ARIZONA TESTING MANUAL FOR 

AIR POLLUTANT EMISSIONS 

REVISION F 

March 1992 

ARIZONA DEPARTMENT OF ENVIRONMENTAL QUALITY 

AIR QUALITY DIVISION 

3033 NORTH CENTRAL AVENU, PHOENIX, ARIZONA 85012 
A11 sections and exhibits of the Arizona 

Testing Manual for Air Pollutant 

Emissions have been updated or 

otherwise amended in this 

revision (Revision F). 
TABLE OF CONTENTS 

Section Subject Page 

1.0 Introduction 1 

1.1 Performance Test Planning and Approval 1 

1.2.1 Agency Observer Requirements 2 

1.2.2 Visible Emissions Evaluator Training 2 

and Certification 

Exhibit 1.2-1 Performance Test Plan Requirements 3 

Exhibit 1.2-2 Process and Control Equipment Operating 6 

Parameters To Be Recorded At Least Every 

30 Minutes 

1.3 Quality Assurance Provisions 7 

1.3.1 Quality Assurance Procedures 7 

1.3.2 Equipment Maintenance and Calibration 7 

1.3.3 Quality Assurance Audits 7 

1.4.1 OAQ Observer Activities 7 

1.4.2 Test Procedures 7 

1.4.3 Test Documentation and Reporting 8 

Exhibit 1.4.3-1 Performance Test Report Outline 9 

1.4.4 Test Report Review 11 

Exhibit 1.4.4-1 Compliance Test Report 12 
TABLE OF CONTENTS (CONT.) 

Section Subject Page 

2.0 Listing of Environmental Protection 13 

Agency Reference Test Methods for 

Source Emissions, 40 CFR 60, 

Appendix A, updated thru 6/30/91 

3.0 Listing of Environmental Protection 19 

Agency Performance Specification 

Test Procedures for Continuous 

Emissions Monitoring Systems: 

40 CFR 52, Appendices D& E; 

40 CFR 60, Appendix B, updated thru 

6/30/91 

4.0 Listing of Environmental Protection 21 

Agency Quality Assurance RequireMents for Gas Continuous Emissions 

Monitoring Systems Used For 

Compliance Determinations, 

40 CFR 60, Appendix F, updated thru 

6/30/91 

5.0 Listing of Environmental Protection 22 

Agency Test Methods for Hazardous 

Air Pollutant Emissions, 40 CFR 61, 

Appendix B, updated thru 6/30/91 

6.0 Listing of Environmental Protection 24 

Agency Quality Assurance Procedures 

for Testing Emissions of Hazardous 

Air Pollutants, 40 CFR 61, Appendix C, 

updated thru 6/30/91 

7.0 Arizona Emission Test Method A1 25 

> 
1.0 INTRODUCTION 

The Office Air Quality (OAQ), acting for the Director of the 

Department of Environmental Quality, is responsible for determining 

each regulated air pollution source's capability and continuing 

ability to comply with air pollution source's emission rules, adopted 

by the Director pursuant to Arizona Revised statutes §49 - 401 et 

seq.; and any terms of conditional permits issued by the Arizona Air 

Pollution Control Hearing Board. This applies to all sources under the 

jurisdiction of tkie Department in matters of air pollution control. 

Performance tests, and/or visible emissions observations by 

agency personnel, are required to assure that sources are compliant 

with all applicable emission limitations at all major emission points 

before air pollution source operating permit are issued or renewed. If 

OAQ engineering analysis and field inspection provide defensible 

assurance of compliance, these requirements may be waived. OAQ may 

also require additional performance testing at anytime during the 

permit period when lack of compliance with the applicable rules is 

demonstrated or suspected. 

1.1 PERFORMANCE TEST PLANNING AND APPROVAL 

Performance testing for regulated pollutants is required of all 

sources subject to air pollution control for verification of 

compliance with applicable Arizona rules, unless compliance can be 

assured and documented by a department engineering analysis confirmed 

by on-site inspections. 

Regulated air pollution sources shall conduct any required 

compliance verification performance testing in accordance with OAQ 

approved methods. 

All performance testing and field evaluations to determine the 

compliance status of regulated air pollution sources is subject to onsite verification by qualified OAQ representatives. Advance notice of 

performance testing shall be given to OAQ in accordance with A.A.C. 

R18-2-312.D. 

Sources subject to performance testing must also provide test 

facilities and test plans in accordance with A.A.C. R18-2-312. OAQ 

approval of test plans and any variations from approved test methods 

is required. Failure to obtain prior approval for plans and any 

variations from approved methods may result in rejection of the 

performance testing results. Requirements for performance test plans 

are outlined in Exhibit 1.2-1. 

In order to work out the logistics of each test, and to arrange 

for an OAQ observer to be present at the test, a pre-test meeting 

should be arranged with OAQ at least 14 days before testing is to 

occur. 

1 
Major sources having multiple emission points must submit 

facility test schedules assuring annual testing of major emission 

points and rotational testing of minor emissions points as required by 

permit conditions. Rotational testing of identical or essentially 

similar air pollution control devices may also be authorized through 

permit conditions. 

1.2.1 AGENCY OBSERVER REQUIREMENTS 

OAQ representatives assigned to performance test verifications 

are required to have a degree in engineering or a related air 

pollution control discipline from an accredited college, or its 

equivalent. Each OAQ observer undergoes ongoing technical training to 

assure initial and continuing proficiency. Each observer is also 

required to maintain current certification as a visible emissions 

evaluator. 

1.2.2 VISIBLE EMISSIONS EVALUATOR TRAINING AND CERTIFICATION 

Approved training in visually measuring emissions is necessary 

for proper use of EPA Reference Method 9(40 CFR 60, Appendix A). 

Opacity measurement training may be provided by OAQ, or through 

another OAQ-recognized training program. 

Certification testing will be conducted by OAQ personnel or OAQrecognized training personnel. Training course and certification costs 

for persons other than OAQ. personnel are. not the responsibility of 

ADEQ. 

Equipment utilized for visible emissions evaluator training must 

be calibrated, operated, and maintained in accordance with the 

procedures contained in EPA Reference Method 9(40 CFR 60, Appendix 

A) . 

To receive initial certification as a visible emissions 

evaluator, a candidate must successfully attend an OAQ or OAQrecognized training school on the, theory and practice of visible 

emissions evaluation, and pass the field certification test for 

measuring visible emissions within six months thereafter. 

To maintain certification, a person must retake a recognized 

training course once every two years and repass he field 

certification test once every six months. 

2 
Exhibit 1.2-1 

PERFORMANCE TEST PLAN REQUIREMENTS 

The information specified below must be submitted to the 

Compliance Unit of the Office of Air Quality at least 14 working days 

prior to the scheduled test date. This information is required in 

order to insure that proper test methods and procedures are utilized. 

The Compliance Unit will review the test plan, and in the event of any 

deficiencies or comments concerning the plan, will contact the company 

to discuss the test plan. Submittal of this information will minimize 

the possibility of a test being rejected as a result of improper 

sampling or data collection procedures. 

All testing shall be performed in strict accordance with the 

procedures, specified in an OAQ approved test plan. 

Any proposed variation in the sampling or analytical procedures 

must receive approval from OAQ Compliance prior to testing. 

Appropriate chain of custody procedures must be followed during the 

sampling and analysis. 

The following information should be included in the performance 

test plan: 

1. Source Information: 

A. Name (including serial number of equipment), address, and 

location of the facility being tested. 

B. Responsible persons at the facility and telephone number. 

2. Testing Firm Information: 

A. Name and address of the firm conducting the testing. 

B. Responsible person at the testing firm and telephone 

number. 

3. Sampling Equipment: 

A. A description of the emission sampling equipment including 

a schematic diagram of the sampling train. 

4. Procedures: 

A. Types of pollutants to be sampled. 

B. A description of the sampling and analysis procedures. 

C. Documentation for any proposed variations from OAQ approved 

procedures. 

5. Emission Point Information: 

A. A diagram of the stack showing the dimensions, and the 

configuration of the sampling location, location of 

continuous emission monitor (CEM) probes, and the distances 

to the nearest upstream and downstream flow interferences. 

3 
B. A cross-sectional sketch of the stack at the sampling 

location, showing the locations of the sampling traverse 

points. 

C. Estimated flue gas conditions at the sampling location, 

including temperature, moisture content, and velocity. 

6. Process Information: 

A. Schematic diagram identifying gas flow from origination 

point to exit point, including identification of all 

control devices, fans and bypasses. 

B. Other specific process information may be required on a 

case-by-case basis. 

7. Process Equipment: 

A. A description of the process equipment, including a process 

flow sheet. 

B. Type and quantity of raw materials, catalysts, and products 

being used or produced in the process. 

C. Maximum rated capacity of the process. 

D. Actual maximum operating of the process. 

E. Operating capacity during the previous six-month period. 

F. Process data being monitored and recorded to insure 

representative operation throtighout the test, including 

during the sampling interval. 

G. Normal process operating schedule during a 24-hour period. 

H. Normal maintenance schedule for this process. 

I. Types of fuel used in production. 

A 

8. Control Equipment: 

A. Description of emission control system, including the types 

of control equipment, manufacturer of control equipment, 

the rated capacity and efficiency of the control equipment. 

B. Data to be monitored and recorded to insure representative 

operation of the control equipment during testing and the 

sampling period for recording. 

C. Minimum acceptable values of all control devices,parameters 

such as flow rates, pressure drops, temperature, and 

voltage of electrical input. 

D. Description of any preconditioning of gases used with 

control equipment. 

E. Normal maintenance schedule on control equipment for the 

previous year. 

4 
9. Data Sheets: 

A. Copies of all field data sheets to be used during the test, 

including data sheets to record process and control 

equipment parameters. 

10., Chain of Custody: 

A. A description of the procedures that will be followed to 

maintain the integrity of the samples collected. 

B. Copies of chain of custody seals and data sheets. 

11. Quality Control: 

(The following items should be available to the OAQ observer of 

the'performance test prior to the start of the test.) 

A. Calibration sheets for the dry gas meter, pitot tube, 

nozzle, and other equipment requiring calibration. 

B. Quality assurance control charts for the analytical 

procedures to be used in the analysis of the test samples. 

C. A list of preweighted filters to be used during particulate 

emissions testing. 

A 
Exhibit 1.2-2 

PROCESS AND CONTROL OPERATING PARAMETERS 

TO BE RECORDED AT LEAST EVERY 30 MINUTES 

ASPHALT PLANTS 

Process Rate 

Recycle Rate 

Drum Temperature 

POWER PLANTS 

Generation Rate 

Coal Feed Rate 

Opacity, SOzr NOx and %CO Z or %02 from CEM's (record at least 

every 15 minutes) 

Coal Analysis 

OTHER SOURCES 

Process Rate 

Other parameters as applicable 

ESP 

Operating voltage (per field) 

Operating current (per field) 

Spark rate 

Cleaning cycle 

Fan current or speed 

SCRUBBER 

Pressur.e drop 

Water flow rate 

Water supply pressure 

Fan speed or current 

Other parameters such as pH values, as applicable 

BAGHOUSE 

Pressure drop (total) 

Pressure drop (each compartment) 

Number, type, and temperature range of bags 

Damper position 

Fan current or speed 

Cleaning cycle 

C? 
1.3 QUALITY ASSURANCE PROVISIONS 

1.3.1 QUALITY ASSURANCE PROCEDURES 

The applicable procedures contained in the Quality Assurance 

Handbook for Air Pollution Measurement Systems, Volume III - 

Stationary Source Specific Methods, incorporated herein by reference, 

shall be used. 

1.3.2. EQUIPMENT MAINTENANCE AND CALIBRATION 

Performance test equipment, including instrumentation, must be 

maintained in accordance with manufacturers' instructions- and good 

engineering practice. Instrumentation for measurement of pertinent 

physical parameters shall be currently calibrated with traceability to 

documented reference standards or procedures.. Verification of such 

maintenance and calibration must be documented in each test record. 

Performance of all calibration and control checks required by the 

approved test methods must be documented. 

1.3.3. QUALITY ASSURANCE AUDITS 

Audits of the sampling equipment and of the analytical techniques 

used may be required at any time during performance testing. The OAQ 

may use the results of such audits to determine the acceptability of 

test results. 

1.4..1. OAQ OBSERVER ACTIVITIES 

OAQ personnel are assigned to observe all performance testing 

activities. Observation of laboratory analysis may also be performed. 

Visible emissions observations are recorded by the observer at 

appropriate times during performance testing. A summary of the field 

observations is documented. 

1.4.2. TEST PROCEDURES 

The procedures used during performance tests and subsequent 

sample analysis shall conform to that .agreed upon in an approved test 

plan and/or at a pre-test meeting. When.necessary, the OAQ observer 

may authorize minor modifications to agreed procedures at the time of 

the test. 

The number of test runs required shall be in accordance with 

A.A.C. R18-2-312.F. 

7' 
1.4.3. TEST DOCUMENTATION AND REPORTING 

The OAQ observer may initial field data sheets, and may require 

that copies be provided on-site. Preliminary results may be required 

to be furnished on-site if feasible, or by telephone within three days 

of completion of the testing. The final test report shall be 

submitted to the OAQ within four weeks after the completion of 

testing. The test report will contain, at a minimum, the information 

listed in Exhibit 1.4.3-1. All pages of the report must be numbered to 

maximize it usefulness. All test samples must be maintained and be 

available to OAQ upon request for a period of one year after testing. 

A complete copy of all test records shall be retained by the source 

for a minimum period of three (3) years. This record shall include 

all applicable documents noted in this manual. 

8 
Exhibit 1.4.3-1 

PERFORMANCE TEST REPORT OUTLINE 

GENERAL 

1. Plant name and location. 

2. Source sampled. 

3. Testing company or agency, name and address. 

CERTIFICATION 

1. Certification by team leader. 

2. Certification by reviewer (e.g., P.E.). 

TABLES OF CONTENTS (Include page numbers) 

INTRODUCTION 

1. Test purpose. 

2. Test location, type of process. 

3. Test dates. 

4. Pollutants tested. 

5. Observers' names (source and 9A9 AQD). 

6. Any other important background information. 

SUMMARY OF RESULTS 

1. Emission results. 

2. Process data. 

3. A1lowable emissions. 

4. Discussion of errors, both real and apparent. 

SOURCE OPERATION 

1. Description of source and control devises. 

2. Process and control equipment diagram. 

3. Process and control equipment data. 

4. Representativeness of materials and operation. 

5. Demonstration of any specially-required operation. 

SAMPLING AND ANALYSIS PROCEDURES 

1. Sampling port location and cross-section with dimensions. 

2.. Sampling port description, including labeling system. 

3. Sampling train description. 

4. Description of sampling procedures, and any deviations from 

standard procedures . 

5. Description of analytical procedures, and any deviations from 

standard procedures. 

9 
Exhibit 1.4.3-1 (Cont.) 

APPENDICES 

1. Complete results with example calculations. 

2. Copies of original field and laboratory data sheets. 

3. Copies of original production data signed by plant official. 

4. Test log. 

5. Calibration procedures and results. _ 

6. Project participants and titles. 

7. Related correspondence. 

F4i7 
1.4.4. TEST REPORT REVIEW 

Upon the submittal of the final test report, the report is 

checked for completion, and the results are checked for accuracy and 

compliance with the applicable emission limits. The results of this 

review is documented on Exhibit 1.4.4-1. 

The source will be notified of the results of the review and any 

additional information or testing that may be required. 

11 
Exhibit 1.4.4-1 

ARIZONA DEPARTMENT OF ENVIRONMENTAL QUALITY 

OFFICE OF AIR QUALITY 

COMPLIANCE TEST REPORT 

Name of Company County 

Source Tested 

Person Submitting Test Report 

Date(s) of Test(s) 

Circle One: PASS FAIL Process Rate 

Plant Emission Rates 

Maximum Allowable Emission Rate 

Review of Test Method 

Review of Test Calculations 

Report Demonstrates Compliance with Applicable Emission Standards 

Reviewer Date 

Comments (Precision and accuracy of replicate tests, percent 

isokinetic sampling, operating anonmalies): 

cc: _ Source Permit File 

Permit Engineer 

Source 

12 
SECTION 7.0 

A1. ARIZONA EMISSION TEST METHOD A1 

Determination of Particulate Emissions from Stationary 

Sources in the Presence of Sulfuric Acid Mist and Sulfur 

Oxides 

A1.1 Principle 

Particulate matter is withdrawn isokinetically from 

the source and collected on a glass fiber filter. The 

temperature of the probe and filte'r is maintained 

above the dewpoint of water and sulfuric acid mist. 

The solid particulate mass is determined 

gravimetrically after removal of water and sulfuric 

acid by solvent extraction with acetone-heptane. 

A1.1.1 Sulfuric acid mist, sulfur trioxide, and arsenic are 

collected in an impinger train, and the amount 

determined by chemical analysis. The sulfuric acid 

mist in the solvent extract is also determined by 

chemical analysis. Sulfur dioxide is oxidized and 

collected in the impinger train. 

A1.2 Applicability 

The method is applicable for the determination of 

solid particulate emissions as well as condensible 

sulfates from stationary sources where the emissions 

contain high levels of sulfuric acid mist and sulfur 

oxides. 

A1.3 Apparatus and Reagents 

The basic sampling train is the same as for EPA Method 

5 described in APTO-0581, "Construction Details of 

Isokinetic Source Sampling Equipment." Commercial 

models of this sample train are available or can be 

fabricated. (See Figure 1 for train used.) The sample 

train is modified to include five impingers and a 

filter between the first and second impingers. The 

filterbox is capable of being heated to 350 ° F 

(177 0 C).All surfaces in contact with the gases are of 

a chemically inert material with the exception of the 

probe nozzle. 

A1.3.1 Nozzle - Stainless steel with a sharp, tapered edge. 

The tip diameter should be carefully measured. 

(Chemically inert material construction is 

permissible.) 

25 
A1.3.2 Probe - Constructed to include an S-type pitot tube tc 

measure stack gas velocity and a thermocouple to 

measure temperature. The liner should be chemically 

inert and be capable of being heated to 350?F (177 0 C). 

A Teflon liner may be used at stack gas temperatures 

lower than 500 ° F (260 0 C). 

A1.3.3 Filter - The filter holder is constructed of inert 

material capable of supporting a glass fiber filter 

not less than four inches in diameter and'capable of 

being heated to 350 ° F (177 0 C). 

A1.3.4 Impingers - Impingers shall be standard and modified 

Greenburg-Smith designs or equivalent. They shall be 

connected by leak-free fittings. The first and third 

impingers are standard design; the second, fourth and 

fifth are modified. 

A1.3.5 Method 8 Filter - The filter holder is constructed of 

glass or other inert material capable of supporting a 

two inch diameter or larger glass fiber filter. 

A1.3.6 Gas Mover - A leak-free pump capable of moving at 

least one cubic foot per minute at 15" mercury vacuum; 

A1.3.7 Metering System - The system shall, consist of a 

vacuum guage capable of inea.suring to 30" of inercury, 

a dry gas meter with an accuracy of ± 1% and . 

thermometers or equivalent capable of ineasuring the 

temperatures of the inlet and outlet of the dry gas 

meter and the impinger outlet within 9 ° F (5 0 C). 

A1.3.8 Sample Recovery Equipment -The equipment should 

include laboratory glassware, an analytical balance to 

measure f 0.1 mg, a balance to measure ±.1 gram, a pH 

meter and an atomic absorption spectrophotometer (AA) 

or other apparatus and procedures capable of ineasuring 

iron, copper, and zinc to 0.2 ppm and arsenic to 5.0 

ppm. 

A1.3.9 Filters - 31ass fiber filters made without an organic 

binder and having a retention efficiency of 99.95% for 

0.3 micron particles. 

A1.3.10 Silica Gel - The silica gel shall be an indicating 

type, 6-16 mesh. If the silica gel has been used 

previously it should be dried at 350?F (177?C) for two 

hours. 

A1.3.11 Water - The water should be deionized or distilled to 

conform to ASTM specification D 1193-72 Type 3. 

26 
A1.3.12 Isopropanol 80% - This reagent is prepared by mixing 

800 ml reagent grade isopropanol with 200 ml of 

deionized water. 

A1.3.13 Thorin Indicator - This indicator solution is•prepared 

by dissolving 0.2 g of 1-(0-arsonophenylazo)-2- 

napthol-3, 6 disulfonic acid disodium salt in 100 ml 

of deionized or distilled water. 

A1.3.14 Perchloric Acid 25% - This reagent is prepared by 

adding 25 ml of reagent grade perchloric acid (HC109 ) 

to 75 ml of deionized or distilled water. 

A1.3.15 Barim Perchlorate (0.01N), - This titrant is prepared 

by dlssolving 1.95 g of barium perchlorate trihydrate 

(BaC10 4 . 3H2O) in 200 ml of deionized or distilled 

water and diluting to 1 liter with isopropanol. The pH 

of the solution is adjusted to 2.5-4.0 with 25% 

perchloric acid solution. It is then standardized with 

sulfuric acid of known concentration. 

A1.3.16 Normal Sodium Hydroxide - An approximately one normal 

sodium hydroxide solution is prepared and standardized 

against a primary standard. 

A1.4 Procedure 

A1.4.1 Preparation 

All sampling train components shall be maintained and 

calibrated according to procedures_described in APTD 

0576, "Maintenance, Calibration, and Operation of 

Isokinetic Source Sampling Equipment", unless 

otherwise specified herein. 

A1.4.1.1 Check all filters visually against a light for 

irregularities and flaws or pinhole leaks. Label a 

glass fiber filter or its container and desiccate for 

at least twenty-four hours at 68. ± 10 ° F (20 0 ± 5.6 ° C) 

and ambient pressure. Weigh the filter or both the 

filter and container to the nearest 0.1 mg. If both 

the filter and container are weighed, the container 

must be weighed separately to determine the filter's 

exact weight. Carefully place filter in filter holder 

after weighing and seal the holder to prevent 

contamination. 

A1.4.1.2 Weigh approximately 200 grams of silica gel to the 

nearest gram, place in the fifth impinger and seal. 

Place 200 ml of 80% isopropanol in the first impinger. 

27 
The second impinger is empty. Place 150 ml of 10% 

hydrogen peroxide in each of the third and fourth 

impingers. Weigh each of the five impingers to the 

nearest 0.1 g and record the weights. Seal probe, 

filter holder and all impingers to prevent 

contamination. 

A1.4.2 Preliminary Determinations 

Select the sampling site and the minimum number of 

sampling points according to EPA Method 1, 40 CFR 60, 

or as specified by the Director of ADEQ. Determine 

the stack pressure, temperature, and the range of 

velocity heads according to EPA Method 2, and moisture 

content according to Approximation Method 4 or its 

alternatives for the purpose of making isokinetic 

sampling rate calculations. Molecular weight of the 

carrier gas is determined by analyzing at least three 

"grab samples" with an Orsat analyzer during the 

sampling period. An alternative method may be approved 

by the Director. The samples are taken with a 

glass-wool packed tube extending far enough into the 

stack to get a representative sample. The gas samples 

are withdrawn from the stack with a one way aspirator 

bulb. The sampled gas is pumped into the Orsat 

apparatus and through the leveling fluid in the 

measuring burettes to saturate it with the gas to be 

analyzed. 

A1.4.2.1 This Orsat apparatus is a commercially available 

instrument with three or more absorption burettes of 

the contact type. The apparatus is modified to analyze 

for sulfur dioxide, carbon dioxide, and oxygen. 

A1.4.2.1.1 The sulfur dioxide absorbent is iodine-iodide solution 

that is made by dissolving 12.7 g of iodine and 83 g 

of potassium iodide in a liter of water. The carbon 

dioxide absorbent is aqueous 35% potassium hydroxide 

solution above. The oxygen absorbent is 5% pyrogallic 

acid in aqueous 35% potassium hydroxide. Gas 

absorbents which are commercially available may be 

substituted for the above. 

A1.4.2.2 Leak check the apparatus by bringing the level in each 

absorption pipette up to the reference mark and 

closing the pipette stop-cock. In four minutes time 

the liquid level in the pipettes must not fall below 

the capillary. Adjust the level of the confining fluid 

28 
to the graduated portion ofthe rneasuring burette, 

lower,the leveling bulb and take a reading. The level 

of the meniscus should not fall more than 0.2 ml in 

four minutes. 

A1.4.2.3 Draw the sample into the measuring burette after 

saturating the confining fluid with stack gas. Adjust 

to atmospheric pressure with a leveling bulb. Begin 

analysis by passing the sample gas several times 

through the sulfur dioxide absorbent. Take a reading, 

make one more pass and take,another reading. Repeat 

the above procedure if necessary for a constant 

reading. Use the same procedure for carbon dioxide and 

for oxygen. This procedure assumes the carbon'monoxide 

content of the gas to be negligible. The nitrogen 

percent is calculated by adding the percent of sulfur 

dioxide, carbon dioxide, and oxygen then subtracting 

from 1000. 

A1.4.2.4 Calculate the dry molecular.weight of the gas using 

the following formula: 

Md = 0.64 (%S0 2 ) + 0.44 (%CO Z ) + 0.32 (%OZ ) + 0.28 (%N 2 ) 

Estimates may be used for prelirninary calculation of 

the isokinetic flow rate; however, final results will 

be calculated on actual measurements made by Orsat 

analyses during the test. 

A1.4.2.5 Select a nozzle size based on the range of velocity 

heads, such that it is not necessary to change the 

nozzle size in order to maintain isokinetic sampling 

rates. It is recommended that the nozzle size not be 

changed during sampling. 

A1.4.3 Sample Site Preparation 

During preparation and assembly of the sampling train, 

keep all openings where contamination can occur 

covered until just prior to assembly or until sampling 

is about to begin. Mark the probe with heat resistant 

tape or by some other method to denote the sample 

traverse points as calculated by Method 1 during the 

preliminary determinations. 

A1.4.3.1 Set up the train as shown in Figure 1 using, if 

required, a very light coat of silicone grease on all 

ground glass joints, greasing only the outer portion 

to avoid the possibility of contamination by the 

silicone grease. (See APTD-0576.) 

A1.4.3.2 After assembling the sample train at the test site, 

29 
seal the inlet to the filter holder, start the pump 

and carefully bring the vacuum to 15 inches of 

mercury. A leakage rate of 0.02 cfm or less is 

satisfactory. Close the coarse control valve and 

release the vacuum carefully before turning pump off 

to avoid transfer of impinger contents. Attach the 

probe, seal the inlet to the probe, and again leak 

check the system with a vacuum of 1 inch mercury using 

the above procedure. 

A1.4.3.3 Turn on probe and filter oven heaters and bring to a 

temperature of 325 ± 25 ° F (163 ± 15 0 C). During this 

period, add crushed ice to the impiriger box and 

continue to add ice as needed after sampling has 

started to maintain the impinger gas at 70 ° F (21 0 C). 

Also clean the-portholes prior to inserting the probe 

to avoid sample contamination with deposited material. 

A1.4.4 Sampling 

When the temperatures of the probe and filter oven 

have reached the set point of 325 ° F (163 0 C), place the 

probe inlet at the first sampling point. When the 

probe is in position, block off the openings around 

the probe and porthole to prevent dilution of the' gas 

stream. Begin sampling and record the required data 

as shown on the example sheet at least every five 

minutes. (See Figure 2.) Maintain sampling rate to 

within ten percent of isokinetic by adjusting the flow 

rate as necessary. Nomographs are avaliable for 

sampling trains using S-type pitot tubes with 0.85 ± 

0.02 coefficient and when sampling stack gases of a 

molecular weight of 29 ± 4, which aid in the rapid 

adjustment of the sampling rate. 

A1.4.4.1 During the sampling, continue to check the probe and 

filter oven temperatures and the outlet temperature of 

the impingers. It is recommended that a leak check be 

conducted at each port change at the highest vacuum 

reading reached during that sampling traverse. 

A1.4.4.1.1 If_the pressure drop across the filter becomes too 

high to maintain an isokinetic sampling rate, the 

filter may be replaced during the run: It is 

recommended that a complete filter and filter, holder 

be used rather than changing the filter itself. A leak 

30 
check is then performed at 15 inches mercury as 

previously described. The particulate weight will 

include the summation of weight gains of all filters 

used in sampling. 

A1.4.4.2 After sampling has been completed and the minimum 

volume to provide a representative sample as specified 

by the Director has been reached, remove the probe 

from the flue, and record the dr.y gas meter reading. 

Again, leak check the system by plugging the inlet to 

the filter holder and pulling a vacuum equal to the 

highest vacuum recorded.during the sample traverse. 

A1.4.4.2.1 After the leak check, drain the icebath and begin 

purging the impingers by drawing clean ambient air 

through the inlet of the first impinger for 

approximately'fifteen minutes at the sample rate. A 

charcoal filter may be used if necessary to ensure 

that clean air is being drawn. 

A1.4.5 Sample Recovery 

Remove the sample train from the test site after the 

purge has been completed and the probe and filter oven 

have cooled. Insure that.all probe, filter holder, and 

impinger openings are sealed to prevent contaminatlon 

or loss of a sample during transit. 

A1.4.5.1 Disassemble the filter holder in a clean place. The 

filter holder and any glassware connecting the probe 

to the holder should be washed with 3:1 v/v 

acetone-heptane solution into a clean, dry container 

to collect the particulate. The filter also should be 

placed in t$is container. The probe and nozzle should 

be washed with the acetone-heptane solution using a 

nylon bristle brush into the container used for the 

filter. The container should be capped to prevent 

contamination. Typically, 100-200 ml of 

acetone-heptane mixture are used for particulate 

transfer. 

A1.4.5.2. The impingers are weighed to determine the net weight 

gain of the sample train for the rnoisture content of 

the sampled gas. The weight of the sulfur dioxide 

collected is determined by titration (A1.4.6.1.) and 

subtracted from the weight gain (Equation 4) of the 

impingers before calculating the volume of water vapor 

collected. The first and second impingers are then 

rinsed into a clean container with water, along with 

M 
the wash of the Method a filter and filter holder. 

The Method a filter is transferred into the container. 

Any connecting glassware or tubing between the 

particulate filter holder and first impinger is also 

washed into the container. The third and fourth 

impingers and connectors are washed into a clean 

volumetric flask with deionized or distilled water. 

A1.4.6 Analysis 

Transfer the solutions from the first two impingers 

and Method a filter into a volumetric flask and dilute 

to the mark with deionized or distilled water. Pipette 

a 10 ml aliquot into a vessel for titration and 

evaporate on a hot plate to about 3 ml to remove any 

residual sulfur dioxide. Rinse the sides of the 

container with a minimum amount of water, cool, then 

add I isopropanol to make the solution 70-900 

isopropanol. Add 2-4 drops of thorin indicator and 

titrate to the pink endpoint using 0.01 N barium 

perchlorate. Repeat, adjusting the size of the 

aliquots to obtain two accurate determinations. 

Prepare a blank by putting a same-size aliquot of 

distilled water through the above procedure. The blank 

and sample requiring 2.5 -3.0 ml titrant must be 

acidified with 1 to 2 drops of 25% perchloric acid 

before titration, so that the endpoint will be 

distinct. Save the contents of the volumetric flask 

for arsenic analysis by atomic absorption or other 

approved method. The arsenic determined is calculated 

as arsenous oxide and add to Mn used in equation Nos. 

8 and 9 to calculate the total particulate 

concentration. 

A1.4.6.1 Dilute the contents of the volumetric flask containing 

the solutions from the peroxide impingers to the mark 

with deionized or distilled water. Withdraw a 10 to 25 

ml aliquot and titrate to pH7 using standard sodium 

hydroxide. Repeat, adjusting the size of the aliquots 

to obtain two replicate determinations. 

A1.4.6.2 A fine grade fiberglass filter (2.1cm) is placed in a 

.Gooch crucible (Size No.3) seated in a crucible 

holder, which in turn is inserted into a filter flask. 

Vacuum is applied and deionized or distilled water is 

passed through the filter until it is well seated to 

32 
the crucible. Allow the excess water to be apirated. 

Dry the crucible in an oven at 105 ° C for at least 1 

hour, cool in a dessicator, and weigh t'o the nearest 

0.1 mg. 

A1.4.6.3 Break apart the particulates filter (irx,3:. 1 acetoneheptane) into very fine pieces using the glass rods. 

Check that the filter in the pre-weighed Gooch 

filtration crucible is properly set. ;Usi,ng vacuum _ 

assist, filter and resulting slurry through.the tared 

crucible using additonal anhydrous 3;1 acetone-heptane 

and a rubber policeman (or other means) to assure 

quantitative transfer. 

A1.4.6.3.1 Rinse the contents of the crucible several ;times witYi 

10 ml portions of 3:1 acetone-heptane. Dry the ` 

crucible for 3 hours at 105 0 c, cool in a dessicato:r, 

and weigh to the nearest 0.1 mg. The'weight`'difference 

after subtracting the filter tare is;the , so:lid 

particulate weight. 

A1.4.6.4 Transfer the filtrate from the above ~ procedure to an _ _. 

appropriate container for evaporation of the acetoneheptane solvent. Also prepare a blank for analysis 

from 200 ml of 3:1 acetone-heptane. 7f`a rotary 

evaporator is used, 50 ml of water i's-°added and the - 

organic solvent removed in a vacuum :using a hot waterbath. If a steam plate is used, the ~s.olvent._.is 

evaporated in a fume hood with occasional additions of _ . . _ , , ... .- . _.. 

water to avoid heating the sample to:. dryness. . _ 

Evaporation of solvent on a hotplate in afume hood is 

not recommended, however, it can be used"if, extreme 

care is exercised to avoid overheatiiig 'and 'loss of -° -- 

sulfuric acid. Transfer the residual- solution to 100-- -- 

ml volumetric flask and make-up to mark.with-water. _ 

Titrate two 25 ml aliquots with 0.1 N..so.dium._hydroxide 

to the phenolphthalein endpoint. Analyze the . ._ _ 

remainder of the solution and the solution,from the 

first impingers for elements known to be present in 

the emissions in substantial quantities (as specif'ied 

by the Director). Atomic absorption analysis in an 

air-acetylene flame or an equivalent method is 

acceptable. 

For AA analysis, background correction should be used 

or blanks and standards should be prepared in the 

proper sulfuric acid matrix. Blank values are 

subtracted from the determinations and the resulting 

concentrations are calculated as molecular 

33 
species likely to have been collected (as specified by 

the Director)...The elemental contents are expressed as 

the hydrated sulfates and.arsenic is expressed as 

arsenous oxide. (Fe2 S09 • H2O. Znz SO g• CuS09 and 

As 203 ).. Alternate equivalent-methods of analysis may be 

approved by the Director. The weights of these 

compounds ar.p added.to:(Mn) -which is used in Equation 

Nos.'8.and 9 to calculate the particulate 

concentration. 

34 
,. ocli 

W. 

V"j 

CC 

35 




PLANT 

RUN NO. 

DATE 

OPERATOR 

CONTROL BOX NO. 

DGM CORR. FACTOR 

?H(; 

PITOT COEFF'ICIENT Ce 

ORSAT ANALYSIS 

RUN SOZ COZ OZ TIME 

15T 

.Z ND 

3 ftD 

AVG. 

AMBIENT TEMP., ° F 

BAR. PRESS., in HG 

ASSUMED MOISTURE, $ 

PROBE TIP DIAM. , 

STACK DIAM. (ft.) _ 

STATICE PRESS. (in 

LEAK RATE @ in HG cfm 

START/END TSNE _ 

TRA 

VERSE 

POINT 

SAMPLING 

TIME 

(Omin>) 

GAS 

SAMPLE 

VOL.UME 

(V,o ft') 

VELOCITY 

HEAD 

 (?linH_0) 

ORSFICEMETER 

(? 3 inH20) 

DGM TEMP 

Tc( ° F) 

VACUUM 

(mHo) 

FILTBR 

13r . 

(TEMP ° F) 

IMPINGER 

OUTLET 

TEMP( ° F). 

STACK 

TEMP 

DESIRED ACTUAL INLET OUTLET Tc( ° I`) 

FIGURE 2 

9E.