampling line, a calibration gas line, a heated sample pump/filter 

and a semi-non-contact thermoelectric sample conditioner. 

The SIS will be used to cool, dry, filter, convey and distribute sample gas to the 

analytical instruments, which will be housed in one of Avogadro’s mobile laboratories. 

For total hydrocarbons, a portion of the unconditioned sample stream will be diverted 

through heated sample passages directly to the analytical instrument for continuous 

analysis. All sampling components leading to the analyzer will be heated to ≥110 °C (220 

°F). Actual temperatures will be recorded at 10-minute intervals during each test run. 

All instrument output signals will be recorded every 20-30 seconds simultaneously with a 

data logger and a personal computer. Each data point logged will be date/time stamped. 

Instruments, operating ranges and calibration gas concentrations that will be used for this 

test program are summarized in Table 4. Per Method 7E, the average concentration for 

each test run will be 20-100% of the chosen span. For THC, the analyzer range will be 

1.5 to 2.5 times the stack concentration and no less than 25 ppm. All monitors conform 

to the design and performance criteria outlined in 40 CFR 60 Appendix A. 
 9

Calibration gases will be USEPA Protocol. 

TABLE 4: REAL-TIME INSTRUMENTATION SUMMARY 

Parameter Analyzer Operating 

Principle 

Expected Average 

Concentrations 

(client to verify)

Calibration gases 

(% of span) 

CO TECO 48, 48s, 

or 48i 

Non-dispersive, 

infrared 15-20 ppm 0, 40-60, 100 

THC 

JUM VE7 or 

TECO 51 

Flame 

ionizationdetection very low 0, 25-35, 45-55, 80-90

O2

Infrared 

instruments or 

Servomex 

Electro-chemical 7.5-8 % 0, 40-60, 100 

CO2

Summit or Fuji 

ZRH 

Non-dispersive, 

infrared 11-12% 0, 40-60, 100 

PROCEDURE: Table 6 summarizes the quality assurance procedures to which the 

RTMS will be subjected in the field. 

Prior to the testing or during the first test run, a stratification test will be conducted for 

oxygen, as a surrogate for all gaseous test parameters, in accordance with USEPA 

Method 7E, Section 8.1.2. Stratification and traverse points will be determined using the 

criteria in Table 5. In lieu of stratification testing, all gaseous samples may be drawn 

from 12 traverse points chosen in accordance with EPA Method 1. 
 10

TABLE 5: REFERENCE METHOD TRAVERSE POINT DETERMINATION 

CRITERIA 

Number of 

stratification 

check points 

Criteria for all point Number of sample traverse 

points 

|D| ≤ 0.05A (NOx, CO, SO2, O2, CO2) or 

3 or 12 |D| ≤ 0.5 ppmv (NOx, CO, SO2) or 

|D| ≤ 0.3 %v/v (O2, CO2) 

1 (most representative of 

average) 

0.05A ≤ |D| ≤ 0.1A (NOx, CO, SO2, O2, 

CO2) or 

0.5 ppmv ≤ |D| ≤ 1.0 ppmv (NOx, CO, 

SO2) or 

3 

0.3 %v/v ≤ |D| ≤ 0.5 %v/v (O2, CO2) 

3 at 16.7%, 50.0%, and 83.3% of 

diameter 

0.05A ≤ |D| ≤ 0.1A (NOx, CO, SO2, O2, 

CO2) or 

3 on the line with the highest 

concentration, located at: 

0.5 ppmv ≤ |D| ≤ 1.0 ppmv (NOx, CO, 

SO2) or 

16.7%, 50.0%, and 83.3% of 

diameter (stack diameter <7.8 

feet) 

12 

0.3 %v/v ≤ |D| ≤ 0.5 %v/v (O2, CO2) 16”, 39” and 79” from stack wall 

(stack diameter >7.8 feet) 

|D| ≥ 0.1A (NOx, CO, SO2, O2, CO2) or 

3 or 12 |D| ≥ 1.0 ppmv (NOx, CO, SO2) or 

|D| ≥ 0.5 %v/v (O2, CO2) 

12 located per EPA Method 1 

|D| = difference between concentration at traverse point and total concentration average 

0.05A = 5% of the average concentration 

0.1A = 10% of the average concentration 

ppmv = parts per million by volume 

%v/v = percent volume 

With the exception of total hydrocarbons, calibration gas will be introduced directly to 

the instruments during the calibration/linearity error check. First, the instrument will be 

zeroed on the zero gas. The zero gas for all reference method analyzers will be <0.25% of 

span, except for THC, which will be <0.1 ppm (as methane). Then the instrument will be 

calibrated against the high-concentration calibration gas. The lower-concentration 

calibration gas(es) will then be used to check the instrument’s linearity, without making 

any adjustments to the instrument’s calibration. 

Excluding the sample probe, calibration gas will be introduced to the entire sample 

system during the bias check and the calibration/linearity error check of the total 

hydrocarbon analyzer. 
 11

Per EPA Method 25A, this eliminates the need for a separate bias check for total 

hydrocarbons. Whenever possible, the upscale gas used for the bias check and the 

calibration/zero drift checks will be the one closest to the measured average stack 

concentration. A post-test zero/calibration drift check may also serve as the bias check 

for the next test run. 

Instrument response to each calibration gas challenge will be documented on the strip 

chart recorder. Final run averages for all reference method analyzers will be calculated in 

accordance with Section 12.6 of USEPA Method 7E. 

TABLE 6: REAL-TIME INSTRUMENTATION FIELD QA PROCEDURES SUMMARY 

Check Frequency Limit 

Instrument 

calibration/linearity 

error 

• Beginning of each test day 

• Range change 

• After excessive calibration drift 

± 2% of span (except THC) 

± 5% of gas value (THC) 

Sample system bias Before and after each test run ± 5% of span 

Calibration/zero drift After each test run. ± 3% of span 

SAMPLE RATES AND DETECTION LIMIT: The in-stack detection limits outlined 

in Table 3 are based on an analytical detection limit of 1.0 parts per million by volume, 

dry (ppmvd). 

During each total hydrocarbon test run, a portion of the conditioned sample will be 

collected at a constant rate from the RTMS in a Tedlar gas bag. Each gas bag will then be 

analyzed via USEPA Method 18 for methane within 48 hours of the completion of 

sampling. Methane analysis (samples and standards) will be conducted in triplicate. 

4.5 HYDROGEN CHLORIDE, HYDROGEN FLUORIDE, HYDROGEN 

CYANIDE AND MOISTURE MEASUREMENT 

SUMMARY: Outlet hydrogen chloride, hydrogen fluoride and hydrogen cyanide 

emissions will be sampled isokinetically using a modified USEPA Method 26A. 

Hydrogen chloride and hydrogen fluoride emissions will be analyzed in accordance with 

USEPA Method 26A. Hydrogen cyanide emissions will be analyzed in accordance with 

Method CTM-033. 

The primary components of the sampling train include a heated probe, a heated filter, 

three impingers containing sodium hydroxide (NaOH) and an impinger containing silica 

gel. 
 12

Hydrogen cyanide present in the stack gas stream reacts with the NaOH to form a 

cyanide ion, which is retained in the alkaline solution until analyzed by ion 

chromatography (IC). Hydrogen chloride and hydrogen fluoride present in the stack gas 

stream reacts with the NaOH to form chloride and fluoride ions, which are retained in the 

alkaline solution until analyzed by ion chromatography (IC).

PREPARATION OF COLLECTION TRAIN: The entire sampling train is washed 

with detergent, rinsed with tap water, and finally rinsed with distilled/deionized water 

followed by acetone and allowed to air dry. 

The main components of the sample train are the stainless steel nozzle, the probe sheath 

and probe liner, the heated filter holder box, the filter holder itself, the type S pitot tube, 

the moisture or impinger train, the differential pressure gauge, and the metering system 

(vacuum gauge, leak-free vacuum pump and thermometers). The nozzle is connected to 

the probe sheath via a gas-tight connection to the inner (sampling) probe liner. 

The impinger train will consist of four unrestricted Greenburg-Smith impingers 

immersed in an ice bath and connected in series with glass crossovers. In order to 

maintain a pH at or above 12.0 as required by Method CTM-033, the first three 

impingers may contain up to 250 ml of up to 10N NaOH per impinger. The last 

impinger will contain approximately 200 grams of silica gel. The last impinger is 

connected to a positive displacement pump and a calibrated dry gas meter. The 

objective is for the last two reagent impingers to have a pH greater than 12.0. Alizarin 

yellow indicator will be added to the impingers. If the indicator shows that the impinger 

pH is starting to approach 12, additional caustic may be added to the impingers to raise 

the pH. The pH of the last reagent impinger will be checked at the end of the run to 

ensure that the pH is above 12.0. If the pH is found to be below 12.0, the run will be 

repeated. 

SAMPLE TRAIN OPERATION: A single train traversing the stack cross sectional 

area will be used for the entire test run. 

The temperature of the gas stream in the sample train is maintained at a minimum 

temperature of 248o

F to prevent condensation from occurring. This includes the probe 

and filter box temperatures. The filter and filter housing are connected to the impinger 

train. 

During testing, a sample rate is maintained such that it is within 10 percent of the true 

isokinetic. First, the manometer is leveled and zeroed. 

The sample train is assembled and leak checked. The initial dry gas meter volume is 

recorded, and the sampling train is placed at the first sampling point in the stack. 
 13

At this point, the stack gas velocity, the stack temperature and initial gas meter volume 

are all recorded in order to establish the proper sample rate. 

At each traverse point in the stack, the following data are recorded: 

• the temperature of the stack gas; 

• the meter system temperatures; 

• the probe and filter holder temperatures; 

• the exit impinger temperature; 

• the sampling rate. 

This procedure is repeated until the end of the test run. 

LEAK-CHECK PROCEDURES: A leak-check of the entire sample train will be 

performed prior to and after each test run. Leak checking is performed by plugging the 

nozzle and pulling a controlled vacuum in the sample train equal to or greater than the 

highest sample vacuum obtained during the test run. If the leakage rate is measured to 

be less than 0.02 cubic feet per minute (cfm), then it is acceptable. If the leak rate is 

higher, the tester shall, at the discretion of the regulatory personnel, either record the 

leakage rate and correct the sample volume, or void the test run. 

SAMPLE VOLUMES AND DETECTION LIMITS: The in-stack detection limits 

listed in Table 3 are based upon an analytical detection limit of 0.434 ug/ml for 

hydrogen chloride, 0.217 ug/ml for hydrogen fluoride and 0.104 ug/ml for hydrogen 

cyanide, an estimated impinger reagent sample volume of 1,000 ml and a gas sample 

volume of 30 cubic feet. Each test run will be one hour in duration. 

Large amounts of NaOH will likely be needed in order to keep the impinger pH above 

12, because the high stack CO2 consumes the NaOH during sampling. The additional 

NaOH does not affect the detection limit for HCN and is not expected to change the 

detection limit for HCl and HF. 

SAMPLE RECOVERY: The recovery of each sample train is conducted onsite. The 

sampling train is transferred to an area that is clean and protected from external 

conditions. The impingers will be disassembled and wiped free of any water or ice. The 

impinger contents are weighed (to the nearest tenth of a gram) for moisture 

determination. The contents of the impingers along with NaOH impinger rinses will be 

added to container #1. The filter will be discarded after the test run. 

A reagent blank of NaOH will be collected based upon the concentration used during the 

runs. 
 14

Samples will be transported from the test site to Avogadro Environmental’s lab for 

assignment of chain-of-custody and transfer to Enthalpy Analytical, Inc. for analysis. 

ANALYSIS: The impinger samples and blanks will be analyzed by ion 

chromatography by Enthalpy Analytical, Inc. 

4.6 PARTICULATE MATTER, MULTI-METALS AND MOISTURE 

MEASUREMENT 

 

SUMMARY: Stack gas will be sampled isokinetically for suspended (filterable) 

particulate and metal emissions in accordance with USEPA Method 29. Suspended 

particulate in the sampled gas will be collected in the sample train on a heated glass fiber 

filter. Metals in the sampled gas will be collected in the sample train on a filter and in 

acidic impinger reagents. Recovered samples will first be analyzed gravimetrically for 

particulate in accordance with EPA Method 29. Then the samples will be digested and 

analyzed for antimony (Sb), arsenic (As), beryllium (Be), cadmium (Cd), total 

chromium (Cr), cobalt (Co), lead (Pb), manganese (Mn), nickel (Ni) and selenium (Se), 

in accordance with Method 29. 

Key sample train components will include: 

• a sized, tapered –edge, glass “button-hook” sample nozzle, 

• a stainless steel sample probe with a heated glass liner, S-type pitot tube and 

thermocouple 

• a heated glass filter holder with a low-metals quartz fiber filter supported by a 

Teflon frit 

• a condenser system consisting of Greenburg-Smith glass impingers and connecting 

pieces 

• a sample control/metering system consisting of a vacuum pump, dry gas meter, 

sample flow controls, sample rate manometer, stack gas velocity manometer, 

temperature indicator and heat controllers. 

PREPARATION OF SAMPLING TRAIN: Sampling glassware and sample 

containers will be cleaned prior to sampling. A soap and water wash followed by a fourhour soak in 10% HNO3 (plastic ware will be rinsed only) and triplicate rinse with 

distilled, deionized water and an acetone rinse (probe and nozzle only) will be used to 

clean the glassware. 

The condenser will consist of four impingers. All impingers except the third will be 

Greenburg-Smith modified with unrestricted impinger tubes. Impinger 3 will be a 

standard Greenburg-Smith impinger. 
 15

Each impinger will be charged for sampling as follows: 

• Impinger 1, moisture knock-out 

• Impingers 2 & 3, 100ml 5% HNO3 / 10% H2O2. 

• Impinger 4, silica gel. 

All impingers will be weighed prior to sampling. Solutions of 5% HNO3/10% H2O2 will 

be used within 24 hours of preparation. 

LEAK-CHECK PROCEDURES: A leak-check will be performed prior to and after 

each test by creating a vacuum in the sample train equal to or greater than the highest 

sample vacuum obtained during the test. A leakage rate found to be no greater than 0.02 

cubic feet per minute is acceptable. If a higher leakage rate is obtained, the tester shall 

at the discretion of the regulatory personnel, either record the leakage rate and correct 

the sample volume, or void the test run. 

SAMPLE VOLUMES AND DETECTION LIMITS: Detection limit for particulate 

matter summarized in Table 3 are based on an analytical detection limit of 0.0002 grams 

and a sample volume of 3.4 cubic meters. Each test run will be a minimum of four hours 

in duration. 

Detection limits for the metals are summarized in Table 7 and are based on a sample 

volume of 3.4 cubic meters. Each test run will be a minimum of four hours in duration. 

TABLE 7: SUMMARY OF MULTI-METALS DETECTION LIMITS 

 Detection Limit 

Analytical, μg/sample In-stack, Pounds/MMBTU Metal 

Front Half Back Half Front Half Back Half 

Antimony 0.4 0.2 1.20E-07 6.01E-08 

Arsenic 0.4 0.2 1.20E-07 6.01E-08 

Beryllium 0.1 0.05 3.00E-08 1.50E-08 

Cadmium 0.1 0.05 3.00E-08 1.50E-08 

Chromium 0.3 0.15 9.01E-08 4.51E-08 

Cobalt 0.1 0.05 3.00E-08 1.50E-08 

Lead 0.2 0.1 6.01E-08 3.00E-08 

Manganese 0.75 0.25 2.25E-07 7.51E-08 

Nickel 0.5 0.25 1.50E-07 7.51E-08 

Selenium 1 0.5 3.00E-08 1.50E-07 
 16

SAMPLE TRAIN OPERATION: A single train traversing the affected stack cross 

sectional area shall be used for the entire test. The sampling system will consist of a 

sized tapered edge nozzle constructed of glass. The nozzle is connected to a stainless 

steel support tube via a gas-tight connection to a glass inner sampling probe. The gas 

stream will enter a four inch diameter glass fiber filter supported by a quartz glass frit. 

The gas stream temperature will be 250° F (+ 25° F). 

During testing, a sample rate is maintained such that it is within 10 percent of the true 

isokinetic. First, the manometer is leveled and zeroed. The sample train is assembled 

and leak checked. The initial dry gas meter volume is recorded, and the sampling train 

is placed at the first sampling point in the stack. At this point, the stack gas velocity, the 

stack temperature and initial gas meter volume are all recorded in order to establish the 

proper sample rate. 

At each subsequent traverse point in the stack, the following data are recorded: 

• the temperature of the stack gas; 

• the meter system temperatures; 

• the probe and filter holder temperatures; 

• the exit impinger temperature; 

• the sampling rate 

This procedure is repeated until the end of the test run. 

SAMPLE RECOVERY: Sample recovery will occur onsite in the mobile CEM lab 

or in an adequately clean environment. 

The filter is placed into a petri dish (container 1) and sealed to prevent sample loss. The 

probe, nozzle, liner, and the front half of the filter will be washed and brushed with 

acetone into one container (container 2) until the rinse shows no visible particles. The 

amount of acetone used to rinse the front-half sample train components will be at least 

200 milliliters or 30 milliliters per foot of probe length, whichever is greater. The 

impingers will be disassembled and wiped free of any water or ice, and the volume is 

weighed to the nearest gram to determine moisture content. 

 

The probe and nozzle will be rinsed three times with a total of 100 ml of 0.1N HNO3

into a high-density polyethylene (HDPE) sample jar (container 3). Impingers 1, 2 & 3 

contents will be transferred to a HDPE sample jar (container 4). 

Impingers 1, 2 & 3 and connecting glassware will then be rinsed three times with a total 

of 100 ml 0.1N HNO3 into container 4. 
 17

A sample blank of acetone, equivalent to that used for the probe and nozzle rinse for 

each run, will be collected and submitted for analysis. An HDPE jar containing 100 ml 

0.1N HNO3 will be recovered as a front-half rinse blank. A HDPE jar containing 200 ml 

5% HNO3/10% H2SO4 and 100 ml 0.1 N HNO3 will be recovered as a back-half blank. 

ANALYTICAL PROCEDURES: All sample containers will be sealed, labeled and 

marked for fluid level prior to shipment. Samples will be transported or shipped from 

the site by Avogadro personnel. Each sample will be logged on a chain of custody form 

that will accompany the samples to Maxxam Analytics. Prior to shipment, the filters are 

desiccated to constant weight for quantifying the weight gain at the Avogadro 

laboratory. 

At Maxxam Analytics, the acetone rinse will be dried, desiccated and the residue 

quantified as particulate. The acetone rinse residue will then be combined with the 

remaining front-half sample fractions. Front-half and back-half fractions will be 

analyzed separately via Method 29. Inductively coupled plasma mass spectrometry 

(ICP/MS) analysis for all metals will utilize SW-846-6020. 

4.7 MERCURY MEASUREMENT 

MERCURY MEASUREMENT 

SUMMARY: Mercury will be measured in accordance with USEPA Method 30B. The 

analytical procedure for USEPA 30B incorporates the use of solid-sorbent traps filled 

with two segments of iodinated charcoal. Mercury collected onto each segment is then 

desorbed and analyzed separately by thermal decomposition (700°C) outfitted to an AA 

Spectrometric detector. This procedure is referred to as the “thermal procedure” in 

USEPA Method 30B. A sampling train using paired sorbent traps will be used to collect 

samples from the outlet.

Samples are quantified utilizing a calibration curve. The calibration curve is determined 

on the day of analysis by analyzing a minimum of three standards in order to provide a 

minimum of three calibration points. At the end of each set of analysis a post calibration 

is conducted. 

SAMPLING TRAIN: The sorbent traps will be approximately 12 inches long for high 

moisture sources and have two chambers. Both chambers will be carbon impregnated 

and will capture vapor phase Hg. 
 18

The sampling train consists of two sorbent traps mounted at the end of one sampling 

probe in a manner that allows for the gas stream to enter the traps directly. The probe 

will be heated in order to prevent moisture condensation in the probe. After exiting the 

probe, the sample gas stream will pass through a condenser to remove moisture prior to 

entering the metering system. The metering system will consist of either a dry gas meter 

or a mass-flow sensor and a sample pump. If a mass flow sensor is used to measure 

sample volumes, its accuracy will be checked against a second standard in the field 

while sampling stack gas as described in section 10.2.2.5 of Method 30B. 

SAMPLE VOLUMES AND DETECTION LIMITS: The detection limits for 

mercury summarized in Table 3 are based on an analytical detection limit of 0.36 

nanograms and a sample volume of 167 liters. Each test run will be a minimum of two 

hours in duration. 

 

FIELD RECOVERY PAIRED SAMPLE TESTS: For each pair of traps sampled 

during each test run, one will be spiked with 50 ng of Hg onto the front section of the 

trap and the second trap will be un-spiked. Because of the special handling 

considerations for internal spiking and to enhance quality assurance this procedure will 

be performed at Ohio Lumex. 

Both the spiked and un-spiked traps will be analyzed in the same batch and in the same 

manner. Once the amount of mercury found in the spiked trap is corrected for the spike, 

it will be compared to the amount of mercury in the un-spiked trap to see if the amounts 

found agree as specified in Section 8.2.6.2 of Method 30B. 

SAMPLE TRAIN OPERATION: Before sampling, a leak check will be performed 

with the sorbent traps in place. A vacuum will be drawn through the probe and adjusted 

to approximately 15”Hg. Using the gas meter, a leak rate will be determined and must 

not exceed 4% of the target sampling rate. Once the leak check passes the criteria, the 

vacuum will be carefully released and the sorbent trap inlet will be sealed until the probe 

is ready for insertion. 

After performing the leak check, the sample collection is accomplished by removing the 

plug from each end of the traps and inserting the probe through the port, turning on the 

pump, and sampling at the target rate. The sample rate will remain constant (+/- 10%) 

through both sample traps throughout each test run. The sampling train will be leakchecked a second time after each test run has been completed, at the highest pressure 

drop encountered during the test run. The train is returned to atmospheric pressure and 

the sorbent traps will be carefully removed. 
 19

SAMPLE RECOVERY AND ANALYSIS: After the traps have been removed from 

the probe, both ends will be sealed and the traps will be wiped clean and placed in a 

clean storage container to be sent to Ohio Lumex for analysis. 

4.8 PARTICULATE MATTER LESS THAN 2.5 MICRONS (PM2.5) AND 

MOISTURE MEASUREMENT 

SUMMARY: Stack gas will be sampled for PM2.5 emissions in accordance with 

USEPA Other Test Method 27 and Other Test Method 28. 

Suspended (filterable) and condensable particulate matter (CPM) with an aerodynamic 

particle size of 2.5 microns or less will be separated from the sampled gas with an instack cyclone and collected on a glass fiber filter and in water. 

The CPM is collected in the water dropout impinger, the modified Greenburg Smith 

impinger and a CPM filter of the sampling train. The organic and aqueous fractions will 

then be taken to dryness and the residues weighed. The total of both fractions represents 

the CPM. 

Recovered samples will then be analyzed gravimetrically for particulate in accordance 

with Method OTM-27 and OTM-28. 

Key sample train components will include: 

• An in-stack, stainless-steel cyclone and sample nozzle meeting the specifications of 

EPA Other Test Method 27 for PM2.5 sampling; 

• A stainless-steel sample probe with a heated glass liner, S-type pitot tube, probe 

extension and thermocouple; 

• Condenser followed by a dropout impinger; 

• CPM filter holder; 

• A sample control/metering system consisting of a vacuum pump, dry gas meter, 

sample flow controls, sample-rate manometer, stack gas velocity manometer, 

temperature indicator, and heat controllers. 

PREPARATIONS: The cyclone will be cleaned with acetone prior to sampling. The 

glassware portion of the sampling train is washed with soap and water, rinsed with tap 

water, rinsed with distilled/deionized water, rinsed with acetone and finally rinsed with 

MeCl2. After cleaning, the glassware will be baked at 300 ̊C for 6 hours prior to each 

source type sampled. 
 20

Prior to each test run, the glassware used to collect CPM must be rinsed thoroughly with 

deionized, distilled ultra-filtered water that conforms to ASTM D1193-06, Type 1. 

ONSITE LEAK-CHECK PROCEDURES: A leak-check will be performed prior to 

and after each test by plugging the nozzle and creating a vacuum in the sample train 

equal to or greater than the highest sample vacuum obtained during the test. A leakage 

rate no greater than 0.02 cubic feet per minute (cfm) is acceptable. If a higher leakage 

rate than 0.02 cfm is obtained post run, the tester shall, at the discretion of the regulatory 

personnel, either record the leakage rate and correct the sample volume, or void the test 

run. 

SAMPLE VOLUMES AND DETECTION LIMITS: The in-stack detection limits 

outlined in Table 3 are based on an analytical detection limit of 0.0002 grams for 

filterable PM, 0.0015 for condensable PM and a sample volume of 3.4 cubic meters. 

Each test run will be up to six hours in duration. 

SAMPLE TRAIN OPERATION: Completion of each test run will include the 

following key procedures: 

• Proper sample rate and nozzle size will be selected in accordance with Sections 8.5 

through 8.5.5 of Method OTM-27. 

• A pre-test leak check of the entire sample train will be conducted. 

• Sample time at each sample point will be varied for local delta P in accordance with 

Equations 22 and 23 of Method OTM-27. 

• Probe heat will be maintained to prevent internal moisture condensation. Ice will be 

maintained in the impinger ice bath. The CPM filter temperature will be maintained 

at <85 ̊F. The moisture train exit temperature will be maintained at <68 ̊F. 

• A post-test leak check will be performed on the entire sample train without the instack cyclone at a vacuum equal or greater than the highest vacuum achieved during 

the test run. 

• All necessary data for each sample point and test run will be recorded on appropriate 

data forms. 

POST TEST NITROGEN PURGE: After the post-test leak check, a nitrogen purge 

of the impinger train will be conducted. During the purge, the temperature at the exit of 

the silica gel impinger will be monitored and maintained below 68 ̊F. The temperature 

at the exit of the CPM filter will be monitored and maintained below 85 ̊F. If no water 

was collected before the CPM filter, then the nitrogen purge will be omitted. 
 21

During the purge, a stem will be inserted into the dropout impinger. The impinger tip 

length will extend below the water level in the impinger catch. If insufficient water was 

collected, then a measured amount of degassed deionized, distilled ultra-filtered ASTM 

D1193-06, type 1 or equivalent, water will be added until the impinger tip is at least 1 

cm below the surface of the water. The amount of water added to the dropout impinger 

to correct the moisture content of the effluent gas will be recorded. The train will be 

purged using nitrogen for one hour using zero-grade ultra-high purity nitrogen. 

SAMPLE RECOVERY: Sample recovery will be performed in the field in a suitable 

area that is clean and protected from external conditions. Each impinger will be 

weighed to 0.1 gram for moisture determination. 

OTHER TEST METHOD 27: 

The particulate filter and loose particulate will be transferred to a plastic petri dish. The 

PM2.5 exit tube and filter holder front-half will be brushed and rinsed with acetone into 

an amber glass bottle. 

A sample blank of acetone will be collected in a separate amber glass container, adding 

a volume of acetone equal to the volume used for sample cleanup. 

OTHER TEST METHOD 28: 

Tweezers and/or clean disposable gloves will be used to remove the CPM filter from the 

CPM filter holder. The contents of the CPM impingers (impinger catch) will be 

transferred to a clean sample container (glass or plastic). 

A distilled water rinse of the probe, probe extension, condenser, CPM impingers, 

impinger connectors, CPM filter front-half and particulate filter-holder back-half will be 

completed twice, and the rinse will be added to a clean sample container. Next, an 

acetone rinse of these same components will be performed, followed by duplicate 

methylene chloride rinses. The acetone and methylene chloride rinses will be combined 

into a clean sample container. 

Blanks will be recovered as follows: 

Sample blanks of distilled water, acetone and methylene chloride will be collected in 

clean sample containers, adding volumes equal to the volume used for sample cleanup. 
 22

FIELD TRAIN BLANK: One field train blank will be recovered for the test program. 

 The sampling train will be assembled as described above, except 100 mL of water will 

be added to the first impinger. The field train blank will be purged and recovered in the 

same manner as the test run samples, as described above. 

SAMPLE SHIPMENT AND STORAGE: Samples will be labeled according to 

scenario and test run number. All samples will be transported from the test site to 

Avogadro’s offices for a final quality assurance check prior to analysis at Avogadro and 

Maxxam Analytical. The samples will be stored in their recovery containers until 

analysis. 

SAMPLE ANALYSIS: PM2.5 analysis will be performed in accordance with Section 

11.0 of OTM-27. Filters will be dried and desiccated to a constant weight. After 

measuring the quantity of acetone in container 2, its contents will be transferred to a dry, 

desiccated and tared evaporation vessel. After evaporating the acetone, the vessel will be 

dried, desiccated, and re-weighed to a constant weight. 

The CPM samples will be processed according to Figure 6 of Method OTM-28 at 

Maxxam Analytical. 

4.9 FORMALDEHYDE MEASUREMENT 

 

Formaldehyde emissions will be measured at the outlet stack in accordance with USEPA 

Method 316, “Sampling and analysis for formaldehyde emissions from stationary 

sources in the mineral wool and wool fiberglass industries”. 

PRINCIPLE AND APPLICABILITY: Gaseous and particulate pollutants are 

withdrawn isokinetically from the source and are collected in distilled/deionized (DI) 

water. The DI water is then analyzed using the modified pararosaniline method. 

The main components of the sample train are the stainless steel nozzle, the probe sheath 

and glass probe liner, the type-S pitot tube, the moisture or impinger train, the 

differential pressure gauge, and the metering system (vacuum gauge, leak-free vacuum 

pump and thermometers). 

PREPARATION OF SAMPLING TRAIN: The glassware portion of the sampling 

train is washed with soap and water, rinsed with tap water and rinsed with 

distilled/deionized water. For each test run, the first two impingers are filled with 

approximately 100 grams of DI water. The third impinger is empty, and the fourth 

impinger is charged with approximately 200 grams of silica gel. 
 23

LEAK-CHECK PROCEDURES: A leak-check of the entire sample train will be 

performed prior to and after each test run. Leak checking is performed by plugging the 

nozzle and pulling a controlled vacuum in the sample train equal to or greater than the 

highest sample vacuum obtained during the test run. If the leakage rate is measured to 

be less than 0.02 cubic feet per minute (cfm), then it is acceptable. If the leak rate is 

higher, the tester shall, at the discretion of the regulatory personnel, either record the 

leakage rate and correct the sample volume or void the test. 

SAMPLE VOLUMES AND DETECTION LIMITS: The in-stack detection limits 

outlined in Table 3 are based on an analytical detection limit of 5 ug and a sample 

volume of 30 cubic feet. Each test run will be a minimum of two hours in duration. 

SAMPLE TRAIN OPERATION: During testing, a sample rate is maintained such 

that it is within 10 percent of the true isokinetic. First, the manometer is leveled and 

zeroed. The formaldehyde sample train is assembled and leak checked. The initial dry 

gas meter volume is recorded, and the sampling train is placed at the first sampling point 

in the stack. At this point, the stack gas velocity, the stack temperature and initial gas 

meter volume are all recorded in order to establish the proper sample rate. 

 

At each subsequent traverse point in the stack, the following data are recorded: 

• the temperature of the stack gas; 

• the meter system temperatures; 

• the probe and filter holder temperatures; 

• the exit impinger temperature; 

• the sampling rate 

This procedure is repeated until the end of the test run. 

The temperature of the probe is maintained at approximately 248°F +/- 25°F to prevent 

condensation from occurring. The impinger temperatures are maintained to allow 

proper condensation to occur. At no time will the last (exit) impinger temperature 

exceed 68o

F. Accordingly, ice and/or cold water is added, as necessary. 

SAMPLE RECOVERY: The recovery of the formaldehyde sample train is conducted 

onsite. The sampling train is transferred to an area that is clean and protected from 

external conditions. The impingers will be disassembled and wiped free of any water or 

ice. The impinger contents are weighed (to the nearest tenth of a gram) for moisture 

determination. The probe nozzle, probe fitting and the glass liner are washed and 

brushed with DI into one container at least three times and until the rinse shows no 

visible particles. 
 24

Empty the contents of the first three impingers into the same sample bottle. The first 

three impingers and the connecting glassware are rinsed three times with DI water and 

added to same sample container. 

 

A sample blank of DI water is collected in a separate polyethylene bottle adding a 

volume of water equal to the volume used for sample cleanup. [less than or equal to 100 

milliliters (ml)] 

SAMPLE TRANSPORTATION AND STORAGE: Each sample is given a sample 

number and corresponding label for identification purposes. Each sample container is 

sealed and taped to prevent leakage, contamination, or loss. Immediately after recovery, 

samples will be stored cold. Samples are transported from the test site to Avogadro’s 

offices for a final quality assurance check prior to analysis. All samples will be 

shipped cold to the laboratory. 

ANALYTICAL PROCEDURES: Each water sample and the water blank will be 

analyzed by the modified pararosaniline method. 
 25

5.0 QUALITY ASSURANCE / QUALITY CONTROL INFORMATION 

5.1 TEST EQUIPMENT AND INSTRUMENTATION 

Avogadro has access to all items of sampling, measurement, and test equipment required for 

the correct performance of the tests, or calibrations, or both (including sampling, preparation 

of test and/or calibration items, processing and analysis of test and/or calibration data). 

Avogadro’s equipment and software used for testing, calibration, and sampling is capable of 

achieving the required accuracy and complies with specifications relevant to the tests and/or 

calibrations concerned. Avogadro ensures that before being placed into service, equipment 

(including that used for sampling) is calibrated or checked to establish that it meets 

Avogadro’s specification requirements and complies with the relevant standard 

specifications. Additionally, Avogadro ensures that equipment is operated by trained and 

authorized personnel. 

Avogadro assigns a unique identifier to each item of sampling, measurement, and test 

equipment that requires traceability, routine and/or scheduled maintenance, requires routine 

and/or scheduled calibrations and/or has a specific lifespan. The unique identifier is 

prominently and indelibly applied to the item and assignments are documented in the 

inventory management system. 

This equipment is maintained in good operating order and calibrated at regular intervals in 

accordance with the test procedures for which it is used. Additionally, documentation 

substantiating service dates and calibration and maintenance histories is maintained. 

Avogadro uses data sheets and maintains logbooks to capture this information. 

Copies of equipment manuals and calibration records are kept in the Avogadro office so that 

the information is readily available to users and observers. Additionally, each piece of test 

equipment is sent to the field with a reasonable inventory of field-replaceable spare parts. 

Field teams are capable of performing minor service and repairs in the field. Unless the 

service action requires the use of spare parts, the service or maintenance action is not 

recorded. When equipment cannot be serviced in the field, it is tagged and removed from 

service until it is repaired. Service actions that require the use of spare parts, originate from 

field tagging, or are performed by third parties are reviewed to determine when the service 

requirement may have affected test results for other test programs. In the event test results 

for other programs are affected, clients are notified and follow-up actions are completed. 
 26

Avogadro will rent or lease test equipment when there is insufficient equipment in-house to 

adequately service jobs, when owned equipment is being repaired, or when specialized 

equipment is required. Avogadro ensures that when it uses equipment outside its permanent 

control, all requirements of ASTM D 7036 are met. Providers of rental equipment are 

required to furnish documentation indicating acceptable performance of the equipment at the 

time it is shipped. Rented equipment, while not subject to Avogadro’s maintenance 

program, is subject to the calibration requirements of the test method. For this reason, 

Avogadro performs appropriate pre- and post-test calibrations of rented test equipment. 

Test equipment and instrumentation is often used in the field in an industrial environment. 

Whenever possible and practical, test equipment and instrumentation is used within a mobile 

laboratory that provides a satisfactory operating environment for the equipment; however, 

some projects require that test equipment and instrumentation be operated in uncontrolled 

environments. In these instances, environmental factors and their potential impacts will be 

recorded in calibration logs or on data sheets and reported in the test report. 

5.2 CALIBRATION AND HANDLING OF TEST EQUIPMENT AND 

INSTRUMENTATION 

All equipment used for tests, or calibrations, or both, including equipment for subsidiary 

measurements (for example, for environmental conditions) having a significant effect on the 

accuracy or validity of the result of the test, calibration or sampling will be calibrated by 

Avogadro before being put into service. Where possible, Avogadro will use reference 

materials traceable to certified reference materials. Checks needed to maintain Avogadro’s 

confidence in the calibration status of reference, primary, transfer or working standards and 

reference materials will be carried out, as far as technically and economically practicable, in 

accordance with defined procedures and schedules. 

Avogadro has established calibration programs for key quantities or values of the 

instruments where these properties have a significant effect on the results. For example, the 

test equipment manufacturer specifies specific maintenance requirements and Avogadro 

adheres to these requirements. Additionally, calibration requirements are set forth in 

individual test methods and Volume III of the Quality Assurance Handbook for Air Pollution 

Measurement Systems: Stationary Source Specific Methods. Avogadro calibration 

procedures conform to the requirements set forth in these documents. Where appropriate, 

maintenance and calibration procedures are described or referenced in standard operating 

procedures (SOPs). Where applicable, these calibration procedures are traceable to National 

Institutes of Standards and Technology (NIST) reference materials. While Avogadro 

performs most maintenance and calibration activities in-house, Avogadro relies on a vendor 

for annual calibration of mass flow controllers used in dilution systems. 
 27

Avogadro checks the calibration of analytical balances on each day of use with mass 

standards that bracket the range of use, checks the function and calibration of top loading 

balances monthly and either (i) replaces the balances annually or (ii) performs maintenance 

service and recalibrations annually. These daily calibrations are recorded in the log book. 

Thermometers and other temperature measurement equipment are checked periodically, and 

at least annually (quarterly in the case of dial thermometers), against a NIST traceable 

thermometer and appropriate correction factors are developed and applied. 

Copies of calibration data, along with the identification number for the calibrated equipment, 

are stored in either the logbook or requisite project file, and when appropriate, kept with the 

equipment. 

Test equipment, instrumentation, and related calibration standards are handled and stored in 

manners that ensure their integrity, prolong their useful service lives and that provide 

adequate protection to personnel, facilities, equipment, and the environment. Equipment is 

labeled with regard to calibration status and tagged and removed from service if it requires 

repair. Equipment is stored in protected and secure areas. Equipment is properly discarded 

at the end of their useful service life. 

All sampling equipment and instrumentation to be used for this test program are 

calibrated per the applicable test method. Copies of all pre-test and post-test calibration 

data will be included in the final test report. The information presented below addresses 

specific quality assurance items not mentioned in the sections above. Additional 

calibration information may include but is not limited to the following: 

• Dry Gas Meters: Dry gas meters are calibrated prior to use in accordance with 

USEPA Method 5, section 10.3 using a dry gas meter as described in section 16.1. 

Dry gas meter calibrations will be verified in the field in accordance with 

Alternate Method 009, unless data is not available, then post-test calibration 

checks will be performed as per section 10.3.2 of USEPA Method 5. 

• Span Gas Certifications: Each gas supplier provides span gas certifications, and 

copies will be included in the final test report. 

• Thermocouples: Stack temperature thermocouple calibrations are checked after 

each field use in accordance USEPA Alternative Method 2 (ALT-011) by 

comparing the thermocouple to an ASTM mercury-in-glass thermometer at a 

single, convenient temperature. The thermocouple reading must agree within +2o 

F of the thermometer reading. 
 28

Stack temperature thermocouple measurement system continuity will be checked 

in the field prior to sampling in accordance with ALT-011 by observing that the 

temperature reading changes as expected upon insertion or withdrawal of the 

thermocouple from the stack. 

• Heated Sample Lines: Heated sample lines temperature will be visually 

observed and recorded at 15 minute intervals during each test run.

• Nozzles: Copies of calibration data for all glass and/or stainless steel nozzles 

used during the test program will be included in the final report. 

5.3 DATA COLLECTION AND MANAGEMENT 

Insofar as is feasible, recorded information is created using standardized electronic media 

and software. These activities are performed using personal computers (PCs) with or 

without Local Area Network (LAN). The LAN is backed-up on a daily basis and data are 

stored for ten years. Standardized directory formats are used for the storage of client and 

Avogadro administrative files. 

Avogadro is able to provide documentation or otherwise demonstrate on request that it 

complies with the relevant and appropriate federal, state, and local requirements for 

conducting testing procedures under its scope, including compliance with ASTM D 7036. 

Additionally, Avogadro is able to provide documentation or otherwise demonstrate on 

request that it complies with applicable local, state, and federal requirements governing 

health and safety, transportation, shipping, and other relevant requirements. 

Avogadro has established and maintains procedures for handling, control and storage of all 

documents (including quality and technical records) that form part of its quality system 

(internally generated or from external sources). Quality records include reports from 

customer and regulatory authority feedback, internal audits and management reviews as well 

as records of corrective and preventive actions. All records will be (1) legible, (2) stored in 

facilities that provide a suitable environment to prevent damage or deterioration and to 

prevent loss, and (3) retained in such a way that they are readily retrievable. All records in 

possession of Avogadro are secure and held in confidence in accordance with established 

record retention periods. Avogadro has procedures to protect and back-up records stored 

electronically and to prevent unauthorized access to or amendment of these records. At the 

end of the designated retention period, records are destroyed or returned to the client. 
 29

Avogadro retains records of original observations, derived data and sufficient information to 

establish an audit trail, calibration records, staff records and a copy of each test report or 

calibration certificate issued, for a defined period. The records for each test or calibration 

contain sufficient information to facilitate, if possible, identification of factors affecting the 

uncertainty and to enable the test or results, or calibration to be repeated under conditions as 

close as possible to the original. The records include the identity of personnel responsible 

for the sampling performance of each test, or calibration, or both. 

Other records include but are not limited to quality records, results of internal and external 

audits, training and qualification records for personnel, performance feedback, gas 

certifications, and chain-of-custody records. Observations, data and calculations are 

recorded at the time they are made and are identifiable to the specific task. When mistakes 

occur in records, each mistake is crossed out, not erased, made illegible or deleted, and the 

correct value entered alongside. Such alterations to records are dated and signed or initialed 

by the person making the correction. In case of records stored electronically, equivalent 

measures are taken to avoid loss or change of original data. 

SPREADSHEETS 

Spreadsheets are an essential tool for the reduction and management of emission testing data 

and Avogadro relies on a number of standard spreadsheets for routine work. When 

spreadsheets are initially developed, they are checked against a known data set or by hand 

calculations. Once the accuracy and reliability of the spreadsheet have been established, the 

master version is password protected to prevent overwriting. Only the master version is to 

be used for project work. This is accomplished by opening the master version, 

acknowledging that it is a read-only version and then saving it with a new name. Once the 

document has been saved with a new name, data can be entered and saved. 

Attachment 1 contains example calculations relevant to the proposed testing. 

HANDWRITTEN DATA AND RECORDS 

Field data are often recorded by hand. Handwritten field data must be recorded in indelible 

ink. When corrections are made, they are made such that the original entry is not obliterated 

(i.e., a single line is drawn through the erroneous entry). Each correction is initialed and 

dated. 
 30

It is often necessary to transfer handwritten data to spreadsheets for data reduction purposes 

and the accuracy of the transfer must be verified by either the person making the transfer or 

by another individual. Once data transfer accuracy has been verified, the spreadsheet is 

printed, initialed and dated by the verifier. 

Occasionally, it may be necessary to modify quality system or project documents (e.g., test 

plans, SOPs, data summaries, etc.) by hand. In cases where it is necessary to amend a 

document by hand, the document will be formally re-issued as soon as practicable. 

Original signature and initials are maintained in appropriate company files. 

Attached 3 contains sample field data sheets relevant to the proposed testing and a blank 

chain of custody form. 

TEST REPORTS 

The results of each test, calibration or series of tests or calibrations carried out by Avogadro 

will be reported accurately, clearly, unambiguously and objectively, and in accordance with 

any specific instructions in the test or calibration methods. Avogadro test reports adhere to a 

standard format that is determined by the scope of work. Each report bears a unique project 

number and each page in the report is numbered. The report includes all information 

requested by the client and relevant regulatory authority and necessary for the interpretation 

of the test or calibration results and all information required by the method used. Each test 

report or calibration certificate includes at least the following information, unless Avogadro 

has valid, documented reasons for not including it: 

• A title, 

• The name and address of Avogadro and the testing location, 

• Unique identification of the test report and on each page an identification in order to 

ensure that the page is recognized as a part of the test report, and a clear 

identification of the end of the test report, 

• The name and address of the client, 

• Unambiguous identification of the substance, material or product sampled, 

• The location of sampling, including any diagrams, sketches or photographs, 

• Detailed process description and process operations for each test run, 

• Identification of the method(s) used, 

• A description and unambiguous identification of the item(s) tested, 

• The date(s) of performance of the test, 

• Reference to the test plan and procedures used by Avogadro, 

• The test results with, where appropriate, the units of measurement, 

• Deviations from, additions to, exclusions from the test protocol, test methods, 

Avogadro’s quality manual, or this practice, 
 31

• Information on specific test conditions, such as environmental conditions, 

• A discussion of test results including the uncertainty associated with the test and 

discussion of possible errors or limiting conditions, 

• Calibration certificates for all equipment significant to the testing performed, 

• Documentation and sufficient raw data to verify and reproduce all report 

calculations, 

• The name(s), function(s) and signature(s) or equivalent identification of person(s) 

authorizing the test report, and 

• A signed statement by a responsible official that Avogadro operates in conformance 

with the requirements of this practice during the test project. 

Technical Coordinators, with assistance from other Avogadro personnel, prepare individual 

report components and work product intermediates. The components and work product 

intermediates are compiled into a complete draft by Air Quality Scientists. The Project 

Manager, with support from the Quality Manager or Technical Director, then performs a 

review and revision of the report. The Project Manager signs all project reports. If the work 

is subject to ASTM D 7036, then the report will also be signed by the Qualified Individual 

overseeing the project. 

Project specific quality control data including calibration data, and audit, spike, and replicate 

sample results are all reviewed by the Quality Manager using acceptance criteria established 

in test methods, regulatory agencies, or project plans. When quality control data do not meet 

established acceptance criteria, the Quality Manager must review the data, investigate the 

cause for outliers, and provide a written description of the impact on reported source data. 

The written description must be incorporated into the final report. 

Corrective actions can result in the requirement to re-issue a test report. When it is necessary 

to re-issue a test report, the original report identification number is retained and the suffix 

“Revised Day-Month-Year” is added. A Foreword is added to describe the reasons for 

revising the report. Revised data and supporting documentation are included in appropriate 

sections of the report. Other corrective actions can result in the requirement to add or append 

information to an existing test report. In these instances, appropriate correspondence and 

documentation is prepared and submitted to the client. Amended reports or data that amends 

or supplements a report will include the statement “Supplement to Test Report dated DateMonth-Year” along with a reference to the original report. Amendments, corrections, or 

replacements will conform to the requirements of this section and ASTM D 7036. 
 32

RECORDS MANAGEMENT 

Avogadro maintains project and quality system records for at least ten years from the date of 

origination. Hardcopy documents are controlled in secure areas where they are protected 

from reasonably foreseeable exposure to damage or theft. Additionally, hardcopy documents 

are scanned for electronic archival. Access to stored records is documented with “file out” 

cards and logbooks. Electronic records are backed-up daily. Weekly, the back-up drives are 

changed and are stored offsite. 

In the event Avogadro is sold, the records will be transferred to the new owner. In the event, 

Avogadro ceases business operations, appropriate arrangements will be made for either (i) 

the return of project files to clients, (ii) the proper destruction and disposal of records that 

have been retained for more than 10 years, or (iii) continued storage of records until the 10-

year period has elapsed. 

CONFIDENTIALITY 

The nature of Company work requires confidentiality to prevent the unauthorized release of 

confidential, sensitive, or proprietary business data to third parties. Avogadro does not 

release project summaries or client lists without approval from the clients. 
 33

6.0 EMISSIONS TEST REPORT 

The raw field data will be combined into spreadsheets to calculate the applicable test 

results. All field data sheets, emissions calculation spreadsheets, analytical data, 

calibration data and analyzer data summaries will be included in the final report. Test 

results will be presented in the reporting units as listed in Table 3. 

 

Avogadro will issue a draft comprehensive emissions test report to American Bituminous 

within 45 days of completion of testing. The final report will be signed by a licensed 

Certified Industrial Hygienist (CIH) or a Professional Engineer (PE) licensed in the 

Commonwealth of Pennsylvania. It will document all results of the testing program, and 

it will include all of the support data to independently calculate the test results. Other 

than the title and certification pages, the main components of the report will be as 

follows: 

1. Introduction, which includes an overview and a summary of purpose and scope; 

2. A summary and discussion of results, which includes comparison to permit standards, as 

well as a summary of test dates and times; 

3. Summary of sampling locations; 

4. Sampling / analysis procedures as well as any departures from USEPA test methods; 

5. Appendices. 

The appendices may include but are not limited to raw field data, notes, 

process/production data, laboratory reports and chains of custody, calibration certificates, 

results summaries, calculations and spreadsheets, example calculations using actual field 

data, quality assurance data, diagrams and a copy of the approved test protocol and 

related correspondence. 

Protocol submitted by: Reviewed by: 

 

 

Janeen D. Maruskanic Thomas F. Mattei 

Air Quality Scientist Quality Assurance Manager / Technical Director 

F:\2010 Projects\2010 projects\American Bituminous ICR MACT 10-7091\QAPP\final American Bituminous QAPP.doc
Attachment 1 

Example Calculations
Attachment 2 

Field Data Sheets and Chain of Custody Form
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