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Test Plan for Environmental Protection Agency (EPA) 

Information Collection Request (ICR) 

Prepared for: 

Shintech Louisiana LLC 

Test Scheduled for: 

August, 2014 

Test Location: 

Plaquemine Plant 

Plaquemine, Louisiana 

LDEQ Permit No. 1280-00118-V4 

Prepared by: 

Weston Solutions, Inc. 

Integrated Air Services 

5599 San Felipe, Suite 700 

Houston, TX 77056

24 July 2014 

Valid through November 2014 

This test plan has been prepared by Weston Solutions, Inc. (WESTON) for the exclusive use of 

Shintech Louisiana LLC (Shintech) and affiliated companies, and WESTON. WESTON recognizes 

that a copy of this protocol may become public record under EPA authority. 

This document may be shared with regulatory agencies having jurisdiction over the tested source. 

Otherwise, this document may not be released to, or used by others, without the advance written 

approval of WESTON.
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Section Page No. 

1. INTRODUCTION.................................................................................................... 5

2. OBJECTIVE AND SUMMARY OF THE EMISSION TEST PROGRAM ...... 5

3. SOURCE DESCRIPTION AND OPERATING CONDITIONS ........................ 7

3.1. Facility Overview....................................................................................................................7

3.2. PVC Unit and Supporting Facilities ........................................................................................8

3.3. VCM Unit................................................................................................................................9

3.4. Control Devices....................................................................................................................10

4. TEST MATRIX & SAMPLING LOCATIONS .................................................. 11

5. TEST METHODS .................................................................................................. 13

6. PROCESS DATA REQUIREMENTS ................................................................. 19

7. QUALITY CONTROL PROCEDURES AND AUDITS ................................... 19

8. REPORTING FORMAT AND REPORTING UNITS ...................................... 20

9. PLANT DIRECTIONS, ENTRY, & SAFETY REQUIREMENTS .................. 23

10. TEST PROGRAM PERSONNEL & RESPONSIBILITIES ............................. 24

11. TEST PROGRAM SCHEDULE .......................................................................... 26

12. SOURCE TESTING METHODOLOGY ............................................................ 26

12.1. Volumetric Flow Rate...........................................................................................................26

12.2 Oxygen/Carbon Dioxide (Instrumental)...............................................................................27

12.3 Hydrogen Chloride (Table 1.1 Compound List)....................................................................28

12.4 Formaldehyde, Methanol and Ethylene Glycol (Table 1.5 Compound List)........................30

12.5 Semivolatile Organic Compounds (Table 1.4 Compound List, Site Specific HAP)...............34

12.6          Total Hydrocarbon Concentrations (Table 1.1 Compound List, 30‐Day Monitoring).........39

12.7 Volatile Organic Compounds (SW846 Method 0031) (Table 1.3 Compound List) ...............42

12.8 Speciated HAP – Direct Interface (Table 1.1 Compound List, Site Specific HAP).................46

13. LABORATORY SAMPLE SUMMARY ............................................................. 50

14. VOST DETECTION LIMITS .............................................................................. 52

APPENDIX A - EPA ICR LETTER – MAY 15, 2014 .................................................................. 56
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APPENDIX B - JULY 14, 2014 EPA EMAIL REGARDING PCB TESTING ..................... 60

APPENDIX C - ENCLOSURE 1, ATTACHMENT B AND C .................................................... 66

List of Tables and Figures 

Table 2-1 Initial ICR Test Program ..................................................................................... 6

Table 2-2 Thirty Day THC Monitoring Program ............................................................... 7

Table 4-1 Test Matrix & Sampling Locations, Shintech SCR Inlet ................................ 11

Table 4-2 Test Matrix & Sampling Locations, Shintech GTO Scrubber Stack ............ 12 

Table 5-1 Enclosure 1 Attachment B Table Summary - Methodology ........................... 13

Table 5-2 Initial ICR Test Program – GTO Scrubber Stack Location .......................... 14

Table 5-3 Total Hydrocarbon 30-Day Test Program – GTO Scrubber Stack ............... 16

Table 5-4 Total Hydrocarbon 30-Day Test Program – SCR Control Device Inlet ........ 17

Table 5-5 Detection Limits .................................................................................................. 18

Table 8-1 Anticipated Organization for Shintech ICR Report ....................................... 21

Table 8-2 Anticipated Organization for Shintech ICR 30-Day THC Monitoring Rep . 22

Table 10-1 Test Program Personnel & Responsibilities ................................................... 24

Table 10-2 Shintech Contacts ............................................................................................. 24

Table 10-3 Analytical Support Contacts ............................................................................ 25

Table 11-1 Planned Test Schedule ...................................................................................... 26

Figure 12-3-1 EPA Method 26A Sampling Train ............................................................. 29 

Figure 12-4-1 EPA Method 316 Sampling Train .............................................................. 32 

Figure 12-5-1 EPA Method 0010 Sampling Train ............................................................ 35 

Figure 12-5-2 Sample Recovery Procedures for Method 0010 Sampling Trains .......... 36 

Table 12-5-1 Method 0010 Reagent Blank Samples ......................................................... 37 

Table 12-5-2 Organic Glassware Cleaning Procedure ..................................................... 38

Figure 12-6-1 EPA M25A Samling Configuration ............................................................ 41 

Figure 12-7-1 EPA Method 0031 Volatile Organic Sampling Train (VOST) ................ 43

Figure 12-8-1 EPA Method 18 Sampling Configuration .................................................. 48

Table 13-1 Sample Collection Summary ...................................................................... 50 
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List of Acronyms 

C2H6 ................................................................................................................................. Ethane 

CH4 ............................................................................................................................... Methane 

DSCM ............................................................................................ Dry Standard Cubic Meter 

EDC ........................................................................................................... Ethylene Dichloride

EPA .................................................................................... Environmental Protection Agency

FID .................................................................................................. Flame Ionization Detector 

GC ......................................................................................................... Gas Chromatography 

GPC .................................................................................... Gel Permeation Chromatography 

GTO ....................................................................................................... Gas Thermal Oxidizer

HAPs ................................................................................................. Hazardous Air Pollutants

HCl ............................................................................................................. Hydrogen Chloride 

ICR ........................................................................................ Information Collection Request 

MDL ............................................................................................... Minumum Detection Limit 

MACT .................................................................. Maximum Achievable Control Technology 

NMNE ........................................................................................... Non-Methane / Non-Ethane 

O2 ................................................................................................................................. Oxygen 

PCBs ................................................................................................ Polychorinated Byphenyls 

RDL ................................................................................................ Reporting Detection Limit

SCR ............................................................................................ Selective Catalytic Reduction

TBD ............................................................................................................... To Be Determined 

THC ........................................................................................................... Total Hydrocarbons 

VOC ........................................................................................... Volatile Organic Compounds

 
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1. Introduction 

Weston Solutions, Inc. (WESTON®) has been retained by Shintech Louisiana LLC (Shintech) to conduct 

emission testing at its Plaquemine facility in Plaquemine, Louisiana. This test program has been initiated in 

response to a letter dated May 15, 2014 from the EPA in regards to an ICR for PVC manufacturing facilities. 

This test plan has been prepared at the request Shintech and has been formatted to clearly and efficiently satisfy 

the requirements set forth in Section 12.3 of ASTM D7036-04, Standard Practice for Competence of Air 

Emission Testing Bodies. WESTON certifies that at the date of this transmittal it operates in conformance with 

ASTM D7036-04 standard and is accredited by the Louisiana Environmental Laboratory Accreditation 

Program (LELAP) effective December 2001 and valid through 30 June 2015. 

The technical approach described in this test plan is valid for 120 days from the revision date. Note that 

regulations and test methods are always evolving. Should regulations or test methods affecting this test 

program change within the period of test plan validity, WESTON will advise Shintech. 

The project schedule described in this test plan is valid through November 2014. WESTON will confirm or 

update the project schedule via email. A formally revised and reissued test plan will not be provided unless 

specifically requested and authorized. 

The compounds of interest for the ICR are outlined in the May 15, 2014 letter received by Shintech from the 

EPA. The letter includes six enclosures, with “Enclosure 1” consisting of the document “Maximum 

Achievable Control Technology (MACT) Standards Development Information Collection Request” with 

tables 1.1 through 1.6 outlining compounds of interest as well as describing test methodologies and reporting 

requirements. WESTON will use the services of two analytical laboratories to collect and/or analyze the 

samples as outlined in the ICR request. 

WESTON’s contract laboratory will be Enthalpy Analytical, Inc. (Enthalpy) for the compounds of interest 

identified in Table 1.1, 1.4, 1.5, and site specific HAP compounds, as identified and labeled in the PVC ICR 

collection request and subsequent May 14, 2014 letter from the EPA to Shintech. Enthalpy is accredited by 

the NELAC institute. 

WESTON’s contract laboratory will be Maxxam Analytics Inc. (Maxxam) for the compounds of interest 

identified in Table 1.3 of the ICR request. Maxxam is accredited by the NELAC institute. 

Shintech considered the addition of PCBs to the list of site specific HAP as it was previous detected under a 

previous 114D request. Shintech, via the Vinyl Institute, made an inquiry to US EPA (Jodi Howard)if testing 

of this compound was necessary. US EPA responded that testing for PCB was not necessary and, as a result, 

is not included as parameter as part of this test plan. See Appendix B for the e-mail correspondence regarding 

this issue. 

2. Objective and Summary of the Emission Test Program 

The ICR request for PVC manufacturing facilities consists of two distinct testing programs. One program 

consists of performing three test runs for various compounds as outlined in Tables 1.1-1.5 of the ICR request. 

The second program is outlined in Table 1.6 of the document, and consists of performing thirty-days of 

continual monitoring for oxygen, moisture, total hydrocarbons and methane. Ethane measurements will also be 
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performed during the thirty-day monitoring period to more accurately determine non-methane / non-ethane 

(NMNE) hydrocarbons although ethane measurements are not a requirement of the ICR request.

Initial ICR Compliance Test Program 

The emission testing program will be conducted to comply with the EPA ICR request as outlined in the May 

15, 2014 letter sent to Shintech from the EPA. The test program will involve the measurement of volumetric 

flow, gas composition, and select HAPs using EPA Methods 1, 2, 3A, 4, 25A, 26A, 316 (modified), SW-846 

Methods 0010, and 0031. Three test runs will be performed for all parameters. 

Table 2-1 Initial ICR Test Program 

Reference Method/Parameter 

Process Location 

GTO Scrubber Stack 

Flowrate X 

Moisture X 

Gas Composition (M3A) X 

Hydrogen Chloride X 

Total Hydrocarbons X 

Methane X 

Ethane X 

Speciated HAP X 

Total Hydrocarbon 30-Day Monitoring Test Program 

As per the instructions found in the EPA letter, the “Total Hydrocarbon 30-Day Monitoring Test Program”, as 

described in the next paragraph, will be initiated before the start of the initial ICR compliance test program and 

data will be collected concurrently with the main ICR test program. Table 2-1 summarizes the initial ICR test 

parameters. 

Total hydrocarbons (THC), methane (CH4), oxygen (O2), and moisture will be monitored and recorded for 

thirty consecutive days as outlined in Table 1.6 of the ICR Enclosure 1, Attachment B. Although not required 

by the ICR, ethane (C2H6) will also be recorded. Due to the unique configuration of the process at the 

Plaquemine facility, the monitoring will be performed at two locations. The scrubber stack will be monitored 

at the outlet to the stack. Additionally, the inlet to the SCR will be monitored to provide a baseline reading of 

THC, methane and ethane before the selective catalytic reduction (SCR) process. Due to the temperature 

requirements of the SCR, the gas stream entering the device must be heated by natural gas burners. It is 

anticipated that the THC levels at the stack location may be biased high due to this heating process. Table 2-2 

summarizes the thirty day THC monitoring program test parameters. 

 
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Table 2-2 Thirty Day THC Monitoring Program 

Reference Method/Parameter 

Process Location 

Inlet to SCR GTO Scrubber Stack 

Total Hydrocarbons X X 

Methane X X 

Ethane(1) X X 

Oxygen X X 

Moisture (Method 4, Once per Day) X 

Moisture (Saturation Temperature, Once per Day) X 

1

 Ethane measurements are for engineering purposes and are not a requirement of the ICR program 

3. Source Description and Operating Conditions 

3.1. Facility Overview 

Shintech Louisiana, LLC (Shintech), a wholly owned subsidiary of C-K Tech, Inc., is currently operating the 

Shintech Plaquemine Plant 1 (SPP-1) on the west bank of the Mississippi River near Plaquemine, Louisiana in 

Iberville Parish. SPP-1 is part of the Shintech Plaquemine Plant Complex, which includes the following 

facilities: 

 SPP-1 – Authorized by Prevention of Significant Deterioration (PSD) Permit No. PSD-LA-709(M-1) 

and Clean Air Act (CAA) Title V Permit No. 1280-00118-V4 issued on May 9, 2012 by the Louisiana 

Department of Environmental Quality (LDEQ) 

 Hydrochloric Acid Plant (HAPF-1) – Authorized by PSD Permit No. PSD-LA-738 and CAA Title V 

Permit No. 3064-V1 issued on June 29, 2012 by the LDEQ 

 SPP-2 – Authorized by PSD Permit No. PSD-LA-731 and CAA Title V Permit No. 3063-V2 issued on 

July 31, 2012 by the LDEQ 

 HAPF-2 – Authorized by PSD Permit No. PSD-LA-739 and CAA Title V Permit No. 3066-V1 issued 

on June 29, 2012 by the LDEQ 

   
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3.2. PVC Unit and Supporting Facilities 

   
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3.3. VCM Unit 

 
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3.4. Control Devices 

Thermal destruction is accomplished in Gas Thermal Oxidizers (GTOs). Fresh air is forced into the GTO by a 

blower, where it supports combustion of natural gas to produce heat. An operating temperature of 980°C is 

maintained in the Thermal Oxidizer combustion chamber, which provides thorough decomposition of residual 

EDC, VCM, and other organic chemicals in the vent streams. The products of this decomposition are CO2, 

HCL, and small amounts of CL2 and NOx. Steam is injected into the combustion chamber to encourage the 

conversion of elemental chlorine to HCL. 

Vapors in the combustion chamber pass through the tube side of MHE551A/B boiler for heat recovery before 

entering the Vent Scrubbing Subsystem. The recovered heat produces steam for use in the plant as a utility. 

These vents enter the Scrubber below its packed section and flow upwards through a circulating stream of 

caustic water. The caustic reacts with HCL to make salt and with the chlorine to make bleach. A small flow 

of sodium thiosulfate is added to the caustic water and converts the bleach to harmless sodium sulfate. A 

constant makeup of caustic is added to replace what is lost to neutralization. A steady liquid purge to the 

Copper Removal unit removes accumulated salt, and demineralized water is added to replace the level lost to 

the purge and evaporation. 

Vents leaving the Scrubber, now essentially free of HCL and chlorine, enter the NOx Decomposer area. First 

they pass through the GTO Demister for droplet removal, then exit to the inlet side of the Vent Gas heater for 

warming, where a natural gas flame heats them to operating temperature. On their way to the NOx 

Decomposer Reactor (SCR), atomized ammonia water is sprayed into the vent stream and mixed by static 

mixers. Within the NOx Decomposer, any nitrogen oxides react on the surface of the SCR catalyst with 

ammonia to produce water and nitrogen. Hot vents exiting the SCR enter the Vent Gas Reheater where heat is 

recovered back to the SCR feed prior to these vents being released to the atmosphere. 

The purpose of the NOx Decomposer subsystem is to remove NOx in flue gases to comply with environmental 

regulations. 

   
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4. Test Matrix & Sampling Locations 

Table 4-1 summarizes information about the sampling locations and source gas characteristics (matrix) at the 

test location. 

Table 4-1 Test Matrix & Sampling Locations, Shintech SCR Control Device Inlet 

Characteristic Available Information 

Duct Geometry Circular 

Duct Size, inches ~40 

Port Size, inches >10 (Valve Assembly) 

No. of Ports & Placement 1, Vertical Plane 

Distance to Upstream Disturbance, feet TBD 

Distance to Downstream Disturbance, feet TBD 

Flow, ACFM < 14,149 

Flow, DSCFM < 8,490 (based on scrubber) 

Temperature, °F ~135 

Moisture, % 17 

Entrained Droplets? Possible (Saturated) 

O2, % ~8 

CO2, % ~8 

N2, % >80 (assumed) 

The test program involves the measurements of THC, ethane and methane from a location that has not been 

previously tested. An assumption has been made that concentrations of THC and methane will be lower at 

the SCR inlet location than at the stack. Previous testing at the stack indicates concentrations of THC have 

averaged as much as 16 ppmv @ 3% O2, concentrations of methane have averaged as high as 31 ppmvw @ 

3% O2, oxygen has averaged approximately 8% (dry), and carbon dioxide has averaged approximately 7% 

(dry). Once on site, WESTON will verify source dimensions. Volumetric flow rates will NOT be 

determined at the SCR inlet location. Shintech personnel have indicated that the source location is 

saturated. Temperature measurements will be recorded and used to calculate the percent moisture of the 

location based on saturation. 

TBD=To Be Determined 

   
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Table 4-2 Test Matrix & Sampling Locations, Shintech GTO Scrubber Stack 

Characteristic Available Information 

Duct Geometry Circular 

Duct Size, inches 71.625 

Port Size, inches 4”, 13.25” deep 

No. of Ports & Placement 2, Vertical Plane, 90 degrees apart 

Distance to Upstream Disturbance, feet 18 

Distance to Downstream Disturbance, feet 45 

Flow, ACFM 14,149 

Flow, DSCFM 8,490 

Temperature, °F 328 

Moisture, % 11.3 

Entrained Droplets? No 

O2, % 8.0 

CO2, % 6.8 

N2, % >80 (assumed) 

Previous data is available for the GTO (Stack) outlet. Previous data indicates that the location is not 

stratified, cyclonic, or saturated. WESTON will verify source dimensions, stratification, and the absence of 

cyclonic flow. 
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5. Test Methods 

This test program involves simultaneous testing using isokinetic methods for several of the test parameters. 

Each isokinetic method will generate its own set of volumetric flow data which will be used for emission 

calculations. Because simultaneous testing will involve the use of multiple ports, volumetric flow data for 

simultaneous methods may differ slightly. 

Tables 5-1 through 5-4 provide information about the test methods that will be used for the test program. 

Table 5-1 Enclosure 1 Attachment B Table Summary – Methodology 

Enclosure 1

Attachment B

Table

Pollutant Collection Method Contracted Laboratory

Table 1.1

Hydrogen Chloride (HCl) US EPA M26A Enthalpy

THC US EPA M25A  ‐

Methane US EPA M18 Direct Interface Enthalpy

Vinyl Chloride  ‐Not Requested NA

Dioxins/Furans  ‐Not Requested NA

Table 1.2 Dioxin/Furan Congener List  ‐Not Applicable NA

Table 1.3 Table 1.3 Speciated HAP List SW‐846 M0031 Maxxam

Table 1.4 Table 1.4 Speciated HAP List SW‐846 M0010 Enthalpy

Table 1.5

Ethylene glycol,

Formaldehyde, Methanol

US EPA M316

US EPA M316 Modified

Enthalpy

Acetaldehyde, 1,3‐Butadiene,

Chlorobenzene,

Chloromethane, Cumene,

Ethylbenzene,

1,1,2,2,‐Tetrachloroethane,

2,2,4‐Trimethylpentane, Vinyl

acetate, Vinyl bromide,

Xylenes (‐m/p, ‐o)

US EPA M18 Direct Interface Enthalpy

Site Specific Hap

Carbon tetrachloride,

Tetrachloroethylene,

Trichloroethylene, Methyl

isobutyl ketone

US EPA M18 Direct Interface Enthalpy

Dichloroethyl ether,

1,4‐Dichlorobenzene

SW‐846 M0010 Enthalpy
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Table 5-2 Initial ICR Test Program – GTO Scrubber Stack Location 

Method No. Parameter Condition 1, Full Load

1 

Traverse Points -- 

Test Method EPA Reference Method 1 

Number of Runs Stack measured at outset, traverse points selected 

Run Duration, Minutes NA 

Simultaneous with Methods 2, 3A, 4, 26A, 316(Modified), 0010 

Reporting Units Each 

2 

Volumetric Flow -- 

Test Method EPA Reference Method 2 

Number of Runs 3 per test 

Run Duration, Minutes Corresponds to the length of simultaneous test 

Simultaneous with Methods 1, 3A, 4, 18, 25A, 26A, 316 (Modified), 0010, 0031 

Reporting Units ACFM/DSCFM 

3A 

Gas Composition (O2, CO2, N2) -- 

Test Method EPA Reference Method 3A

Number of Runs 3 per test 

Run Duration, Minutes Corresponds to the length of simultaneous test 

Simultaneous with Methods 1, 3A, 4, 18, 25A, 26A, 316 (Modified), 0010, 0031 

Reporting Units % 

4 

Moisture -- 

Test Method EPA Reference Method 4 

Number of Runs 3 per test 

Run Duration, Minutes Corresponds to the length of simultaneous test 

Simultaneous with Methods 1, 3A, 4, 18, 25A, 26A, 316 (Modified), 0010, 0031 

Reporting Units % 

18 

Methane, Site Specific HAPS by GC -- 

Test Method EPA Reference Method 18 

Number of Runs 3 per test 

Run Duration, Minutes 240 

Simultaneous with Methods 1, 2, 3A, 4, 25A, 0010, 316 (Modified), 0031 

Reporting Units ppmvd@3% O2

25A*1

Total Hydrocarbons (THC) -- 

Test Method EPA Reference Method 25A 

Number of Runs 3 per test 

Run Duration, Minutes 240 

Simultaneous with Methods 1, 2, 3A, 4, 18, 0010 

Reporting Units ppmvd @ 3% O2 (as propane) 

26A 

Hydrogen Chloride (HCl) -- 

Test Method EPA Reference Method 26A 

Number of Runs 3 per test 

Run Duration, Minutes 120 (2 dscm) 

Simultaneous with Methods 1, 2, 3A, 4, 18, 25A, 316 (Modified), 0031 

Reporting Units ppmvd@3% O2

316 

Formaldehyde, Methanol, Ethylene 

Glycol

-- 

Test Method EPA Reference Method 316 Modified 

Number of Runs 3 

Run Duration, Minutes 60 

Simultaneous with Methods 1, 2, 3A, 4, 18, 25A, 316,26A, 0031 

Reporting Units ppmvd@3% O2

Reporting Units ppmvd @ 3% O2
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Table 5‐2    Initial ICR Test Program – GTO Scrubber Stack Location Cont’d

0010 

Semivolatile Organic Compounds 

(SVOCs) 

-- 

Test Method SW 846 Method 0010, Prep SW 846 3542, Analysis 8270D 

Number of Runs 3 per test 

Run Duration, Minutes 180 (3 dscm) 

Simultaneous with Parameter No. 1, 2, 3A, 4, 18, 25A 

Reporting Units ppmvd @ 3% O2

0031 

Volatile Organic HAPs -- 

Test Method SW 846 Method 0031, Preparation SW 846 Method 5041A, 

Analysis SW 846 M8260B 

Number of Runs 3 per test 

Run Duration, Minutes 80 (1L/min) 

Simultaneous with Parameter No. 1, 2, 3, 4, 18, 23, 25A, 26A, 316 (Modified) 

Reporting Units ppmvd @ 3% O2

*1 The 30‐day monitoring program for total hydrocarbons will be initiated before the start of the general ICR

data collection as outlined in the table above.    Calibrations will be performed before and after the four

hour test runs to bracket the THC data that will be utilized to satisfy Table 1.1 of the ICR request.    The

relevant time periods of the 30‐day monitoring data bracketed by calibrations will also be utilized for the

purposes of the four hour ICR test runs using the same THC data signal/analyzer.

   
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Table 5-3 Total Hydrocarbon 30-Day Test Program – GTO Scrubber Stack Location 

Method No. Parameter 

3A 

Gas Composition (O2, CO2, N2) -- 

Test Method EPA Reference Method 3A 

Number of Runs 30 Days Continuous(1)

Run Duration, Minutes Calibrations at a minimum daily 

Simultaneous with Methods 3A, 4, 18, 25A 

Simultaneous with Source ID SCR Inlet 

Reporting Units % 

4 

Moisture -- 

Test Method EPA Reference Method 4 

Number of Runs 1 per Day 

Run Duration, Minutes 1 hr 

Simultaneous with Methods 3A, 18, 25A 

Simultaneous with Source ID SCR Inlet 

Reporting Units % 

18/25A(2)

Methane/Ethane 

Test Method EPA Reference Method 25A using chromatographic column

Number of Runs 30 Days Continuous (1)

Run Duration, Minutes Calibrations at a minimum daily 

Simultaneous with Parameter No. 3A, 4, 18, 25A 

Simultaneous with Source ID SCR Inlet 

Reporting Units ppmvd @ 3% O2 (as methane) 

25A 

THC 

Test Method EPA Reference Method 25A 

Number of Runs 30 Days Continuous(1)

Run Duration, Minutes Calibrations at a minimum daily 

Simultaneous with Methods 3A, 18, 25A 

Simultaneous with Source ID SCR Inlet 

Reporting Units ppmvd @ 3% O2 (as propane) 

1

Thirty days of data will be collected on the unit.    If sampling time is interrupted due to weather, analyzer

failure, or unforeseen events the program will be extended until the data objective has been met.

2

A VIG 210 hydrocarbon analyzer will be used to measure THC, methane, and ethane at the inlet to the SCR

control device and at the outlet stack location.    This analyzer utilizes two FID detectors.    One FID

detector measures total hydrocarbons.    The second FID detector is attached to a chromatographic column

that separates methane and ethane from the other hydrocarbons and periodically reports their value.   

The ICR Enclosure 1 document, Table 1.6, references an analyzer using these principles in the “Alternate

Method” column.

   
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Table 5-4 Total Hydrocarbon 30-Day Test Program – SCR Control Device Inlet Location 

Method No. Parameter 

3A 

Gas Composition (O2, CO2, N2) -- 

Test Method EPA Reference Method 3A 

Number of Runs 30 Days Continuous(1)

Run Duration, Minutes Calibrations at a minimum daily 

Simultaneous with Methods 3A, 4, 18, 25A 

Simultaneous with Source ID GTO (Stack) Outlet 

Reporting Units % 

4 

Moisture -- 

Test Method EPA Reference Method 4 (psychrometric chart) 

Number of Runs Calculated from Temperature, Saturated 

Run Duration, Minutes NA 

Simultaneous with Methods 3A, 18, 25A 

Simultaneous with Source ID GTO (Stack) Outlet 

Reporting Units % 

18/25A(2)

Methane/Ethane 

Test Method EPA Reference Method 25A using chromatographic column 

Number of Runs 30 Days Continuous (1)

Run Duration, Minutes Calibrations at a minimum daily 

Simultaneous with Parameter No. 3A, 4, 18, 25A 

Simultaneous with Source ID SCR Inlet 

Reporting Units ppmvd @ 3% O2 (as methane) 

25A 

THC 

Test Method EPA Reference Method 25A 

Modifications None 

Number of Runs 30 Days Continuous(1)

Run Duration, Minutes Calibrations at a minimum daily 

Simultaneous with Methods 3A, 18, 25A 

Simultaneous with Source ID GTO (Stack) Outlet 

Reporting Units ppmvd @ 3% O2 (as propane) 1

Thirty days of data will be collected on the unit.    If sampling time is interrupted due to weather, analyzer

failure, or unforeseen events the program will be extended until the data objective has been met.

2

A VIG 210 hydrocarbon analyzer will be used to measure THC, methane, and ethane at the inlet to the SCR

control device and at the outlet stack location.    This analyzer utilizes two FID detectors.    One FID

detector measures total hydrocarbons.    The second FID detector is attached to a chromatographic column

that separates methane and ethane from the other hydrocarbons and periodically reports their value.   

The ICR Enclosure 1 document, Table 1.6, references an analyzer using these principles in the “Alternate

Method” column.

   
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 Reporting and Calculating Method Detection Limits 

Tables 1.1-1.5 of the document “Enclosure 1 Attachment B” provide the units of measure for reporting. 

Section 2.0 of the ICR document titled “Enclosure 1 Attachment C” outlines the procedure for handling 

detection limits for each test run and test series. Section 3.0 of the same document outlines how data will be 

submitted. 

Detection limits for the various compounds are listed in Table 5-5. The detection limits are based on the 

theoretical sample volumes listed in Table 5-5. Actual detection limits may vary. 

Table 5-5 Detection Limits 

Enclosure 1

Attachment B

Table

Pollutant Minimum Detection Limit

(MDL)

Minimum Sample

Volume

Table 1.1

Hydrogen Chloride (HCl) <15 ppb ( EPA M26A) 2 DSCM

THC US EPA M25A  ‐

Methane .20 – 0.50 ppm (EPA M18) NA

Vinyl Chloride  ‐Not Requested NA

Dioxins/Furans  ‐Not Requested NA

Table 1.2 Dioxin/Furan Congener List  ‐Not Applicable NA

Table 1.3 Table 1.3 Speciated HAP List See Section 14 of Protocol 20L/Tube Set

Table 1.4 Table 1.4 Speciated HAP List <0.05 ppb (SW‐846 M0010) 3 DSCM

Table 1.5

Ethylene glycol,

Formaldehyde, Methanol

0.50 g/mL (EPA M316/EPA

M316 Modified

2 DSCM

Acetaldehyde, 1,3‐Butadiene,

Chlorobenzene,

Chloromethane, Cumene,

Ethylbenzene,

1,1,2,2,‐Tetrachloroethane,

2,2,4‐Trimethylpentane, Vinyl

acetate, Vinyl bromide,

Xylenes (‐m/p, ‐o)

.20 – 0.50 ppm (EPA M18) NA

Site Specific Hap

Carbon tetrachloride,

Tetrachloroethylene,

Trichloroethylene, Methyl

isobutyl ketone

0.20 – 0.50 ppm (EPA M18) NA

Dichloroethyl ether,

1,4‐Dichlorobenzene

<0.05 ppb (SW‐846 M0010) 3 DSCM

 
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6. Process Data Requirements 

Shintech will collect sufficient process and fuel data to confirm operating conditions for each test. The 

WESTON Test Team Leader will coordinate with a designated Shintech representative before starting each run 

and upon completion of each run to (1) ensure that testing is conducted under desired conditions and (2) allow 

Shintech to flag process data appropriately. WESTON will include supplied Process Data in the Test Report. 

Per Enclosure 1, Attachment B of the ICR letter, the following process data should be reported: 

 Type of resin being processed and the resin grade 

 Emissions control device(s) 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 

 Process parameters (such as percent oxygen) 

The testing should be conducted while the PVC production process and any other non-PVC production 

process(es) that send emission streams to the same control device, is/are operating as close as possible to 

maximum mass loading of all HAP compounds to the control device and under “Normal” operation (page 2, 

paragraph 4, Enclosure 1, Attachment B) 

7. Quality Control Procedures and Audits 

Quality Control Procedures 

The quality control procedures specified in the test methods described in Section 12.0 of this test plan apply to 

the test program. 

The project reports will be reviewed by the WESTON technical director or designated WESTON quality 

assurance representative and the project manager prior to transmittal. Verification of these reviews will be 

indicated by signatures on the report transmittal page and by initialing of the DPI control sheet. All data will be 

peer reviewed before submittal to any client representative. 

Field data sheet entries and averages will be calculated and checked by a second person while onsite. Data sheets 

will be initialed and dated by the person performing the verification. Spreadsheet entries will be reviewed to 

include verification of laboratory data. Data package submittals will include the following: organized field data 

with descriptions of test problems and/or deviations, daily activity summaries describing delays encountered and 

names of regulatory observers and plant personnel present, copies of calibration records and spreadsheets as 

applicable. 

The M0031 test train will be recovered in a separate mobile laboratory from the M0010 test train to avoid 

sample contamination from organic solvents used in the recovery of those sample trains. 

Data from the 30-day total hydrocarbon monitoring program will be backed up daily during the data collection 

period to WESTON data servers. 
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WESTON may release measurement data while on site. Such data provided are considered “preliminary” and 

labeled accordingly. Final data are released following appropriate technical reviews. 

Audit Materials 

As this testing is not for compliance purposes, the audit sample for M26A (HCl) will not be requested, 

analyzed and is not required. 

8. Reporting Format and Reporting Units 

Overview 

WESTON will prepare a comprehensive test report that follows the outline established in Section 15.3 of ASTM 

D 7036-04 and will satisfy requirements established by the EPA. Measurements will be reported in the units 

specified in Tables 5.1 – 5.3. 
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Report Organization 

The Emission Test Reports will be organized as follows: 

Table 8-1 Anticipated Organization for Shintech ICR Report 

Section 1: Introduction (summary of test program objectives, personnel, and schedule) 

Section 2: HAPs Results and Discussion (including summary of all test program results) 

Section 3: Source Testing Methodology 

Section 4: Process and Sampling Location Descriptions 

Section 5: Quality Control Procedures 

Appendix A: Detailed Test Data and Results 

Appendix B: Field Data 

Appendix C: Process Data 

Appendix D: Laboratory Analytical Data 

Appendix E: Quality Control Data 

Appendix F: Example Calculations 

Please note that the final outline may vary from this draft outline if there are changes in simultaneous 

testing requirements or test methods. 

 
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Table 8-2 Anticipated Organization for Shintech ICR 30-Day THC Monitoring 

Table of Contents

Section 1: Introduction (summary of test program objectives, personnel, and schedule) 

Section 2: Results and Discussion (including summary of all test program results) 

Section 3: Source Testing Methodology 

Section 4: Process and Sampling Location Description 

Section 5: Quality Control Procedures 

Appendix A: Detailed Test Data and Results 

Appendix B: Field Data 

Appendix C: Process Data 

Appendix D: Quality Control Data 

Appendix E: Example Calculations 

 

Please note that the final outline may vary from this draft outline if there are changes in simultaneous 

testing requirements or test methods. 

 
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Report Submittal Requirements 

The initial ICR Scope test report will be submitted within six weeks after completion of the test program. A 

final report will be provided within one week of draft comments. 

The 30-Day THC Monitoring test report will be submitted within four weeks after completion of the test 

program. A final report will be provided within one week of draft comments. 

Report submittals will be in the form of hard copies and electronic (PDF) copies. If requested, WESTON will 

assist Shintech in submitting the test data to EPA via the electronic reporting tool “ERT” as required in the ICR 

documents. 

Reports shall be sent to: 

Mr. Thomas Andersen 

Shintech, Inc. 

5618 East Hwy 332 

Freeport, Texas 77541 

tandersen@shin-tech.com 

9. Plant Directions, Entry, & Safety Requirements 

Driving Directions 

The physical address for the Shintech Louisiana LLC Plaquemine Facility is: 

Shintech Louisiana LLC 

26270 Louisiana 405 

Plaquemine, LA 70764 

Entry 

Check in at Security Gate 1. 

The plant contact is Mr. Tim Gilder / Thomas Andersen.

Health & Safety 

A site-specific health and safety (H&S) plan will be prepared for this project. All field team members are 

responsible for reading the health and safety plan and signing it prior to performing work in the field. The original, 

signed H&S plan must be retained in the office and a copy prepared for use in the field. The Field Team Leader is 

responsible for maintaining a copy of Material Safety Data Sheets at the project site and for enforcing compliance 

with the Health and Safety Plan. Any changes in field situations that may require amendment of the H&S plan 

while in the field must be documented and replaced in the original document. 
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10. Test Program Personnel & Responsibilities 

Weston Organization 

The WESTON project team for this effort consists of the following individuals with the indicated responsibilities: 

Table 10-1 Test Program Personnel & Responsibilities 

Individual Cell Phone No. Responsibility Role 

Wes Fritz 610-721-6419 Client Service Manager Project Direction 

Jason Myers 512-658-4211 PM/SHSC/TTL Project Management 

Paul Meeter 484-645-2626 TD/QA Quality/Technical Management 

Donnie Fetzer 713-410-0966 TTM 

Hunter Goodlett 334-750-1507 TTM 

Jim Wallis 334-332-7127 TTM 

Enthalpy Analyst ---- TTM Onsite GC Analysis 

Ashley Bryant 334-338-5839 RC 

Natalie Hornsby 334-466-5607 QA 

Responsibilities: PM = project manager, TD = technical director, TTL = test team leader, TTM = test team member, 

AS = analytical services, SH = Sample Handler, QA = quality assurance/quality control, RC = report coordinator, EC 

= equipment coordinator, SHSC = site health and safety coordinator 

Client Organization 

Key Client contacts are summarized below: 

Table 10-2 Shintech Contacts 

Shintech 

Primary 

Shintech 

Alternate 

Name: Thomas Andersen Tim Gilder 

Shipping Address 5618 Highway 332 East 

Freeport, TX 77541 

26270 Louisiana 405 

 Plaquemine, LA 70764 

Office Phone (979) 233-7861 ext. 398 (225) 687-2105 ext. 5619 

Mobile Phone (979) 236-5641 (225) 278-5593 

E-mail: tandersen@shin-tech.com tgilder@shin-tech.com

 
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Analytical Support Contacts 

Analytical support for this project will be provided by the following laboratories: 

Table 10-3 Analytical Support Contacts 

Lab: Enthalpy Analytical Maxxam Analytics 

Contact: David Berkowitz Jim Jacklin/Clayton Johnson 

Shipping Address: 800 Capitola Dr. 

Durham, NC 27713 

6740 Campobello Road 

Mississauga, ON Canada L5N2L8 

Telephone: 919-850-4392 ext. 225 800-563-6266 

Fax: 919-491-9841 905-817-5777 

E-mail: David.Berkowitz@enthalpy.com jjacklin@maxxam.ca 

Parameters: Table 1.1 (M26A, Methane), Table 1.4, 

Table 1.5, Site Specific HAPS 

Table 1.3 (M0031) 

Turn-around Time 21-Day 21-Day 

   
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11. Test Program Schedule 

Table 11-1 Planned Test Schedule 

Day Date Activity 

GTO Scrubber Stack SCR Inlet 

1-2 10-11 Aug 2014 Travel to Site, begin setup 

3 12 Aug 2014 Continue Set-up/Begin 30-Day 

THC Monitoring 30 Day THC Monitoring 

4 13 Aug 2014 Test Run 1 / 30 Day THC 

Monitoring 30 Day THC Monitoring, Cont’d 

5 14 Aug 2014 Test Run 2 / 30 Day THC 

Monitoring 30 Day THC Monitoring, Cont’d 

6 15 Aug 2014 Test Run 3, Demobilize / 30 Day 

THC Monitoring 30 Day THC Monitoring, Cont’d 

7-32 16 Aug – 10 Sept 2014 30 Day THC Monitoring, Cont’d 30 Day THC Monitoring, Cont’d 

30 8 Sept 2014 Laboratory Data Packages Due ‐

33 11 Sept 2014 Demobilize 30 Day THC Monitoring 

51 Sept 29, 2014 Main ICR Program Draft Report Due 

61 Oct 8, 2014 30 Day THC Monitoring Program Draft Report Due 

- Nov 14, 2014 ICR Data Submission Deadline – EPA 

12. Source Testing Methodology 

The sampling methodologies to be used in the EPA ICR test program are described in the following sections. 

Table 12-1 provides detailed information regarding the sample fractions for each method and the reporting 

detection limits for the various analyses. 

12.1. Volumetric Flow Rate 

Mass emission rates are calculated by multiplying measured target analyte concentrations by calculated 

volumetric flow rates. Volumetric flow rates are calculated using measurement data obtained by EPA 

Reference Methods 1-4. 

The ductwork is measured at the sample location to the nearest 0.25 inch using a steel tape measure. Traverse 

points are selected in accordance with EPA Reference Method 1 on the basis of ductwork dimensions, 

geometry, and upstream and downstream disturbances. When a sample location does not meet EPA 

Reference Method 1 criteria, the maximum recommended number of traverse points is used. 

Gas Velocity 

The velocity of the gas stream is measured in accordance with EPA Reference Method 2 by reading the 

instantaneous velocity pressure with an inclined manometer at each traverse point using either a standard “P” 

type or an “S” type pitot tube. The stack pressure is calculated from the measured static pressure of the stack 

and the ambient barometric pressure. The static pressure is measured by using the static side of the pitot tube, 

and the barometric pressure is measured using a calibrated aneroid barometer. Magnahelic gauges with 

scales of 0 to 5 and 0 to 25 inches of water or an inclined manometer with a scale of 0 to 10 inches of water is 

used for velocity pressure measurements. Manometer selection is determined by the velocity pressure of the 
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gas stream. A manometer with a 0 to 0.25 inch scale may be used when the velocity pressure of the gas stream 

is less than 0.25 inches of water. By convention, any measured velocity pressures of less than 0.005 inches of 

water are recorded and reported as less than 0.005 inches of water. The stack temperature is measured with a 

calibrated thermocouple and pyrometer. 

For low velocity pressure measurements (less than 0.005 inches of water) a digital manometer may be used to 

measure the velocity of the gas stream. 

Gas Composition and Moisture Content 

The moisture content of the gas stream is determined using one of the following procedures: 

 For sources requiring testing by EPA Reference or Test Methods 5, 8, 12, 13, 17, 23, 26A, 29, 0010, 

or 0011, moisture is determined by EPA Reference Method 4. At the conclusion of each run the 

volume of condensed moisture in the impingers of the sampling train is measured and used to 

calculate the moisture content of the gas stream. 

 For sources with temperatures greater than 212 °F, the approximation technique described in EPA 

Reference Method 4 may be used with midget or full sized impingers to condense moisture before dry 

gas volume measurement. 

 For sources with a temperature of less than 212 °F, wet bulb/dry bulb temperature measurements may 

be made, and the moisture content calculated using vapor pressure tables. 

The molecular weight of the gas stream is calculated using the measured moisture, oxygen, and carbon dioxide 

concentrations. The balance of the gas stream is assumed to be nitrogen. The volumetric flow is then 

calculated at stack and standard conditions using the calculated molecular weight, the measured stack 

temperature, and measured velocity, stack and barometric pressures. Standard conditions are 68 °F and 29.92 

inches of mercury and 0% moisture. 

Data Acquisition and Reporting 

Data are recorded at the time of collection on preprinted data sheets. Calculations are performed (where 

possible) with verified preprogrammed calculators or spreadsheet software. 

Quality Control 

Quality control procedures for volumetric flow measurements involve leak checks of pitot tubes, pitot tube 

lines and manometers. 

Data transfers are minimized. Data sheets are checked for completeness and accuracy. Calculations are 

verified by a second person. 

 

12.2 Oxygen/Carbon Dioxide (Instrumental) 

Oxygen (O2) and carbon dioxide (CO2) testing is conducted in accordance with EPA Reference Method 3A. 

The sample is withdrawn continuously from the source through a heated probe, filter, and sample line to a 
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sample conditioner, which removes moisture from the gas stream. The sample is then transported to a 

paramagnetic O2/CO2 analyzer. The analyzer uses a paramagnetic detector to produce an electrical signal, 

which is linearly proportional to the O2/CO2 concentrations. 

12.3 Hydrogen Chloride (Table 1.1 Compound List) 

Hydrogen chloride is determined following procedures outlined in EPA Reference Method 26A. 

Sampling Equipment and Procedures 

Figure 12-3-1 presents a schematic of the sampling train. The empty first impinger in the figure is optional. The 

nozzle and heated probe is constructed of borosilicate glass and connected to a heated filter holder containing a 

Teflon® coated quartz filter. This is connected to an impinger train. The first and second impingers are each 

charged with 100 mL of 0.1 N H2SO4. The third and fourth impingers contain 100 mL of 0.1 N NaOH. The fifth 

impinger is charged with 200-300 grams of indicating silica gel. All impingers are maintained in a crushed ice 

bath. A gas measuring control console with a leakless vacuum pump, a calibrated dry gas meter, a calibrated 

orifice, and inclined manometers are connected to the final impinger via an umbilical cord to complete the train. 

Flue gas velocity is measured with a calibrated S-type pitot tube (provided with extensions) fastened alongside the 

sampling nozzle. Flue gas temperature is monitored with a calibrated direct readout pyrometer equipped with a 

chromel-alumel (Type K) thermocouple positioned near the sampling nozzle. The impinger exit gas temperature 

is monitored with a calibrated direct readout pyrometer equipped with Type K thermocouples positioned in the 

sample gas stream after the last impinger. Stack gas stream composition (carbon dioxide and oxygen content) is 

determined as described previously. The sampling rate is adjusted, based on stack velocity, at each point to 

ensure the sample is collected isokinetically. 

After completion of the sample run, the sample train is leak checked. Following a successful leak check, the 

contents of the first and second impingers are measured and transferred to a borosilicate glass sample container 

with a Teflon® lined lid. The impingers are then rinsed with deionized water into the same sample container. 

Sample Analysis 

The samples are analyzed for chloride using ion chromatography (IC) as described in the Method 26A. All IC is 

performed using acceptable laboratory procedures. Adherence to prescribed quality control procedures as 

described below ensures data of consistent and measurable quality. Analytical quality control focuses on 

instrument calibration as per EPA Reference Method 26A and the use of control standards to provide a measure of 

analytical precision and accuracy. Specific acceptance criteria is defined for analytical operations including 

calibrations and control standard analyses. 

 
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Figure 12‐3‐1 EPA Reference Method 26A Hydrogen Chloride Sampling Train

Optional
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Analytical quality control includes analysis of a laboratory blank, method spikes, and duplicates. The laboratory 

blank consists of the DI H2O used for any sample dilutions analyzed per the procedures specified in draft Method 

26A to check for laboratory contamination. Method spikes for EPA Reference Method 26A are prepared by 

spiking a representative amount of HCl into 0.1 N H2SO4 and adjusting the volume to 100 mL using DI H2O. The 

method spikes are handled in the same manner as (and analyzed with) the field samples. 

Data Acquisition and Reduction 

Data is recorded at the time of collection on preprinted data sheets. Calculations are performed (where possible) 

with preprogrammed calculators or spreadsheet software. 

Quality Control 

Calibration and leak checking of the appropriate sampling equipment, including meter boxes, temperature sensors, 

nozzles, pitot tubes, and umbilicals, are performed according to the requirements specified in EPA’s “Quality 

Assurance Handbook, Volume III” (600/4-77-027b). The results are documented and retained. 

Dry gas meters are calibrated before and after sampling. Thermocouples are calibrated against mercury 

thermometers, and aneroid barometers are calibrated against a mercury barometer. The temperature of the gas 

leaving the impinger train is kept at 68 °F or less throughout the sampling by maintaining the ice bath. Care is 

taken to prevent sample loss during sample recovery. Sample storage bottles are purchased new or cleaned prior 

to use and are kept sealed at all times. Samples are transported to the laboratory under chain-of-custody. Upon 

receipt by the laboratory, the liquid level in each sample bottle is noted. If a noticeable amount of liquid has been 

lost, the sample is voided. Reagents used during testing meet American Chemical Society specifications. A blank 

is analyzed with each series of samples. 

Data transfers are minimized. Field and laboratory data sheets are checked for completeness and accuracy. 

Calculations are verified by a second person. 

12.4 Formaldehyde, Methanol and Ethylene Glycol (Table 1.5 Compound List) 

Formaldehyde, methanol, and ethylene glycol are determined following procedures outlined in EPA Reference 

Method 316 and through a series of analysis developed by Enthalpy Analytical, Inc. to meet the objectives of 

the PVC ICR. 

Sampling Equipment and Procedures 

Figure 12-4-1 presents a schematic of the sampling train. The nozzle and heated probe is constructed of 

borosilicate glass and is connected to an impinger train. When stack moisture levels are high, the first impinger is 

left empty. The second, third and fourth impingers are each charged with 100 mL of distilled water. The fifth 

impinger is charged with 200-300 grams of indicating silica gel. All impingers are maintained in a crushed ice 

bath. A gas measuring control console with a leakless vacuum pump, a calibrated dry gas meter, a calibrated 

orifice, and inclined manometers are connected to the final impinger via an umbilical cord to complete the train. 

Flue gas velocity is measured with a calibrated S-type pitot tube (provided with extensions) fastened alongside the 

sampling nozzle. Flue gas temperature is monitored with a calibrated direct readout pyrometer equipped with a 

chromel-alumel (Type K) thermocouple positioned near the sampling nozzle. The impinger exit gas temperature is 

monitored with a calibrated direct readout pyrometer equipped with Type K thermocouples positioned in the 

sample gas stream after the last impinger. Stack gas stream composition (carbon dioxide and oxygen content) is 
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determined as described previously. The sampling rate is adjusted, based on stack velocity, at each point to ensure 

the sample is collected isokinetically. 

After completion of the sample run, the sample train is leak checked. Following a successful leak check, the 

contents of the first, second and third impingers are measured and transferred to a polyethylene sample container. 

The contents of the fourth impinger are measured and transferred to a separate polyethylene sample container. The 

impingers are then rinsed with deionized water into the respective sample containers. 
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Sample Analysis 

FormaldehydeThe samples are analyzed for formaldehyde using ion chromatography (IC) as described in the 

Method 316. All IC is performed using acceptable laboratory procedures. Adherence to prescribed quality control 

procedures as described below ensures data of consistent and measurable quality. Analytical quality control 

focuses on instrument calibration as per EPA Reference Method 316 and the use of control standards to provide a 

measure of analytical precision and accuracy. Specific acceptance criteria are defined for analytical operations 

including calibrations and control standard analyses. 

Analytical quality control includes analysis of a laboratory blank, method spikes, and duplicates. The laboratory 

blank consists of the DI H2O used for any sample dilutions analyzed per the procedures specified in Method 316 to 

check for laboratory contamination. Method spikes for EPA Reference Method 316 are prepared by spiking a 

representative amount of formaldehyde into DI H2O. The method spikes are handled in the same manner as (and 

analyzed with) the field samples. 

An EPA Method 316 blank train (identical to the source sample train) is setup with one of the test runs. The blank 

train samples along with a blank DI H2O site blank is analyzed with the source samples. 

An analysis of the final impinger is performed separately to evaluate sample train collection efficiency. 

MethanolMethanol is analyzed from the Method 316 impingers using a modified Method 308 approach. An analysis of the 

final impinger is performed separately to evaluate sample train collection efficiency by GC/FID. 

A matrix spike (MS) is prepared and analyzed for each source. 

Ethylene GlycolEthylene glycol analysis is conducted from the Method 316 impingers using a modification of EPA Method 18 

which employs an azeotropic distillation to remove water from the sample to ensure complete derivatization. An 

analysis of the final impinger is performed separately to evaluate sample train collection efficiency. An internal 

standard and surrogate are added to ensure accurate results. Enthalpy has developed this method due to the 

known challenges analyzing ethylene glycol at low concentrations from a water matrix by GC/FID. A matrix 

spike (MS) is prepared and analyzed for each source. 

Data Acquisition and Reduction 

Data is recorded at the time of collection on preprinted data sheets. Calculations are performed (where possible) 

with preprogrammed calculators or spreadsheet software. 

Quality Control 

Calibration and leak checking of the appropriate sampling equipment, including meter boxes, temperature sensors, 

nozzles, pitot tubes, and umbilicals, are performed according to the requirements specified in EPA’s “Quality 

Assurance Handbook, Volume III” (600/4-77-027b). The results are documented and retained. 
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Dry gas meters are calibrated before and after sampling. Thermocouples are calibrated against mercury 

thermometers, and aneroid barometers are calibrated against a mercury barometer. The temperature of the gas 

leaving the impinger train is kept at 68 °F or less throughout the sampling by maintaining the ice bath. Care is 

taken to prevent sample loss during sample recovery. Sample storage bottles are purchased new or cleaned prior to 

use and are kept sealed at all times. Samples are transported to the laboratory under chain-of-custody. Upon receipt 

by the laboratory, the liquid level in each sample bottle is noted. If a noticeable amount of liquid has been lost, the 

sample is voided. Reagents used during testing meet American Chemical Society specifications. A blank is 

analyzed with each series of samples. 

Data transfers are minimized. Field and laboratory data sheets are checked for completeness and accuracy. 

Calculations are verified by a second person. 

 12.5 Semivolatile Organic Compounds (Table 1.4 Compound List, Site Specific HAP) 

The semivolatile organic compounds train is described in SW-846 as Method 0010. Semivolatile organic 

compound analysis is conducted according to EPA SW-846 8270D. 

Sampling Equipment and Procedures

The Method 0010 Sampling Train is shown in Figure 12-5-1. Please note that an optional extra impinger is 

depicted before the silica gel impinger. The impinger train is assembled in the sample recovery area. The 

pre-cleaned impingers are assembled with the first impinger being an empty knockout impinger with a short stem. 

The purpose of this impinger is to collect the majority of the condensate which forms in the condenser coil and 

XAD resin module. The next two impingers are standard type Greenberg-Smith impingers, each containing 100 

mL of HPLC grade water. The fourth impinger is empty and the fifth impinger is charged with approximately 

300 grams of indicating silica gel. The glass fiber filter is placed in a filter holder and connected to the 

condenser coil and XAD resin module. The train components are then transferred to the sampling location and 

assembled completely. 

After the sampling train is assembled and all components are heated appropriately, a leak check is performed. 

During sampling, the temperature of the sorbent module resin is not to exceed 68 °F. The probe temperature is 

maintained above 248 °F + 25 °F ; the filter temperature is controlled at 248 °F + 25 °F, and the outlet of the 

silica gel impinger is maintained at less than 68 °F during operation. 

The sampling train is leak-checked at the beginning and end of the run and each port change. An acceptable leak 

rate is less than 0.02 acfm at the highest vacuum measured plus one inch of Hg or less than 1.5% of the sampling 

rate. 

After a successful pre-test leak check, the train assembly is placed in the stack and operated along each of the 

traverse points for each of the two horizontal traverses. Sampling is performed for a total of three hours using a 

sampling rate between 0.5 and 0.75 scfm to collect a total sample volume of at least 106 dscf (3 dscm). Sampling 

train data are recorded on standard data forms. 

The Method 0010 sampling trains are recovered following the scheme presented in Figure 12.5.2. Liquid 

samples are placed in pre-cleaned amber glass sample containers with Teflon® liners. The filters are placed in 

pre-cleaned glass petri dishes or amber glass sample containers. The reagent blank containers for the train 

fractions are listed in Table 12-5-1. 
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Figure 12‐5‐1 M0010 EPA Method Sampling Train for Semivolatile Organics
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Figure 12-5-2 Sample Recovery Procedures for Method 0010 Sampling Trains 
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Reagent blank samples are collected as follows: 

Table 12-5-1 – M0010 Reagent Blank Samples 

Reagent Amount Fraction Blank Trains 

Trip 

Blanks 

HPLC Water 300 mL IMP CON 1/source 1/trip 

Methanol/Methylene 

Chloride 200 mL FHR, BHR IMPR 1/source 1/trip 

XAD Sorbent Modulea N/A ---- 1/source 1/trip 

Glass Fiber Filter N/A ---- 1/source 1/trip 

Methanol 200 mL ---- 1/source ----- 

Methylene Chloride 200 mL ---- 1/source ----- 

a

XAD sorbent module is randomly selected from the on-site XAD modules used for the test program. 

Sample Analysis

Semivolatile Organic Compounds

The M0010 semi-volatile samples are normally analyzed according to SW-846 Method 8270D. For the PVC 

ICR, the EPA mandates that SW-846 Method 3542 be used for sample preparation and SW-846 Method 8270D 

with a low resolution GC/MS SIM analytical finish be used for analysis. The methanol/methylene chloride front 

half (FH) probe rinse is concentrated to about 2 mL using a Kuderna-Danish (KD) apparatus and then combined 

with the filter in a soxhlet apparatus. A set of 8 Base/Neutral/Acid (BNA) surrogates along with the above 

labeled standards is spiked into the soxhlet at 100 mg levels. The combined filter and FH rinses are then soxhlet 

extracted with methylene chloride for 16 hours. 

The methanol/methylene chloride back half rinses (BHR) are concentrated to about 2 mL using a KD apparatus 

and then combined with the XAD resin in a soxhlet apparatus. The eight BNA surrogates along with the labeled 

standards are spiked into the soxhlet and the combined XAD and BHR are soxhlet extracted with methylene 

chloride for 16 hours. 

The impinger water is spiked with the eight BNA surrogates and labeled standards at 100 mg levels and then 

liquid-liquid extracted with methylene chloride. 

Each extract is dried over sodium sulfate, concentrated to a volume of 5 mL and cleaned using gel permeation 

chromatography (GPC). 

For a list of the compounds that will be determined during this test program by SW-846 Method 0010, please 

refer to Table 5.1. 
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Data Acquisition and Reduction

Data will be recorded at the time of collection on preprinted data sheets. Calculations will be performed (where 

possible) with verified preprogrammed calculators or spreadsheet software. 

Quality Control

The standard M0010 pre-cleanup requirements include several unique preparation steps which ensure that the 

sampling train components are not contaminated with organic compounds that may interfere with the analysis. 

The glassware, glass fiber filters, and XAD adsorbing resin are pre-cleaned using strict protocols. 

The glassware is normally cleaned as shown in Table 12-5-2. Glassware is washed in soapy water, rinsed with 

distilled water, baked and then rinsed with acetone followed by methylene chloride. Once the glassware is dried, 

the open ends will be sealed with either methylene chloride-rinsed aluminum foil or Teflon® tape. 

Non-glass components (such as the Teflon® filter supports and seals, tweezers, Teflon® squeeze bottles, nylon 

nozzle, and probe brushes) are cleaned following the same procedure, except that no baking is performed. 

Table 12-5-2 

Organic Glassware Cleaning Procedure 

(Train Components, Sample Containers, and Laboratory Glassware) 

NOTE: USE VITON GLOVES AND ADEQUATE VENTILATION WHEN RINSING WITH 

SOLVENTS 

1. Soak all glassware in hot soapy water (AlconoxÔ). 

2. Tap water rinse to remove soap. 

3. Deionized H2O rinse (x3).a

4. Bake at 450° for 2 hours.b

5. Methanol rinse (x3), (pesticide grade). 

6. Methylene chloride (x3), (pesticide grade). 

7. Cap glassware with Teflon® tape or methylene chloride rinsed aluminum foil. 

8. Mark cleaned glassware with color-coded identification sticker. 

a

(x3) = three times. 

b

Step (4) is added to the cleanup procedure to replace the dichromate soak specified in the reference method. 

It has been demonstrated that baking at 450 °F sufficiently removes organic artifacts. It is not used for probe 

liners and non-glass components of the train that cannot withstand 450 °F (i.e., Teflon®-coated filter screen and 

seals, tweezers, Teflon® squeeze bottles, nylon probe and nozzle brushes). 
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The XAD adsorbent resin and glass fiber filters are pre-cleaned by separate procedures. The XAD, which is 

purchased in 100 gram amber glass containers, is placed in the glass modules under strict laboratory-controlled 

conditions. Each lot of XAD resin is recorded in a laboratory notebook and a control sample is withdrawn for a 

quality assurance analysis. The laboratory archives a sample from each lot for analysis with the field sample as a 

lab blank. 

To prepare the filters, a batch of 50 filters are placed in a soxhlet extraction apparatus and extracted using 

methylene chloride for 16 hours. Afterwards, the filters are checked for holes, tears, creases, and discoloration. 

Acceptable filters are placed in pre-cleaned containers and labeled by date of extraction and sealed with Teflon®

tape. 

The remaining equipment preparation includes routine checking and calibration of the Method 5-type equipment 

as specified in Method 0010. 

During one of the runs, an M0010 field blank train is assembled with glassware that has previously been use for 

M0010 sampling. This train is charged exactly as the other M0010 trains and left at a sampling location during 

the test run. The field blank train is then recovered with the other M0010 train for that run. The sample train 

results are used to assess the level of contamination that occurs from handling, charging, recovering, and 

transporting the sampling train. 

One sample train blank is prepared for each source. One set of trip blanks are collected and archived for future 

examination, if contamination is determined. A lab method blank using the control XAD blank that is withheld 

during the XAD module preparation phase is also analyzed. 

QC guidelines can be found in SW-846 Method 0010. 

To further ensure sample integrity and stability, smoking is not allowed in or around the Laboratory Recovery 

Area, and XAD resin samples are immediately stored at or below 4 °C. 

Data transfers are minimized. Field and laboratory data sheets are checked for completeness and accuracy. 

Calculations are verified by a second person. 

 12.6 Total Hydrocarbon Concentrations (Table 1.1 Compound List, 30-Day Monitoring) 

Total hydrocarbon (THC) concentrations are sampled using EPA Reference Method 25A and analyzed by 

WESTON on site with a flame ionization detector (FID) analyzer. It should be noted that Method 25A 

determines total organics, including methane, which is not a regulated volatile organic compound (VOC). 

Sampling Equipment and Procedures

Figure 12-6-1 is a schematic of the EPA Reference Method 25A sampling system. An extractive system is used 

at the sampling locations to obtain vent gas samples. Samples are withdrawn continuously at a single point and 

transported to the FID through a heated probe Teflon® filter, and heated Teflon® sample line. All hydrocarbon 

measurements are made on a "hot, wet" basis. 

Sample Analysis

A continuous emission monitor is used to measure the total hydrocarbon concentration in the source gas. This 

analyzer utilizes a FID as described by EPA Reference Method 25A. The technique is not selective between 

species, and the results are reported as carbon volume equivalents of the calibration gas (propane in nitrogen or 

propane in air). 
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Calibration gases are introduced at the probe and recovered through the sampling and analytical system. After 

zeroing, a high level certified calibration gas is used to span the analyzer and generate a linear response line 

between the zero and high gas concentration. A low and mid-level certified calibration gas is then introduced to 

the analyzer to verify the linear response of the analyzer. An interference response study was performed by the 

manufacturer of the analyzer. The data from this study are on file at WESTON. 

Data Acquisition and Reduction

Data is acquired electronically using a computer with software designed by WESTON for EPA Reference Method 

25A analysis. 

Quality Control

The calibration and check gases are propane, in either nitrogen or air, certified according to EPA Protocol-1. 

Following each sample run, the calibration drift of the system is checked by introducing the zero and one upscale 

gas to the system and recording the response. This difference in concentration must be within three percent of the 

full scale span value. 

 
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 12.7 Volatile Organic Compounds (SW846 Method 0031) (Table 1.3 Compound List) 

Volatile organic compounds are measured using the Volatile Organic Sampling Train (VOST). Four runs of 

SW-846 Method 0031 are conducted on each stack. Analysis is performed by Maxxam Analytics, Inc. using 

a gas chromatograph with a mass spectrophotometer (GC/MS) according to the procedures outlined in SW-846 

Method 8260B. 

VOST Sampling Equipment and Preparation 

The volatile organic sampling train (VOST) of SW-846 Method 0031 is used to collect the volatile organic 

samples. Figure 12-7-1 is a schematic of the Method 0031 sampling train. 

The VOST equipment, except the sorbent cartridge, is cleaned and calibrated by WESTON according to 

Method 0031. The sorbent cartridges used for sampling are prepared by an outside lab. This consists of first 

cleaning the glass tubes and metal parts with a nonionic detergent, rinsing in organic-free water, and drying at 

the specified temperatures. The Tenax and Anasorb are soxhlet extracted with methanol and dried. The 

Tenax and Anasorb tubes are then assembled and conditioned by heating to 190 °C while organic-free 

nitrogen is passed through them. Each set of tubes are blank checked by thermal desorption and gas 

chromatographic techniques prior to sampling to ensure cleanliness. 

VOST Sampling Procedures 

The volatile organic sampling train is assembled as shown in Figure 12-7-1. Samples are collected using a set 

of paired Tenax (two) and Anasorb cartridges, with each cartridge preceded by a condensing module. The 

first condenser cools the gas stream and condenses the water vapor present. The flue gas and condensed 

moisture then pass through a pair of cartridges containing 1.5 grams of Tenax resin (60-80 mesh). The 

condensate is collected in an impinger that is continually purged by the gas stream. 

The second condenser and cartridge containing Anasorb serves as a backup for breakthrough compounds. 

Following the third cartridge is a silica gel drying tube for residual moisture removal. 

Each sample run consists of four or five tube sets. The individual tube sets are collected at a set sample 

volume for at least 20 minutes. The sample volumes for each of the sets of cartridges are approximately 20 

liters. Sampling is conducted at a single point. The system is leak-checked by closing the valve at the inlet to 

the first condenser and evacuating the system at 10 inches Hg. The system will then be isolated and the leak 

rate noted. The leak rate must be less than 1 inch Hg after one minute. The train will be returned to 

atmospheric pressure by purging through a charcoal tube. The leak checks will be conducted before and after 

each set of VOST tubes is collected. The first three tube sets will be analyzed. The fourth tube set will be 

archived. A fifth set will be retained as a field blank. 

 
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Figure 12-7-1 

EPA Method 0031 Volatile Organic Sampling Train (VOST) 

       
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Gas sample temperatures are to be monitored at the outlet of the sampling probe and the inlet to the Tenax and 

Anasorb cartridges using thermocouples. The temperature of the gas through the sorbent tubes is maintained at 

less than 20 °C.

VOST Sample Recovery 

After recovering the sample for the VOST the system is leak-checked as required, the cartridges are capped 

and placed in original glass culture tubes with glass wool to absorb the shock. The volume of condensate 

impinger is measured in a precleaned graduated cylinder and transferred to 40 mL VOA vials and diluted to 

volume with HPLC water to decrease headspace, which reduces the possibility of revolatilization of the 

compounds. To reduce reactivity store samples at 4 C. 

The samples collected during each VOST run consist of the four sets of sorbent tubes (Tenax cartridge, Tenax 

cartridge, and Anasorb cartridge), and the condensate. One additional set of Tenax, Tenax, and Anasorb 

cartridges serves as field blanks per day. The set is taken to the sampling site and the end caps removed for the 

period of time required to exchange one set of traps on the VOST. After the VOST traps have been 

exchanged, the end caps are replaced on the field blanks, and are stored and analyzed with the field samples. 

A second set of blank cartridges is included in the cartridge shipment to the test site. These trip blanks are 

treated like the other cartridges except that the end caps are not removed during storage at the site. These are 

also analyzed with the field samples. 

One pair of blank cartridges, a laboratory blank, remains stored in the laboratory. This blank is analyzed if the 

field or trip blanks show high contaminant concentrations. 

VOST Sample Analysis 

The volatile organic contents of each cartridge and condensate sample are thermally desorbed onto a gas 

chromatographic column (GC). The Tenax cartridges are analyzed separately from the Anasorb cartridge; 

likewise the condensate fractions are also analyzed separately. Prior to sample recovery, the contents of the 

sorbent cartridges are spiked with a deuterated standard as well as other unlabeled internal standards that are 

similar to the analytical characteristics of the compounds of interest. Following spiking, the cartridge 

contents are thermally desorbed using an inert gas which is then bubbled through organic-free water. The 

desorbed components pass into the bottom of the water column where they are purged from the water, and 

collected on an adsorbent trap. After completion of the desorption, the compounds are described from the 

adsorbent trap onto a gas chromatographic column. 

For the condensate sample, the sample fraction is spiked with the same internal standards indicated above. 

Afterward, an inert gas is bubbled through the solution at ambient temperature and the volatile compounds are 

transferred from the aqueous phase to the vapor phase. The vapor is swept through a sorbent column where 

the volatile compounds are trapped. Upon completion of purging, the sorbent column is heated and 

backflushed with inert gas to desorb the components onto a gas chromatographic column. 

The volatile organic target compounds of interest are analyzed following the procedures specified in EPA 

Reference Methods 5041A for the media and 8260B for the condensate. 
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Following the procedures outlined in Method 8260B, the volatile compounds are directed into the GC/MS 

system. The volatile compounds are separated by temperature programmed gas chromatography and detected 

by low-resolution mass spectrometry. The concentrations of the volatile compounds of interest are calculated 

using the labeled and unlabeled internal standard technique. 

For a list of the compounds that will be determined during this test program by SW-846 Method 0031, please 

refer to Table 5.1. 

Volatile Sample Quantitative Analysis 

Quantitative analysis is performed by GC/MS using extracted ion current profile (EICP) areas: 

The GC/MS system is calibrated using a quantitation ion and the compound concentration is determined using 

an internal standard technique. 

For compounds where standards are not available, compound concentrations are determined using known 

response factors from the closest internal standard. 

Volatile Analysis Quality Control 

The major QC procedures contained within the method will include GC/MS tuning, calibrations system 

performance checks and analysis of specific QC check samples. During actual sample measurements, several 

field blanks, trip blanks and a laboratory method blank are analyzed with the field samples. The quality of the 

analysis is assured through reproducible calibration and testing of the purge and trap and GC/MS systems. 

Spiked cartridges are transported to the field, and returned to the laboratory and analyzed to determine analyte 

recovery from the sorbents. 

VOST Sampling QC Procedures 

Quality Control procedures for VOST sampling are designed to ensure the collection of high quality gas stream 

concentrations and emission data without interference of contaminants. Gas stream concentrations of each 

analyte are determined by dividing the mass of each analyte collected by the standardized gas volume 

collected. 

VOST sampling QC procedures include: 

 Use of precleaned glassware. 

 Sampling train composed of glass and/or Teflon. 

 Sorbent traps are prepared and stored in a manner to prevent contamination. 

 Recovery procedures are completed in a clean environment. 

 Four samples are collected and three are analyzed per run to ensure adequate analysis. 

 Samples are stored and shipped at reduced temperature (~4 °C). 

 At least one field blank per day and one trip blank per test program will obtained and analyzed. 
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Data Reduction, Validation, And Reporting 

Data quality audits are conducted using data quality indicators which require the detailed review of: (1) the 

recording and transfer of raw data; (2) data calculations; (3) the documentation of procedures; and (4) the 

selection of appropriate data quality indicators. 

Some of the data quality indicators to be used for data validation are: 

 Comparison of the relative concentrations of the emissions at the different sampling locations. 

 Comparison of the results for a particular parameter with those from each condition (i.e., are the 

concentrations similar and do they show the same relationship for a material balance). 

 All data and/or calculations for flow rates, moisture content, and isokinetic rates made using a computer 

software program are validated by an independent check. All calculations are spot checked for accuracy 

and completeness. 

In general, all measurement data is validated based on the following criteria: 

 Process conditions during sampling or testing, 

 Acceptable sample collection procedures, 

 Consistency with expected other results, and 

 Adherence to prescribed QC procedures. 

Any suspect data is flagged and identified according to the specific deviation from prescribed criteria and its 

potential effect on the data quality. Upon completion of testing, the field coordinator is responsible for 

preparation of a data summary including calculation results and raw data sheets. 

The test report includes QA/QC summaries reporting the QC data collected and the results of any audits. The 

outside laboratory reports its QA/QC results in the analytical report. All QA/QC results are reviewed 

internally by WESTON before the data are released; any data that fail to meet the program’s QA requirements 

are noted. 

12.8 Speciated HAP – Direct Interface (Table 1.1 Compound List, Site Specific HAP) 

EPA Method 18 outlines three different sampling approaches with gas chromatography as the analytical 

method. The three approaches include direct interface, adsorption media, or whole gas sample collection 

utilizing flexible Tedlar® bag enclosures. The GC conditions are not defined as the number of compounds 

and compound mixtures requires selective GC conditions. 

Sampling Equipment and Procedures 

For the direct interface approach, the sampling equipment incorporates a heated sample probe with filter 

(in-stack or heated-out-of-stack), heated sample line, heated diaphragm pump. The sample is delivered 

continuously to the onsite mobile laboratory at a rate of 1-2 L/min. Excess sample gas is vented from the 

laboratory. 
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At all times during the sampling period, the heated sampling system is maintained at a temperature above the 

condensation temperature of the stack. Maintaining the sample above the condensation temperature ensures 

that the target compounds are maintained in the vapor phase and any moisture present in the sample is not 

condensed (condensed moisture will selectively remove polar organic compounds). 

A schematic representation of the direct interface sampling and analytical equipment is shown in Figure 

12-8-1. 

   
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Figure 12‐8‐1 Direct Interface Sampling System
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Sample Analysis 

For the analysis of gaseous samples, the chromatography conditions required to resolve and quantify the target 

compounds are developed prior to sample collection. 

The analytical system is comprised of three main components, sample introduction system, chromatograph 

with selected columns and detector, and the data collection system with report generator. 

The sample injection system uses a heated rotary valve with Teflon® sample loop. The certified calibration 

gas mixtures and samples are introduced to the chromatograph using the same injector. The GC uses capillary 

columns which are commercially available and chosen to resolve the target compounds within a reasonable 

time frame, 5 - 45 minutes. 

Detection and relative intensity of calibration gas or sample gas matrices is performed by the GC FID detector, 

which measures a change in potential across an enclosed flame. The difference in potential is directly 

proportional to the concentration present. Calibration curves for the target compounds are prepared at a 

minimum of three concentration levels, and bracket the concentration range of the samples. 

The identity of target compounds is determined by comparison of the sample gas retention times compared to 

the retention times of calibration gas mixtures. The concentration of the target compounds is determined from 

comparison of the intensity of the sample peaks compared to the intensity of the calibration peaks. 

Commercially available calibration gas mixtures are obtained which meet the method accuracy criteria. 

For high concentration sources, where commercially available gas standards are not available, calibration gas 

mixtures are prepared by injection of a known mass of the target compound into a known volume of air or 

nitrogen. 

For a list of the compounds that will be determined during this test program by EPA Method 18, please refer to 

Table 5.1. 

Data Acquisition and Reduction 

The output from the GC/FID system is collected using a commercially available data acquisition interface and 

software. The system generates the calibration curves and produces a report and chromatogram at the 

conclusion of each analysis. 

Quality Control 

Quality controls for the direct interface system include a leak check of the entire sampling system and target 

compound recovery checks. 

For the direct interface recovery study, the mid-level calibration gas (for at least one of the target compounds) 

is presented to the sample probe. The calibration gas is collected and analyzed as a sample. An acceptable 

recovery yields a GC response to within 10% of the direct calibration standard analyzed response. 

 
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13. Laboratory Sample Summary 

Table 13-1 Sample Collection Summary, Main ICR Test Program

Container Number

Number

Collected /Test

Program Designation(1) Description

EPA M26A – HCl (ICR Table 1.1 Compound List)

1 0  ‐  Filter

2 0  ‐  Front Half (FH) Rinse

3 3 S Knockout/Acid Impingers

4 0  ‐  Alkaline Impingers

5 0  ‐  Silica Gel

6 1 RgB 0.1 N H2SO4 Diluted w/ Water

7 0  ‐  0.1 N NaOH

8 1 RgB Rinse Water

9 1 RgB Acetone

HCl is collected with a M26A isokinetic sampling train consisting of sulfuric acid (H2SO4) charged impingers.   

The samples are analyzed using IC by Enthalpy Analytical.    This approach has an in‐stack MDL of < 15ppb /

analyte based on a minimum sampling volume of 2.0 DSCM.    Samples will be recovered into HDPE bottles.

As this test program is not to demonstrate initial compliance, audit samples have not been requested.

‐One fraction analysis per train‐ 

EPA M316 – Formaldehyde, Methanol, Ethylene Glycol (ICR Table 1.5 Compound List)

1A 4 3S, 1FB FH Rinse, Knockout, Imp. 1, Imp.2

1B 4 3S, 1FB Imp. 3

2 1 RgB Reagent Water

3 0  ‐  Silica Gel

Flue gas is withdrawn isokinetically from the source and formaldehyde, methanol, and ethylene glycol is

collected using an initial condenser followed by three impingers charged with high purity water.    The

condenser catch will be combined with the contents of the first two impingers and the third impinger will

be recovered separately to evaluate the train for breakthrough.

Formaldehyde

Formaldehyde will be analyzed by Enthalpy using the modified pararosaniline method.    Formaldehyde

reacts with the acidic pararosaniline and sodium sulfite to form a purple chromophore that is measured by

spectrophometer at 570nm.    The MDL for formaldehyde is 0.05g/mL.    A matrix spike (MS) will be

prepared and analyzed for each source.

‐Two fraction analyses per train‐ 

Methanol

Methanol is analyzed by Enthalpy from the Method 316 impingers using a modified Method 308 approach

with analytical MDL of 0.50 g/mL.    A matrix spike (MS) will be prepared and analyzed for each source.

‐Two fraction analyses per train‐ 

Ethylene Glycol

Ethylene glycol analysis will be performed by Enthalpy from the Method 316 impingers using a modification

of EPA Method 18 which employs an azeotropic distillation to remove water from the sample to ensure a

complete derivatization.    An internal standard and surrogate are added to ensure accurate results.   

Enthalpy has developed this method due to the known challenges analyzing ethylene glycol at low

concentrations from a water matrix by GC/FID with a 0.50 g/mL analytical MDL.    A matrix spike (MS) will

be prepared and analyzed for each source.

‐Two fraction analyses per train‐ 
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SW‐846 0010/8270D – Semi‐VOHAPs (ICR Table 1.4, Speciated HAP Compound List)

1 5 3S, 1FB, 1RgB Filter

2A 4 3S, 1FB Probe / FH Rinse

2B 1 RgB FH Rinse Blank

3 5 3S, 1FB, 1RgB Sorbent Trap

4 4 3S, 1FB Condensate and BH Filter House

5 4 3S, 1FB Filter to 1st Wet Impinger

6 0  ‐  Silica Gel

7 1 RgB Water

8 1 RgB MeOH

9 1 RgB MeCl2

Semi‐VOHAPs are collected by EPA SW‐846 Method 0010 utilizing a Method 5 type configuration with the

addition of an XAD trap after the heated filter.    Enthalpy packs and spikes ball and socket traps with blank

checked XAD‐2 resin.    After collection the filter, XAD trap, rinses, and water are recovered and returned to

Enthalpy for analysis.    Samples are prepared by SW‐846 Method 3542 and analyzed by EPA SW‐846

Method 8270D with a low resolutions GC/MS SIM analytical finish.    The analytical technique has an MDL

of <0.05 ppb/compound in‐stack based on a sampling volume of 3 DSCM

‐Three fraction analyses per train‐ 

SW‐846 Method 0031/5041/8260B – VOC by VOST (ICR Table 1.3 Compound List)

1 3 S Tube Set – Tenax/Tenax/Anasorb

2 3 FB Tube Set – Field Blank (1/Test Run)

3 1 TB Tube Set – Travel Blank (1/Test)

4 3 S Condensate

5 3 FB Condensate – Field Blank

Sample is collected by SW‐846 M0031, samples are prepared by SW‐846 5041, and samples are analyzed by

SW‐846 8260B.    Analysis will be performed by Maxxam Analytics.    Samples will be collected at 1L/min

over two hours, with tube sets being changed every twenty minutes.    Each tube set consists of two Tenax

tubes and one Anasorb tube.    Six tube sets, one condensate, one field blank tube set, and one field blank

condensate will be captured per test run.    Traps for each test run will be combined to lower detection

limits.

‐Three fractions per analyses‐  (1) S=Sample, FB=Field Blank, RgB=Reagent Blank, TB=Trip Blank 
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14. VOST Detection Limits 

   
NONT,

French Test Name :

Test Code : VOCVOSTM-A AIR

Spanish Test Name :

Description :

Instrument :

Result Unit :

Storage Temp :

Preservation Code :

Default Report On ? :

Current :

English Method :

French Method :

Spanish Method :

Test Sig. Digits :

DL Sig. Digits :

Linked Tests :

Test Location :

Matrix Code :

SubMatrix Code :

Location Code :

Report Group Code :

Detector :

Parameter Group :

Analysis Time :

Department No :

Product Code :

Reference Number :

Aliquot Volume :

VOST Analysis (5041mod)

Analyse VOST (5041mod)

VOST Analysis (5041mod)

VOST Analysis

GC

ug

4

YES

Yes

EPA 5041mod(M0030)

EPA 5041mod(M0030)

EPA 5041mod(M0030)

3

2

BRL SOP-00302

VOLAIR

4014

14

VOL

MS

VOC

NONT

English Test Name :

Calculation Block : NO

Test Group : VOLVOS

Price Bin # : 1 _______________________________________ 330.00

List of Parameters

Code Parameter Description Rpt. Def. Prm. Grp. Rpt. Ord. Instr. RDL IDL

Ord.

BASEN8 Hexachlorobutadiene NO BN 105 0 0

CB1 Chlorobenzene YES CB 35 0.011 0

CB2 1,3-Dichlorobenzene YES CB 44 0.02 0

CB3 1,4-Dichlorobenzene YES CB 45 0.02 0

CB4 1,2-Dichlorobenzene YES CB 46 0.02 0

CB41 1,2-Dichlorotetrafluoroethane NO CB 103 0 0

CB6 1,2,4-Trichlorobenzene NO CB 104 0 0

HAL 43 Iodomethane YES VOL 9 0.015 0

HAL1 Chloromethane YES VOL 2 0.015

HAL10 cis-1,2-Dichloroethylene YES VOL 15 0.01 0

HAL11 Chloroform YES VOL 16 0.011

HAL12 1,1,1-Trichloroethane YES VOL 19 0.014 0

HAL14 Carbon Tetrachloride YES VOL 20 0.016 0

HAL15 1,2-Dichloroethane YES VOL 17 0.007 0

HAL16 Trichloroethylene YES VOL 24 0.011 0

HAL17 1,2-Dichloropropane YES VOL 23 0.011 0

HAL18 Bromodichloromethane YES VOL 26 0.011 0

HAL2 Vinyl Chloride YES VOL 3 0.013 0

HAL20 cis-1,3-Dichloropropene YES VOL 27 0.01 0

HAL21 trans-1,3-Dichloropropene YES VOL 28 0.007 0

Page 1 of 2

VOST Reporting Limits - RDL in microgram/mL Page 53 of 66
HAL22 1,1,2-Trichloroethane YES VOL 22 0.016 0

HAL23 Tetrachloroethylene YES VOL 34 0.018 0

HAL24 Dibromochloromethane YES VOL 29 0.009 0

HAL26 Bromoform YES VOL 41 0.014 0

HAL27 1,1,2,2-Tetrachloroethane YES VOL 42 0.014 0

HAL28 Dichlorodifluoromethane (FREON 12) YES VOL 1 0.02 0

HAL3 Bromomethane YES VOL 4 0.015 0

HAL4 Chloroethane YES VOL 5 0.009 0

HAL5 Trichlorofluoromethane (FREON 11) YES VOL 6 0.01 0

HAL6 1,1-Dichloroethylene YES VOL 8 0.011 0

HAL7 Methylene Chloride(Dichloromethane) YES VOL 11 0.019 0

HAL8 trans-1,2-Dichloroethylene YES VOL 14 0.01 0

HAL9 1,1-Dichloroethane YES VOL 12 0.012 0

MAH 16 m / p-Xylene YES VOL 38 0.015 0

MAH1 Benzene YES VOL 21 0.009 0

MAH2 Toluene YES VOL 32 0.014 0

MAH3 Ethylbenzene YES VOL 37 0.014 0

MAH4 o-Xylene YES VOL 40 0.015 0

MAH7 Styrene YES VOL 39 0.012 0

VOL1 Acetone (2-Propanone) YES VOL 7 0.045 0

VOL3 Carbon Disulfide YES VOL 10 0.026 0

VOL41 1,2,4-Trimethylbenzene NO VOL 102 0 0

VOL57 1,3,5-Trimethylbenzene NO VOL 101 0 0

VOL6 Methyl Isobutyl Ketone YES VOL 30 0.019 0

VOL60 Methyl Butyl Ketone (2-Hexanone) YES VOL 31 0.031 0

VOL62 Ethylene Dibromide YES VOL 33 0.01 0

VOL67 Trichlorotrifluoroethane NO VOL 100 0 0

VOL7 Methyl Ethyl Ketone (2-Butanone) YES VOL 18 0.036 0

VOL59 Vinyl Acetate NO VOL 13 0.015 0

VOL35 Dibromomethane YES VOL 25 0.01 0

VOL29 1,1,1,2-Tetrachloroethane YES VOL 36 0.01 0

VOL31 1,2,3-Trichloropropane YES VOL 43 0.015 0

MAH12 Acrylonitrile NO VOL 90 90 0.025 0

CLPRENE Chloroprene NO VOL 91 91 0.025 0

List of Surrogates

Code Surrogate Description MDL Criteria "A"

D4-CL2ETH2 D4-1,2-Dichloroethane D4-CL2ETH2 D4-CL2ETH2

D8-TOL D8-Toluene D8-TOL D8-TOL

BROMOF Bromofluorobenzene BROMOF BROMOF

D10-ETHY2 D10-Ethylbenzene (FS) D10-ETHY2 D10-ETHY2

List of Spikes

Code

MVOCB

Page 2 of 2

VOST Reporting Limits - RDL in microgram/mL Page 54 of 66
H

Test Code : VOCCOND-W

English Test Name : VOST Condensate (8260Cmod)

Description : Determination of volatile aromatic and

halogenated organics in liquid by purge

and trap GC/MS.

Result Units : ug/L

Reference Number : BRL SOP-00305

List of Parameters

Code Parameter Description RDL

HAL28 Dichlorodifluoromethane (FREON 12) 1

HAL1 Chloromethane 2

HAL2 Vinyl Chloride 0.4

HAL3 Bromomethane 3

HAL4 Chloroethane 1

HAL5 Trichlorofluoromethane (FREON 11) 2

VOL1 Acetone (2-Propanone) 15

HAL6 1,1-Dichloroethylene 0.5

HAL 43 Iodomethane 0.6

VOL3 Carbon Disulfide 0.5

HAL7 Methylene Chloride(Dichloromethane) 1

HAL9 1,1-Dichloroethane 0.4

VOL59 Vinyl Acetate 1.5

HAL8 trans-1,2-Dichloroethylene 1

HAL10 cis-1,2-Dichloroethylene 1

HAL11 Chloroform 0.4

HAL15 1,2-Dichloroethane 0.5

VOL7 Methyl Ethyl Ketone (2-Butanone) 10

HAL12 1,1,1-Trichloroethane 0.5

HAL14 Carbon Tetrachloride 0.5

MAH1 Benzene 0.5

HAL22 1,1,2-Trichloroethane 0.5

HAL17 1,2-Dichloropropane 0.5

HAL16 Trichloroethylene 0.5

VOL35 Dibromomethane 0.5

HAL18 Bromodichloromethane 0.4

HAL20 cis-1,3-Dichloropropene 0.4

HAL21 trans-1,3-Dichloropropene 0.6

HAL24 Dibromochloromethane 0.4

VOL6 Methyl Isobutyl Ketone 10

VOL60 Methyl Butyl Ketone (2-Hexanone) 10

MAH2 Toluene 0.5

VOL62 Ethylene Dibromide 0.5

HAL23 Tetrachloroethylene 0.5

CB1 Chlorobenzene 0.5

VOL29 1,1,1,2-Tetrachloroethane 0.5

MAH3 Ethylbenzene 0.5

MAH13 p+m-Xylene 0.5

MAH7 Styrene 0.5

MAH4 o-Xylene 0.5

HAL26 Bromoform 0.4

HAL27 1,1,2,2-Tetrachloroethane 1

VOL31 1,2,3-Trichloropropane 0.6

CB2 1,3-Dichlorobenzene 0.5

CB3 1,4-Dichlorobenzene 0.5

CB4 1,2-Dichlorobenzene 0.5

List of Surrogates

Code Surrogate Description

D4-CL2ET D4-1,2-Dichloroethane

D8-TOL D8-Toluene

BFB 4-Bromofluorobenzene

VOST Reporting Limits - RDL in microgram/mL Page 55 of 66
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Appendix A - EPA ICR Letter – May 15, 2014 

   
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Appendix B - July 14, 2014 EPA Email Regarding PCB Testing 

   
1

Myers, Jason

To: Thomas Andersen; Fritz, Wesley; Tim Gilder; James Bell; Atsushi Eguchi; Tadayoshi 

Hiyama; David Blye; David Wise; David Gratson

Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents

To PVC MACT Working Group:

Per Jodi Howard’s reply below, PCB testing is not required for the 2014 PVC Process Vent Section 114 Request.  I have

asked her to clarify that same requirement for the PVC MACT compliance performance test.  I will keep you informed on

her reply.

Regards,

Rich

Richard Krock

Technical Director

 

The Vinyl Institute

1737 King Street Suite 390

Alexandria, VA 22314

Direct: 571.970.3392

Mobile: 571.216.4474

Fax: 571.970.3271

Email: rkrock@vinylinfo.org

http://www.vinylinfo.org

http://www.vinylindesign.com

 

 

From: Richard Krock 

Sent: Monday, July 14, 2014 5:22 PM 

To: 'Howard, Jodi'; Bouchard, Andrew 

Cc: Lassiter, Penny; Kataoka, Mark; JC Walker 

Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents 

Dear Ms. Howard,

Thank you for the quick response on the  2014 PVC Process Vent Section 114 Request.    Does this same answer

apply for those companies seeking to use this S114 test as their compliance performance test for the PVC

MACT?  Again, thank you for the clarification.

From: Howard, Jodi [mailto:Howard.Jodi@epa.gov] 

Sent: Monday, July 14, 2014 3:09 PM 

To: Richard Krock; Bouchard, Andrew 

Page 61 of 66
2

Cc: Lassiter, Penny; Kataoka, Mark; JC Walker 

Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents 

Mr. Krock,

Testing for polychlorinated biphenyls is not required for the 2014 PVC process vent 114.

Thanks.  

From: Richard Krock [mailto:rkrock@vinylinfo.org]  

Sent: Monday, July 14, 2014 11:46 AM

To: Bouchard, Andrew; Howard, Jodi

Cc: Lassiter, Penny; Kataoka, Mark; JC Walker

Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents

Dear Mr. Bouchard,

Thank you for the responses to our earlier questions on the S114 for Process Vents.  We have an

additional clarification regarding PCB testing as explained in the attached letter.  Your quick response is

needed and will be highly appreciated.  Please do not hesitate to contact me with any questions on this

matter.

Thank you.

Richard Krock

Technical Director

 

The Vinyl Institute

1737 King Street Suite 390

Alexandria, VA 22314

Direct: 571.970.3392

Mobile: 571.216.4474

Fax: 571.970.3271

Email: rkrock@vinylinfo.org

http://www.vinylinfo.org

http://www.vinylindesign.com

 

 

From: Bouchard, Andrew [mailto:Bouchard.Andrew@epa.gov] 

Sent: Friday, July 11, 2014 3:44 PM 

To: Richard Krock; Howard, Jodi 

Cc: Lassiter, Penny; Kataoka, Mark; JC Walker 

Subject: RE: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents 

Mr. Krock,

Page 62 of 66
3

Per the email below, attached you will find a consolidated Q&A document consisting of all the

questions VI has raised on EPA’s CAA Section 114 request related to the Excel surveys &

instructions, process wastewater and/or resin sampling, and process vent testing. Again, I’d just

like to note that if any facility has site specific issues on how to comply with our CAA section 114

request, they should contact us directly. Thanks.

___________________________________ 

Andrew Bouchard 

Environmental Engineer 

U.S. Environmental Protection Agency 

OAR/OAQPS/SPPD/RCG 

Phone: (919) 541-4036 

Fax: (919) 541-0246 

Bouchard.Andrew@epa.gov

From: Bouchard, Andrew  

Sent: Tuesday, July 01, 2014 4:17 PM

To: 'Richard Krock'; Howard, Jodi

Cc: Lassiter, Penny; Kataoka, Mark; JC Walker

Subject: RE: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents

Mr. Krock,

We are in the process of putting together a consolidated Q&A document consisting of all the

questions VI has raised on EPA’s CAA Section 114 request related to the Excel surveys &

instructions, process wastewater and/or resin sampling, and process vent testing. Portions of

VI’s specific questions related specifically to the process wastewater and/or resin sampling have

already been responded to (see email from May 22, these answers will be consolidated into the

Q&A document for ease and consistency) and EPA is expecting responses from those facilities

asked to provide us with this data by July 31, 2014. We anticipate responding to the remaining

issues raised by VI in the aforementioned consolidated Q&A document by no later than next

week. Thanks for your patience and hope you all have a happy fourth of July weekend!

___________________________________ 

Andrew Bouchard 

Environmental Engineer 

U.S. Environmental Protection Agency 

OAR/OAQPS/SPPD/RCG 

Phone: (919) 541-4036 

Fax: (919) 541-0246 

Bouchard.Andrew@epa.gov

From: Richard Krock [mailto:rkrock@vinylinfo.org]  

Sent: Tuesday, July 01, 2014 2:22 PM

To: Howard, Jodi; Bouchard, Andrew

Cc: Lassiter, Penny; Kataoka, Mark; JC Walker

Subject: RE: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents

Dear Ms. Howard and Mr. Bouchard:

Could you provide a status update on the response requested in the e‐mail below?   Thank you.

Page 63 of 66
4

Richard Krock

Technical Director

 

The Vinyl Institute

1737 King Street Suite 390

Alexandria, VA 22314

Direct: 571.970.3392

Mobile: 571.216.4474

Fax: 571.970.3271

Email: rkrock@vinylinfo.org

http://www.vinylinfo.org

http://www.vinylindesign.com

 

 

From: Richard Krock 

Sent: Friday, June 13, 2014 4:35 PM 

To: Howard, Jodi (Howard.Jodi@epa.gov); Bouchard, Andrew 

(Bouchard.Andrew@epa.gov) 

Cc: Penny Lassiter (lassiter.penny@epa.gov); Kataoka, Mark (Kataoka.Mark@epa.gov); 

JC Walker 

Subject: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents 

Dear Ms. Howard and Mr. Bouchard:

The Vinyl Institute’s PVC MACT Subgroup on Process Vents has raised questions

regarding EPA’s May 15, 2014 Section 114 Request for PVC producer’s Process

Vents.  The Subgroup’s questions are contained in the attached letter.  The Vinyl

Institute appreciates the Agency’s time to review the questions and look forward to

your response.  Please do not hesitate to contact me with any questions in this regard.

Thank you.

Richard Krock

Technical Director

 

The Vinyl Institute

1737 King Street Suite 390

Alexandria, VA 22314

Direct: 571.970.3392

Mobile: 571.216.4474

Fax: 571.970.3271

Email: rkrock@vinylinfo.org

http://www.vinylinfo.org

http://www.vinylindesign.com

 

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Appendix C - Enclosure 1, Attachment B and C 
Enclosure 1 

PVC Section 114 Enclosure 1 – Page 1 

05/15/2014 

MAXIMUM ACHIEVABLE CONTROL TECHNOLOGY (MACT) STANDARDS 

DEVELOPMENT INFORMATION COLLECTION REQUEST 

I. Introduction 

Under the authority of Section 114 of the Clean Air Act, this information collection request 

is to be completed for operations that comprise the Polyvinyl Chloride and Copolymers (PVC) 

source category at your company. The PVC Production source category includes any facility which 

manufactures polymerized vinyl chloride. PVC is be produced by the suspension, suspension 

blending, emulsion/dispersion or bulk processes, although other methods may be used. The source 

category includes the collection of all equipment and activities necessary to produce PVC 

homopolymer or copolymer resin. 

This information collection request consists of two parts: (1) completion of information 

collection request response forms (survey) and submission of supplemental data and information; 

and (2) testing and analysis of emissions from PVC process vents (i.e., at the outlet of the final 

control device). The results of testing are reported in either the Electronic Reporting Tool (ERT) 

or in dedicated worksheets that are contained in a single Microsoft Excel workbook file along 

with the required response forms. Except for the required testing, complete this information 

collection request as completely as possible from best available existing information from the 

2013 calendar year. 

Instructions for obtaining the information collection request response forms are in 

Section II of this enclosure. A summary of the supplemental data and information requested in 

this information collection request is in Section III. Instructions for submitting your response are 

in Section IV. Section V contains general instructions for completing your response and includes 

specific guidance for completing each response form. For your convenience, we have provided 

additional information on the scope and purpose of this information collection request, as well as 

useful definitions, in Attachment A. Respondents should read this material before attempting to 

complete the response forms. Respondents may also wish to review the rule and implementation 

information for PVC production before completing the response forms by visiting the EPA’s 

Technology Transfer Network – Air Toxics Web Site for PVC: 

http://www.epa.gov/ttn/atw/pvc/pvcpg.html 

Additional information on the PVC process vent testing and analysis requirements can be 

found in Attachment B of this enclosure. Information regarding how to calculate and report 

method detection levels in located in Attachment C of this enclosure. 

If you have questions regarding this request, please contact Ms. Jodi Howard, Refining 

and Chemicals Group, at (919) 541-4607 or howard.jodi@epa.gov.

Appendix C Page 1
Enclosure 1 

PVC Section 114 Enclosure 1 – Page 2 

05/15/2014 

II. Instructions for Obtaining the Information Collection Request Files

The information collection request response forms are available as a single Microsoft 

Excel 2007 workbook. The workbook is included with this enclosure and is titled: 

“2014 PVC 114 PV Testing.xlsx”

The workbook should be completed for the entire PVC production facility. Before 

submitting the file, the file name will be changed to reflect the actual company and facility (see

Section III). 

Other files included in this package are an example of how to complete the Excel 

workbook and a copy of this enclosure. Where necessary, examples of how to complete selected 

portions of the information collection request response forms are included directly in the forms 

themselves. Refer to examples and the instructions contained in this enclosure when completing 

your response. 

III. Supplemental Data and Information Requested 

We are requesting you submit supplemental data and information to support the 

information submitted in the information collection request response forms. The following table 

summarizes the supplemental data and information that must be submitted with your response. 

Provide actual recorded data where possible and submit that data in Microsoft Excel format. If 

recorded process data (such as CEMS data) are not available, then provide estimates based on 

engineering assessments, material balances, etc. and provide copies of estimation worksheets and 

other supporting documentation. Recorded process data, sampling results, test results, estimation 

worksheets, engineering calculations, assessments, etc. must be provided to support the 

information submitted for all parts of the information collection request response. 

Except for the results of PVC process vent testing, the information provided in response 

to this information collection request should be from the best available existing information from 

the 2013 calendar year. 

Supplemental Data and 

Information

Related Equipment, 

Stream, Emission Point Time Period

Process Unit Plot Plan Process Unit N/A

Process Unit Flow Diagram Process Unit N/A

HAP/Total VOC Concentration, 

Emissions Data or Estimates All Uncontrolled Emission Points 2013

Safety/Pressure Relief Notifications

and estimates of emissions from 

releases

Process Unit Safety/Pressure Relief 

Devices 2013

Appendix C Page 2
Enclosure 1 

PVC Section 114 Enclosure 1 – Page 3 

05/15/2014 

IV. Instructions for Submitting Your Information Collection Request Response

Use the appropriate file naming format as listed below for the files you submit when 

responding to this information collection request: 

Submission File Name Format

Completed Response 

Workbook 2014 PVC 114 PV Testing.xlsx

Plot Plan [Company]_[Facility] _PlotPlan

Process Flow Diagram [Company]_[Facility] _PFD

Data/Estimates

[Company]_[Facility]_[ProcessUnitID]_[ProcessVent/EmissionPoint/Stream/Waste

waterStream/ProcessEquipment/ControlEquipment 

ID]_[YYYYMMDD]to[YYYYMMDD]

For file names that include dates or date ranges, use four digits for the year (YYYY), two digits 

for the month (MM), and two digits for the day (DD). 

EXAMPLE 

Generic Chemical Corporation has a manufacturing facility in Anytown, USA 

According to the instructions in Section II and IV, the files would be renamed as: 

Submission File Name

Completed Response Workbook PVCICR_Generic_Anytown.xls

and submitted with all other required data and information outlined Section III. 

All recipients must perform the requested stack testing and submit the test results, 

reports, and documentation along with the responses to the information collection request and 

supplemental data and information specified in Attachments A, B and C of Enclosure 1 no later 

than November 17, 2014. Any submissions made after this date will be in violation of this 

Section 114 request. 

Please e-mail the completed non-confidential response to: 

CCG-PVC@epa.gov

If you are submitting confidential business information (CBI) as described in 

Enclosure 2, then this information must be mailed to EPA in hard-copy or on a CD-ROM or 

DVD-ROM disk. Clearly mark the disk and/or the materials with the words “Confidential 

Appendix C Page 3
Enclosure 1 

PVC Section 114 Enclosure 1 – Page 4 

05/15/2014 

Business Information” and send either via U.S. Postal Service Express Mail, registered mail, or 

private courier to: 

Jodi Howard 

U.S. EPA Office of Air Quality Planning and Standards 

Sector Policies and Program Division, Refining and Chemicals Group 

Mail Code E143-01

Research Triangle Park, NC 27711 

 Additionally, if you are submitting CBI via mail in hard-copy or on CD-ROM or DVDROM disk, you must also submit a non-CBI version of your information collection request 

response to the email address listed above. DO NOT ELECTRONICALLY TRANSMIT 

CONFIDENTIAL BUSINESS INFORMATION TO EPA. 

If you have questions regarding this request, please contact Ms. Jodi Howard, Refining 

and Chemicals Group, at (919) 541-4607 or howard.jodi@epa.gov. 

V. Background Information and Instructions for Completing the Information 

Collection Request Response Forms 

NOTE: For the purposes of this information collection request, all HAP and VOC 

concentrations and emissions are to be quantified. Do not report concentrations or 

emissions as “trace” or “minimal.” If a concentration is at or below a detection 

limit, then provide the detection limit. 

Form A – Company Information and Facility Information 

 Forms A-1 and A-2 are where the respondent company and facilities are identified. 

 In question I.1 of Form A-1, identify the legal parent company/legal corporate owner name. 

In questions I.2 through I.6 provide the mailing address for the legal parent company/legal 

corporate owner. 

 Identify the size of the company by selecting the appropriate range for the number of 

employees (including all subsidiaries, branches, and related establishments owned) in 

question I.7. 

 On Form A-2, provide the facility name and address information requested in question II.1, 

including the latitudinal and longitudinal coordinates of the facility. Facility latitudes and 

longitudes should be reported in decimal degrees to the 5th decimal place, and longitudes 

should include negative sign, e.g. (37.91986, -87.32724) Sources of these data include EPA 

permits (e.g., NPDES permits), county property records, facility blueprints, and site plans. 

 Provide the name and contact information for the facility’s technical contact in questions 

III.1 through III.3 on Form A-2.

 On Form A-2, Section IV, respondents are asked to identify whether the facility is a major 

source of HAP emissions by selecting “Yes,” or “No,” in question IV.1. Section 112(a)(1) of 

the CAA defines a major source as any stationary source or group of stationary sources 

located within a contiguous area and under common control that emits or has the potential to 

Appendix C Page 4
Enclosure 1 

PVC Section 114 Enclosure 1 – Page 5 

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emit considering controls, in the aggregate, 10 tons per year or more of any hazardous air 

pollutant or 25 tons per year or more of any combination of hazardous air pollutants. 

Affected sources that have not yet commenced production of PVC resin or that are expanding 

existing production capacity are asked to complete all parts of this information collection 

request. For those sources, projected actual emissions (not “Potential to Emit”) are requested 

in lieu of actual operating emissions. 

 For facilities that are not major sources of HAP emissions (and select “No” for question 

IV.1), the respondent is asked to identify if and when a permit limit for their potential HAP 

emissions to avoid being classified as a major source in questions IV.2 and IV.3, respectively 

was taken. 

 Indicate if the facility manufactures other products in addition to PVC resin by selecting 

“Yes,” or “No,” for question IV.4 on Form A-2. If “Yes,” list the other products 

manufactured in the response field for question IV.5. 

 Indicate if there are any HAP emission associated with any co-located facilities by selecting 

“Yes,” or “No,” for question IV.6 on Form A-2. 

Form B – Control Devices, Recovery Systems, and Process Equipment 

 Prior to completing the remainder of the forms (i.e., forms B through N), you should 

complete a plot plan (plant layout schematic) and process flow diagram(s) for the PVC 

production facility. Do not submit “block flow diagrams.” The level of detail requested is 

more than generally contained in “block flow” diagrams but less than that generally 

contained in piping and instrumentation diagrams (P&IDs). Process flow diagrams should 

accurately show ALL: 

o Process equipment; 

o Recovery systems including all recovery equipment; 

o Process wastewater treatment systems including all wastewater treatment 

equipment; 

o Closed vent systems (identify the collection of piping for each closed vent system 

using a dotted-line boundary on the process flow diagram);

o Control devices (also clearly show any piping configurations that allow a gaseous 

stream routed to a closed vent system and control device to bypass the control 

device);

o Pressure relief devices (PRDs); and

o Emission points; 

Appendix C Page 5
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PVC Section 114 Enclosure 1 – Page 6 

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 Each item in the table below is to be given a unique identifier in the form of Z-x, where “Z” 

is a unique code for each item listed in the table below and x = 1, 2, 3,...n. The unique 

identifier should exactly match between the process flow diagram and information provided 

in the completed response workbook(s). Refer to Attachment A of this Enclosure for relevant 

definitions. 

Control devices (C-x)

Recovery systems (RS-x)

Individual recovery equipment that comprise the recovery system (RE-x)

Individual wastewater treatment equipment that comprise each process 

wastewater treatment system

(WWE-x)

Process equipment (U-x)

Emission points (EP-x)

Pressure relief devices (PRD-x)

Closed vent systems (CVS-x)

Form B-1 – Control Devices 

General Instructions 

 Each control device should be listed in Form B-1. 

 For the purposes of this information collection request, wastewater collection, handling and 

treatment equipment (including process wastewater steam strippers) are considered 

wastewater treatment equipment and not control or recovery devices. 

 For each control device, submit a copy of the most recent emissions test report. The report 

should include information on the process operations that influenced emissions during the 

test, including the resin type being produced. Include information such as the purpose of the 

test, when it was conducted and what test methods were used. If emissions test reports are not 

available, calculations based on emission factors, material balances, or engineering principles 

must be submitted and supported by submitting a step-by-step description of the calculations, 

including assumptions used and a brief rationale for the validity of the calculation method 

used. (See guidance documents listed in Attachment A, Section IV). 

 For the following control devices, complete the appropriate Forms: absorbers - Form F-1; 

thermal or catalytic oxidizers - Form F-2; and, condensers - Form F-3. 

Specific Instructions by Form Column 

 Column 1: Each control device is to be given a unique code or identifier in the form of C-x, 

where x = 1, 2, 3,...n, in Form B-1. This unique code/identifier should exactly match the 

identifier used in the process flow diagram and will be used on subsequent forms. 

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PVC Section 114 Enclosure 1 – Page 7 

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 Column 2: Select the type of control device from the list provided in the Form. 

 Column 3: If “other” was selected in column 2, provide a description of the control device. 

 Column 4: Each emission point from a control device (or from the last control device in a 

series) that exhausts directly to the atmosphere should be shown on the process flow diagram 

and is to be given a unique code or identifier of the form EP-x, where x = 1,2,3,...n in Form 

B-1. This unique code/identifier will be used on subsequent forms. If the exhaust stream from 

the control device immediately enters a subsequent control device (e.g., exhaust from a 

thermal oxidizer is routed to an acid gas scrubber) provide the subsequent control device 

identifier instead of the emission point identifier. 

Form B-2 – Recovery Systems and Closed Vent Systems 

General Instructions 

 Each recovery system should be listed in Form B-2.

 For the purposes of this information collection request, wastewater collection, handling and 

treatment equipment (including process wastewater steam strippers), are considered 

wastewater treatment equipment and not control or recovery systems. 

 If you use a condenser as part of a recovery system, and emissions from the condenser are 

routed directly to the atmosphere without first passing through a control device, complete 

Form F-3 for the condenser(s). 

Specific Instructions by Form Column 

Table 1 

 Column 1: Each recovery system is to be given a unique code or identifier in the form of RSx, where x = 1, 2, 3,...n, in Form B-2. This unique code/identifier should exactly match the 

identifier used in the process flow diagram and will be used on subsequent forms. 

 Column 2: Provide a description of the recovery system. 

 Column 3: Indicate if, at any point in the recovery or closed vent system, emissions can be 

discharged directly to the atmosphere. If you answer yes, complete Table 2. 

 Columns 4-6: List the control devices that control emissions from the recovery and closed 

vent system. The control device ID(s) that you provided on Form B-1 will be available as a 

pick list in columns 4 through 6. 

Table 2 

 If you answered “Yes” in column 3 of Table 1, complete Table 2. 

 Column 1: Identify the recovery system ID. The recovery system ID(s) that you provided in 

Table 1 will be available as a pick list in column 1 of Table 2. 

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PVC Section 114 Enclosure 1 – Page 8 

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 Column 2: Identify each emission point that discharges directly to the atmosphere. Do not list 

emission points for streams exiting the recovery system that are routed through a closed vent 

system to a control device. Each emission point that exhausts directly to the atmosphere 

should be shown on the process flow diagram and given a unique code or identifier of the 

form EP-x, where x = 1,2,3,...n in Form B-2. This unique code/identifier will be used on 

subsequent forms. 

 Column 3: Identify if the emission point is used as a bypass for the control device, or, if the 

emission point is a process vent.

 Column 4: Indicate if the equipment opening standards in 40 CFR Part 61, subpart F are met 

before a discharge occurs through the emission point. 

Table 3 

 Column 1: Each piece of recovery equipment included in the recovery system should be 

shown on the process flow diagram and given a unique code or identifier of the form RE-x, 

where x = 1, 2, 3,...n, in Table 2 of Form B-2. This unique code/identifier will be used on 

subsequent forms. 

 Column 2: Provide a description of the recovery equipment. 

 Column 3: Indicate recovery system ID to which the recovery equipment belongs. The 

recovery system ID(s) you provided in Table 1 will be available as a pick list in column 3. 

Form B-4 – Process Equipment 

General Instructions 

 All remaining process equipment should be listed on Form B-4. Do not list any equipment 

previously noted on Forms B-1 through B-2. 

 Process equipment may be grouped on the process flow diagram if and only if the individual 

pieces of equipment in the group are of identical design and all process vents exiting each 

piece of process equipment are routed to the same control device. 

 If emissions from a condenser (not previously listed as part of a recovery system) are routed 

directly to the atmosphere without first passing through a recovery system or control device, 

complete Form F-3 for the condenser(s). 

Specific Instructions by Form Column 

 Column 1: Each piece of process equipment is to be given a unique code or identifier in the 

form of U-x, where x = 1, 2, 3,...n, in Form B-4. This unique code/identifier should exactly 

match the identifier used in the process flow diagram and will be used on subsequent forms. 

 Column 2: Provide a description of the process equipment. 

 Column 3: Provide an indication if emissions from the process equipment are routed directly 

to the atmosphere without passing first through a recovery system or control device. 

Appendix C Page 8
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PVC Section 114 Enclosure 1 – Page 9 

05/15/2014 

 Column 4-6: If you answered “Yes” in column 3, list the emission point ID(s). Each emission 

point should be shown on the process flow diagram and is to be given a unique code or 

identifier of the form EP-x, where x = 1,2,3,...n in Form B-4. This unique code/identifier 

will be used on subsequent forms. If the emission point is controlled (and therefore listed in 

Form B-1) do not duplicate the emission point in Form B-4; only list uncontrolled emission 

points. 

 Column 7: If you answered “No” in column 3, indicate if emissions from the process 

equipment are routed to a recovery system. 

 Column 8: If you answered “Yes” in column 7, select the appropriate recovery system ID 

entered on Form B-2.

 Column 9-11: If you answered “No” in column 7, list the control device identifiers 

previously identified on Form B-1. If emissions are controlled by multiple control devices, 

list each control device identifier in the order of control (e.g., the overhead stream from a 

resin stripper (U-1) is controlled by 1) a thermal oxidizer (C-1) and an acid gas scrubber (C2)). 

Form F – Control Devices 

General Instruction 

 Complete Form F-1 for each absorber used as a control device, or for any absorber that emits 

directly to the atmosphere. 

 Complete Form F-2 for each thermal or catalytic oxidizer. 

 Complete Form F-3 for each condenser used as a control device or for any condenser that 

emits directly to the atmosphere. 

Specific Instructions by Form Row 

Form F-1

 Rows 1-2: Select the type of equipment (i.e., control device, recovery equipment or process 

equipment). Then in row 2, select the equipment ID you entered into the corresponding Form 

B.

 Rows 3-4: Select the type of absorber from the pick list. If “other,” provide a description of 

the absorber type in row 4. 

 Rows 5-14: Provide the operating characteristics of the absorber in rows 5 through 14. 

Provide as much of the information as possible. 

 Rows 15-16: Indicate the year the equipment was installed and cite any applicable 

regulations. 

Form F-2

 Row 1: Select the control device ID (based on the values you entered in Form B-1). 

Appendix C Page 9
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PVC Section 114 Enclosure 1 – Page 10

05/15/2014 

 Rows 2-3: Provide the number of operating hours per year and indicate if the device is 

considered emergency equipment. 

 Row 5: Indicate the type of oxidizer (i.e., thermal or catalytic). 

 Rows 6-35: Provide the design parameters and operating characteristics requested in rows 6 

through 35. Complete as much of the information as possible for each oxidizer.

 Rows 36-37: Indicate the year the equipment was installed and cite any applicable 

regulations. 

Form F-3

 Rows 1-2: Select the type of equipment (i.e., control device, recovery equipment, or process 

equipment). Then in row 2, select the equipment ID you entered into the corresponding Form 

B.

 Rows 3-4: Select the type of condenser from the pick list. If “other,” provide a description of 

the condenser type in row 4. 

 Rows 5-12: Provide the operating characteristics of the condenser in rows 5 through 12. 

Provide as much of the information as possible. 

 Rows 15-16: Indicate the year the equipment was installed, and cite any applicable 

regulations. 

Form H – Equipment Leaks 

 Complete Form H for equipment leaks at the PVC production facility. 

 Provide information regarding your facility’s leak detection and repair (LDAR) program in 

Table 1. 

 In Table 2, provide equipment counts for all equipment at your facility in the source 

category. In addition, provide the subtotal of the equipment that are associated with your 

closed vent system(s). 

 In addition to completing Form H, submit a copy of the leak detection and repair procedures 

for the facility.

Form I – Equipment Opening 

Table 1 

 Complete this Form for each piece of process equipment, recovery equipment and any 

additional equipment that is not assigned an equipment ID (e.g., in-line filters). 

 Complete a separate Form I for each piece of process equipment, recovery equipment or 

other equipment that was opened in 2013. Identify the equipment (by selecting the recovery 

or process equipment ID from Forms B-2 or B-4 if applicable). Indicate the number of times 

the equipment was opened during 2013 and the reasons for opening the equipment (list all 

that apply). Provide the equipment volume in cubic meters. 

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PVC Section 114 Enclosure 1 – Page 11

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 Indicate how the HAP concentration of the equipment is determined, and how (if at all) HAP 

emissions are controlled. 

Table 2 

 In Table 2, list the individual HAP present in the equipment and the concentration of each 

HAP at the equipment opening. 

 Provide the total mass of each HAP emitted from opening the equipment in 2013, and a basis 

for the emissions values. Values should be reported for normal operations; not for startups, 

shutdowns, or malfunctions. 

 Provide copies of estimation worksheets and any other relevant documentation. 

Form K-1 – Tanks, Vessels, and Portable Containers Used for Feedstock Storage, Product 

Storage, Vent Gas Storage, Holding, and Wastewater 

 Complete a separate Form K-1 for each tank, vessel portable container used for feedstock 

storage, product storage, holding and wastewater, including surge control vessels that are 

used to hold process vent gas prior to the control device for 2013 only. Do not include gas 

holders on Form K-1 (refer to Attachment A, Section V of this Enclosure for the definition of 

a gas holder). 

 In Table 1, identify the process equipment by selecting the equipment ID provided on Form 

B-2 or Form B-4 (if applicable). If the equipment was not identified on Form B-2 or B-4, 

provide an equipment description. 

 Provide a detailed description of the equipment, and include (if applicable) if the tank is a 

fixed, floating internal, or floating external roof. 

 Select the purpose of the equipment from the pick list provided. If none of the options on the 

pick list accurately describe the purpose of the equipment, please select “Other” and specify 

the purpose in the next row. 

 Indicate the number of turnovers for 2013, the equipment volume and the average storage 

temperature. 

 Indicate how the HAP concentration of emissions from the tank/vessel/container are 

determined and if HAP emissions are controlled, identify the method of control. 

 In Table 2, indicate the individual HAP contained in the tank/vessel/portable container and 

the corresponding vapor pressure. Provide concentration values and total emissions for 2013. 

 Provide copies of estimation worksheets and any other relevant documentation. 

Form L – Startup, Shutdown and Malfunction 

 Complete Form L for startups, shutdowns and malfunctions during 2013 as completely as 

possible. 

 Each column in Form L represents a single startup, shutdown or malfunction event. Provide 

emissions in total pounds for the event. 

Appendix C Page 11
Enclosure 1 

PVC Section 114 Enclosure 1 – Page 12

05/15/2014 

 Submit with your response to this information collection request, copies of all records of 

emissions during periods of process startup, shutdown and malfunctions for 2013.

Form P – Process Vent Emissions Testing Data 

 Form P is used to collect results of performance tests that are not supported by the EPA’s 

Electronic Reporting Tool (ERT). Refer to Attachment B to this Enclosure 1, Summary of 

Test Procedures, Methods, and Reporting Requirements for Polyvinyl Chloride and 

Copolymers Facility Emission Points for more information for additional information. 

 Copy Form P as necessary for pollutants/compounds sampled on different dates. 

 For multiple control devices, users may copy Form P within the response workbook. 

 For each test run, provide the required operating parameters collected during the test. Note 

the selection for “PVC Production Rate Units.” If your final product is sold and shipped dried 

(e.g., a suspension resin), select “dry lbs PVC/day.” If your final product is sold and shipped 

without being dried (e.g., an emulsion resin), select “total lbs PVC/day.”

 Provide a numerical result for each compound. Do not provide non-numerical data in the 

compound results columns. 

 In the “Run # Detection” columns, identify the status of the measured values relative to 

detection levels following the instructions in Attachment C to this Enclosure 1, “Guidance 

for Calculating and Reporting Values Measured Below Method Detection Levels.”

Form Q – Total Hydrocarbon 30-Day Monitoring 

 Form Q is used to collect the results of the 30-day, continuous total hydrocarbon (THC) and 

methane (CH4) monitoring required in Section 1.3 of Attachment B to this Enclosure 1, 

Summary of Test Procedures, Methods, and Reporting Requirements for Polyvinyl Chloride 

and Copolymers Facility Emission Points. 

 For multiple control devices, users may copy Form Q within the response workbook. 

 Along with the continuous 30-day THC and CH4 readings, provide the corresponding oxygen 

and moisture values, along with the PVC type and grade being manufactured. 

 Supply the control device temperature, and the control device and THC monitoring 

operations indicator. 

Appendix C Page 12
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 1 

05/15/2014 

Background for Polyvinyl Chloride and Copolymers Production MACT 

Standards Development Information Collection Request

1.0 Introduction 

 The purpose of this attachment is to provide the respondent with additional detail on the 

relevant requirements of the Clean Air Act, the regulatory background of the polyvinyl chloride 

and copolymers production source category, and to provide a list of definitions of key terms used 

in the information collection request. 

2.0 Summary of Clean Air Act Requirements 

 The maximum achievable control technology (MACT) standards development 

information collection request was developed by the U. S. Environmental Protection Agency’s 

(EPA) Office of Air Quality Planning and Standards Emission Standards Division 

(OAQPS/ESD) to help EPA meet its obligations under the Clean Air Act Amendments of 1990. 

Specifically, the Clean Air Act Amendments require EPA to develop regulations under Section 

112(d) to limit emissions of hazardous air pollutants (HAP) from major and area sources of 

emissions. Section 112(a)(1) defines a major source as “any stationary source or group of 

stationary sources located within a contiguous area and under common control that emits or has 

the potential to emit considering controls, 10 tons per year or more of any hazardous air pollutant 

or 25 tons per year or more of any combination of hazardous air pollutants.” Based on the 

Administrator’s determination, EPA may lower the major source cutoff for individual HAP. An 

area source is “any stationary source of hazardous air pollutants that is not a major source.”

 The Clean Air Act Amendments of 1990 prescribe an analytical framework that EPA is 

to apply in developing national emission standards for hazardous air pollutants (NESHAP) for 

major sources. A key concept in this framework is the establishment of the MACT floor. The 

amendments specify that NESHAP for existing sources in a particular category or subcategory 

are to be no less stringent (but may be more stringent) than the average emission limitation 

achieved by the best performing 12 percent of the existing sources in such category or 

subcategory of sources. In categories or subcategories with less than 30 sources, the floor is to be 

based on the average emission limitation achieved by the best performing 5 sources. The MACT 

floor for new sources is the emission control that is achieved in practice by the best controlled 

similar source. 

 The Clean Air Act Amendments allow the EPA Administrator to "distinguish among 

classes, types, and sizes of sources within a category or subcategory in establishing such 

standards" (Section 112(d)). 

3.0 Regulatory Background for the Polyvinyl Chloride and Copolymers Production 

Source Category 

 On October 21, 1976, EPA promulgated emission standards for vinyl chloride under the 

risk-based standard then in effect (41 FR 46560; 40 C.F.R. Subpart F (§§ 61.60 - 61.71); “the 

Part 61 NESHAP”). When Congress amended the CAA in 1990, it required EPA to implement 

Appendix C Page 13
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 2 

05/15/2014 

technology based standards. As a result, EPA proposed MACT standards for the Polyvinyl 

Chloride and Copolymers Production source category on December 8, 2000 (65 FR 76958) and 

promulgated final MACT standards for the source category on July 10, 2002 (67 FR 45886) 

(“the Part 63 NESHAP”). EPA adopted most of the Part 61 NESHAP as the new Part 63 

NESHAP and the Part 61 standards became the MACT floor for existing sources. 

 Mossville Environmental Action NOW and Sierra Club petitioned the U.S. Court of 

Appeals of the District of Columbia to review various provisions of the Part 63 NESHAP. The 

Part 63 NESHAP was vacated on June 18, 2004 in Mossville v. EPA, 370 F. 3d. 1232 (D.C.Cir. 

2004) and remanded to the agency for it to reconsider or properly explain its methodology for 

regulating HAPs emitted in PVC production other than vinyl chloride by use of a surrogate. 

 On April 17, 2012, the EPA promulgated revised standards for PVC major and area 

sources. After promulgation, the Administrator received petitions for reconsideration of certain 

provisions in the final rules. 

 

 The purpose of the current information collection is to gather data from PVC production 

facilities that were either not included in the EPA’s previous data collection efforts for the source 

category or whose data were excluded by the Agency from various technical analyses that 

supported the April 2012 rulemaking. The collected data will support analyses of environmental 

and economic impacts of various revisions to the current Part 63 NESHAP for PVC major and 

area sources. 

4.0 Guidance Documents 

Following is a list of EPA guidance documents and resources that may be useful to respondents 

in estimating HAP emissions. 

1. Compilation of Air Pollutant Emission Factors: Volume I: Stationary Point and 

Area Sources. U. S. Environmental Protection Agency. Research Triangle Park, 

N.C. 1995. http://www.epa.gov/ttn/chief/ap42/index.html 

2. Factor Information Retrieval (FIRE) Data System. U. S. Environmental Protection 

Agency. http://cfpub.epa.gov/oarweb/index.cfm?action=fire.main

3. Protocol for Equipment Leak Emission Estimates. U. S. Environmental Protection 

Agency. Research Triangle Park, N.C. November 1995. Publication No.: EPA453/R-95-017.

4. Batch Process ACT. U. S. Environmental Protection Agency. Research Triangle 

Park, N.C. February 1994. Publication No.: EPA-453/R-94-020.

5.0 Key Term Definitions 

Appendix C Page 14
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 3 

05/15/2014 

The following definitions are provided for the purpose of the information collection request only. 

They are not intended to replace statutory definitions or regulatory definitions developed 

elsewhere. 

Bulk process/resin: A process for producing polyvinyl chloride resin that is 

characterized by a two-step anhydrous polymerization 

process: the formation of small resin particles in a prepolymerized reactor using small amounts of vinyl chloride 

monomer, an initiator, and agitation; and the growth of the 

resin particles in a post polymerization reactor using 

additional vinyl chloride monomer. Resins produced using 

the bulk process are referred to as bulk resins.

Control device: A combustion device, recovery device, recapture device, or 

any combination of these devices used to comply with a 

regulation, numerical emission limit, work practice 

standard, etc. Process condensers are not control devices.

Dispersion process/resin: A process for producing polyvinyl chloride resin that is 

characterized by the formation of the polymers in soap 

micelles that contain small amounts of vinyl chloride 

monomer. Emulsifiers are used to disperse vinyl chloride 

monomer in the water phase. Initiators used in the 

dispersion process are soluble in water. Resins produced 

using the dispersion process are referred to as latex or 

dispersion resins.

Feedstock: Raw material/input to the process unit.

Gas Holder: A surge control vessel with a bell that is floating in a vessel 

filled with water that is used to store gases from the PVC 

production process prior to being recovered or sent to a 

process vent control device. The bell rises and falls as lowpressure gases enter and leave the space beneath the bell and 

the water provides a seal between the enclosed gas within 

the floating bell and the ambient air.

Hazardous Air Pollutants (HAP): See 42 U.S.C. §7412(a)(6).

Appendix C Page 15
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 4 

05/15/2014 

Maintenance wastewater: Wastewater generated by the draining of process fluid from 

components in the PVCPU into an individual drain system 

prior to or during maintenance activities. Maintenance 

wastewater can be generated during planned and unplanned 

shutdowns and during periods not associated with a 

shutdown. Examples of activities that can generate 

maintenance wastewaters include descaling of heat 

exchanger tubing bundles, hydroblasting PVCPU process 

components such as polymerization reactors, vessels and 

heat exchangers, draining of low legs and high point bleeds, 

draining of pumps into an individual drain system, draining 

of portions of the PVCPU for repair and water used to wash 

out process components or equipment after the process 

components or equipment has already been opened to the 

atmosphere.

Malfunction: Any sudden, infrequent, and not reasonably preventable 

failure of air pollution control and monitoring equipment, 

process equipment, or a process to operate in a normal or 

usual manner which causes, or has the potential to cause, 

the emission limitations in an applicable standard to be 

exceeded. Failures that are caused in part by poor 

maintenance or careless operation are not malfunctions. (40 

CFR 63.2)

Polyvinyl Chloride and 

Copolymers Production Facility:

The collection of all polyvinyl chloride and copolymers 

production process unit, storage vessels, surge control 

vessels, heat exchange systems, wastewater, and process 

wastewater treatment systems that are associated with 

producing polyvinyl chloride.

Appendix C Page 16
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Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 5 

05/15/2014 

Polyvinyl Chloride and 

Copolymers Production Process 

Unit or PVCPU:

A collection of process components assembled and 

connected by hard-piping or duct work, used to process raw 

materials and to manufacture polyvinyl chloride and/or 

polyvinyl chloride copolymers. A PVCPU includes, but is 

not limited to, polymerization reactors; resin stripping 

operations; resin blend tanks; resin centrifuges; resin dryers; 

resin product separators; recovery devices; reactant and raw 

material charge vessels and tanks; holding tanks, mixing 

and weighing tanks; finished resin product storage tanks or 

storage silos; finished resin product loading operation; 

connected ducts and piping; equipment including pumps, 

compressors, agitators, pressure relief devices, sampling 

connection systems, open-ended valves or lines, valves and 

connectors and instrumentation systems. A PVCPU does 

not include chemical manufacturing process units, as 

defined in §63.101, that produce vinyl chloride monomer or 

other raw materials used in the PVC polymerization 

process.

Polyvinyl Chloride and Copolymer 

Resin (PVC Resin):

Polyvinyl Chloride Copolymer:

Polyvinyl Chloride Homopolymer:

The general reference to any PVC homopolymer or 

copolymer resin manufactured by the suspension, 

dispersion, bulk, and/or solution processes.

A synthetic thermoplastic polymer that is derived from the 

simultaneous polymerization of vinyl chloride and another 

monomer such as vinyl acetate. Polyvinyl chloride 

copolymer is produced by different processes, including, but 

not limited to, suspension, dispersion/emulsion, suspension 

blending, and solution processes.

Polyvinyl chloride homopolymer means a synthetic 

thermoplastic polymer that is derived from the 

polymerization of vinyl chloride and has the general 

chemical structure (-H2CCHCl-)n. Polyvinyl chloride 

homopolymer is typically a white powder or colorless 

granule. Polyvinyl chloride homopolymer is produced by 

different processes, including (but not limited to), 

suspension, dispersion/emulsion, blending and bulk 

processes.

Appendix C Page 17
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 6 

05/15/2014 

Process equipment: Any unit operation or group of unit operations or any part of 

a process or group of parts of a process that are assembled 

to perform a specific function. Examples of process 

equipment include, but are not limited to, polymerization

reactors, PVC resin strippers, resin dewatering and drying 

equipment storage tanks and vessels, cooling towers and 

heat exchange systems, and transfer operations.

Process unit: The process components assembled and connected by pipes 

or ducts to process raw and/or intermediate materials and to 

manufacture an intended product. For the purposes of this 

information collection request, process unit includes, but is 

not limited to, polyvinyl chloride production process.

Process wastewater: Wastewater that comes into direct contact with HAP or 

results from the production or use of any raw material, 

intermediate product, finished product, by-product or waste 

product containing HAP, but that has not been discharged 

untreated as wastewater. Examples are product tank 

drawdown or feed tank drawdown; water formed during a 

chemical reaction or used as a reactant; water used to wash 

impurities from organic products or reactants; water used to 

cool or quench organic vapor streams through direct 

contact; water discarded from a control device; and 

condensed steam from jet ejector systems pulling vacuum 

on vessels containing organics. Gasholder seal water is not 

process wastewater until it is removed from the gasholder.

Process wastewater stream: Each individual waste stream exiting an individual piece of 

process equipment (including, but not limited to, resin 

stripping equipment, knockout pots, condensers, 

centrifuges, and scrubbers) prior to being combined with 

any other stream. Process wastewater streams also include 

combined streams exiting wastewater collection tanks, 

wastewater treatment equipment/processes, etc.

PVC process wastewater treatment 

equipment:

An individual piece of equipment capable of and normally 

used for the purpose of removing organic compounds from 

a process wastewater stream, used alone or in combination 

with other PVC process wastewater treatment equipment. 

Examples include, but are not limited to, wastewater 

collection, holding, and equalization tanks, wastewater 

steam and vacuum strippers, and wastewater stripper 

feed/bottoms heat exchanger.

Appendix C Page 18
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 7 

05/15/2014 

PVC process wastewater treatment 

system:

A collection of PVC process wastewater treatment 

equipment that removes organic compounds from a process 

wastewater stream before the process wastewater stream is 

discharged from the PVC production facility.

Recovery equipment: Recovery equipment means an individual piece of 

equipment capable of and normally used for the purpose of 

recovering chemicals for fuel value (i.e., net positive 

heating value), use, reuse, sale, and/or destruction or 

disposal. Examples of equipment that may be recovery 

equipment include gas holders, compressors, condensers, 

and liquid separators used to recover vinyl chloride or other 

feedstocks from gaseous streams such as resin stripper and 

wastewater stripper overheads and return those feedstocks 

for reuse in the resin production process and/or eventual 

destruction or disposal. For the purposes of this information 

collection request, wastewater steam and vacuum strippers 

are considered PVC process wastewater treatment 

equipment and not recovery equipment.

Recovery system: A recovery system is a collection of recovery equipment. A 

recovery system typically vents to a control device such as a 

thermal oxidizer and acid gas scrubber.

Resin grade: The subdivision of PVC resin that describes it as a unique 

resin, i.e., the most exact description of a type of resin with 

no further subdivision. Examples include low molecular 

weight suspension resins and general purpose suspension 

resins.

Resin stripper: A unit that removes organic compounds from a raw 

polyvinyl chloride and copolymer product. In the 

production of a polymer, stripping is a discrete step that 

occurs after the polymerization reaction and before drying 

or other finishing operations. Examples of types of stripping 

include steam stripping, vacuum stripping, or other methods 

of devolatilization. For the purposes of this information 

collection request, devolatilization that occurs in dryers or 

other finishing operations is not resin stripping. Resin 

stripping may occur in a polymerization reactor or is a batch 

or continuous stripper separate from the polymerization 

reactor.

Shutdown: The cessation of operation of an affected source or portion 

of an affected source for any purpose. (40 CFR 63.2)

Appendix C Page 19
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 8 

05/15/2014 

Startup: The setting in operation of an affected source or portion of 

an affected source for any purpose. (40 CFR 63.2)

Stream: Any contained or non-contained solid, liquid, gas, or vapor 

entering or exiting an individual unit operation or single 

piece of equipment.

Stripped resin: The material exiting the resin stripper than contains 

polymerized vinyl chloride.

Suspension blending process/resin: A process for producing polyvinyl chloride resin that is 

similar to the suspension polymerization process, but 

employs a rate of agitation that is significantly higher than 

the highest range for non-blending suspension resins. The 

suspension blending process uses a recipe that creates 

extremely small resin particles, generally equal to or less 

than 100 microns in size, with a glassy surface and very 

little porosity. The suspension blending process 

concentrates the resins using a centrifuge that is specifically 

designed to handle these small particles. Polyvinyl chloride 

resins produced using the suspension blending process are 

referred to as suspension blending resins and are typically 

blended with dispersion resins.

Suspension process/resin: A process for producing polyvinyl chloride resin that is 

characterized by the formation of the polymers in droplets 

of liquid vinyl chloride monomer or other co-monomers 

suspended in water. The droplets are formed by agitation 

and the use of protective colloids or suspending agents. 

Initiators used in the suspension process are soluble in vinyl 

chloride monomer. Polyvinyl chloride resins produced using 

the suspension process are referred to as suspension resins.

Type of Resin: The broad classification of PVC homopolymer and 

copolymer resin referring to the basic manufacturing 

process for producing that resin, including, but not limited 

to, suspension, dispersion, bulk, and solution processes.

Volatile Organic Compounds 

(VOC):

See 40 CFR 51.100(s).

Waste management: Handling, treatment, storage, and disposal of waste 

products.

Appendix C Page 20
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 9 

05/15/2014 

Wastewater: Process wastewater and maintenance wastewater. The 

following are not considered wastewater for the purposes of 

this subpart: 

(1) Stormwater from segregated sewers;

(2) Water from fire-fighting and deluge systems, 

including testing of such systems;

(3) Spills;

(4) Water from safety showers;

(5) Samples of a size not greater than reasonably 

necessary for the method of analysis that is use;

(6) Equipment leaks;

(7) Wastewater drips from procedures such as 

disconnecting hoses after cleaning lines; and

(8) Noncontact cooling water.

Appendix C Page 21
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 10

05/15/2014 

6.0 Key Acronyms and Units of Measure 

% percent

acfm actual cubic feet per minute

acfm/ft2actual cubic feet per minute per square foot

batches/yr batches per year

Btu/scf British thermal units per standard cubic foot

CAA Clean Air Act

day/yr days per year

DC District of Columbia

dscfm dry standard cubic feet per minute

EPA U.S. Environmental Protection Agency

ft feet

ft/s feet per second

ft3/1,000 afcm cubic feet per thousand actual cubic feet per minute

gpm U.S. gallons per minute

gr/dscf grains per dry standard cubic foot

HAP Hazardous Air Pollutants

hr/day hours per day

in inches

in H2O inches of water

kPa kilopascals

LAER lowest achievable emission rate

lb/day pounds (mass) per day

lb/gal pounds (mass) per U.S. gallon

Appendix C Page 22
Enclosure 1 

Attachment A 

PVC Section 114 Enclosure 1, Attachment A – Page 11

05/15/2014 

LDAR leak detection and repair

MACT maximum achievable control technology

mg/l milligrams per liter

MMlb/yr million pounds (mass) per year

NAICS North American Industry Classification System

NESHAP National Emission Standards for Hazardous Air Pollutants

OAQPS Office of Air Quality Planning and Standards

oC degrees Celsius

oF degrees Fahrenheit

ohm-cm ohm-centimeter

P&ID piping and instrumentation diagram

PFD process flow diagram

ppmv parts per million, by volume

ppmw parts per million, by weight

PVC polyvinyl chloride

S second or seconds

scfm standard cubic feet per minute

SPPD Sector Policies and Programs Division

ton/yr tons per year, or short tons per year

VOC Volatile Organic Compounds

vol% volume percent, or percent by volume

wt% weight percent, or percent by weight

Appendix C Page 23
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 1 

05/15/2014 

Summary of Test Procedures, Methods, 

and Reporting Requirements 

for Polyvinyl Chloride and Copolymers 

Facility Emission Points 

This document provides an overview of approved sampling and analysis methods, target 

reported units of measure, and reporting requirements for polyvinyl chloride and copolymer 

(PVC) production facilities required to conduct emissions testing and provide emission test data 

according to the section 114 letter. The purpose for this testing is to gather data on hazardous air 

pollutant emissions from process vents within this source category. These data will be used to 

supplement the existing HAP data set for process vents. The document is organized as follows: 

1.0 Stack Testing Procedures and Methods 

2.0 How to Report Data 

3.0 How to Submit Data 

4.0 Contact Information for Questions on Test Plan and Reporting 

1.0 Stack Testing Procedures and Methods 

This information collection request includes stack (performance) test data requests for 

several pollutants. If you operate a PVC production facility, then you are required to conduct 

testing as outlined in this document to determine your emissions. 

1.1 How to Select Sample Location and Gas Composition Analysis Methods 

You must use U.S. EPA Method 1 of Appendix A of part 60 to select the locations and 

number of traverse points for sampling. See http://www.epa.gov/ttn/emc/methods/method1.html 

for a copy of the method and guidance information. 

You must use U.S. EPA Method 3A or 3B of Appendix A of part 60 for analysis of flue 

gas composition, including oxygen concentration. See 

http://www.epa.gov/ttn/emc/methods/method3a.html for Method 3A or 

http://www.epa.gov/ttn/emc/methods/method3b.html for Method 3B information. 

1.2 Polyvinyl Chloride and Copolymers Production Test Methods and Reporting 

Testing must be conducted at the outlet or in the stack of the final control device 

including, but not limited to, a thermal oxidizer and acid gas scrubber (in series) used to control 

emissions from PVC production. Table 1.1 summarizes the required test methods for each 

pollutant, possible alternative methods, and the target reported units of measure. 

For copies of the recommended U.S. EPA methods and additional information, please 

refer to EPA’s Emission Measurement Center website: http://www.epa.gov/ttn/emc/. For 

Appendix C Page 24
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 2 

05/15/2014 

copies of the SW-846 methods, please refer to EPA’s SW-846 Online website: 

http://www.epa.gov/waste/hazard/testmethods/sw846/index.htm. If you would like to use a 

method not listed in Table 1.1, please contact the EPA for approval of an alternative test method. 

The request for an alternative test method should include the alternative test method or 

prescriptive alternative procedure, the reason for the request (e.g., lower detection limit, site 

specific matrix interference, increased precision, etc.), supporting empirical data (e.g. 

comparison with specified method, precision determination, etc.), and quality control procedures 

which ensure results are sufficiently accurate and precise. See the Emission Measurement 

Center’s Guideline Document 22 (http://www.epa.gov/ttn/emc/guidlnd/gd22.pdf) for more 

information on what information should be included in an alternative test method request. 

Each test should be comprised of a minimum of three valid runs at each sampling 

location. All pollutant concentrations should be corrected to 3 percent oxygen and should be 

reported on the same moisture basis. The target units of measure are specified in Table 1.1. 

Report the results of each stack test according to the instructions in Section 2.0 of this 

attachment. 30 days of THC monitoring is also required as specified in Section 1.3. In addition 

to the emission test data, you must also report the following process information taken during the 

testing period: 

 The type of resin being processed and the resin grade; 

 Emissions control device(s) 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 percent oxygen). 

The testing should be conducted while the PVC production process and any other nonPVC production process(es) that send emission streams to the same control device, is/are 

operating as close as possible to maximum mass loading of all HAP compounds to the control 

device and under “normal” operation, that is, not during periods of startup, shut down, or 

malfunction. A thorough description of the process(es), including production rate(s) and a 

comparison of those production rates to maximum production capacity for PVC process units 

and non-PVC process units during the entire testing cycle should also be provided. If, during the 

performance testing, it becomes clear that one or more “off specification” or “out of 

specification” resin batches will be produced, then the testing and process data and any other 

associated information must still be submitted and labeled as an “off spec” test.

In most instances, we are not specifying numerical detection limits; instead we have 

specified testing conditions and methods, including test run times and minimum sample volumes 

when appropriate, which we believe will provide sufficient data quality for decision making. We 

remind source owners and testers of the Clean Air Act section 114(a)(1) requirement to provide 

information requested for the development of emissions standards using methods that provide 

data necessary for the decisions. That includes data of quality sufficient to support those 

decisions. For the most part, we can identify test methods and procedures that will satisfy those 

decision making needs (e.g., minimum sampling times). In other cases, we recognize that the 

source owner's or tester's selection of test procedures or equipment could bear significantly on 

Appendix C Page 25
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 3 

05/15/2014 

the quality of the data. See Attachment C of this enclosure for information regarding guidance 

for calculating and reporting values measured below method detection levels.

We believe that the Clean Air Act is clear that it is incumbent on the source and the tester 

to apply methods and procedures resulting in data quality necessary for those decisions including 

providing for the lowest possible detection limits considering practical and reasonable 

limitations. For example, source owners and testers should not automatically choose to use low 

or medium quality equipment for testing (e.g., for cost reasons) if high quality equipment is 

reasonably available. We will review test reports in light of this expectation and will be 

particularly mindful of whether the testing procedures applied are representative of the highest 

reasonably expected capabilities (e.g., comparing reported minimum measurement detection 

levels between tests and testers). If we believe that a source owner or tester has failed to meet 

the requirement of the Act to provide data sufficient decisions, we can and will request additional 

measurements requiring the use of improved testing procedures. The enclosed certification 

statement must be signed by a responsible official (See Enclosure 6). 

Table 1.1: Summary of Polyvinyl Chloride and Copolymers’ Control System Outlet Emissions 

Measurement Methods and Alternative Methods1 

Pollutant Required Method

Possible Alternative 

Method

Target Reported 

Units of Measure

Vinyl Chloride U.S. EPA Method 18 with a 

minimum sample time of 1 

hour per run and a nominal 

detection level of less than 200 

ppbv.

None ppbvd @ 3% O2

HCl/Cl2 U.S. EPA Method 26 or 26A. 

Collect a minimum sample 

volume of 2 dscm per run. 

None ppmvd @ 3% O2

THC U.S. EPA Method 25A with a 

minimum sampling time of 4 

hours per run. Calibrate the 

measuring instrument with a 

mixture of the organic 

compounds being emitted or 

with propane. 

None ppmvd as propane

@ 3% O2

CH4 U.S. EPA Method 320. Have 

a minimum sample time of 4

hours per run.

U.S. EPA Method 18. Have a 

minimum sample time of 4

hours per run.

ppmvd @ 3% O2

Dioxins/Furans2 U.S. EPA Method 23. Collect 

a minimum sample volume of 

5 dscm per run. Use high

resolution GC/MS for the 

analytical finish. 

None ng/dscm @ 3% O2

Appendix C Page 26
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 4 

05/15/2014 

Pollutant Required Method

Possible Alternative 

Method

Target Reported 

Units of Measure

Speciated HAP listed 

in Table 1.33

Sample collection by SW-846 

Method 0031, sample

preparation by SW-846 

Method 5041A, and sample 

analysis by SW-846 Method

8260B4. Combine traps in 

each run if lower detection 

limit is needed. Sample at a 

rate of 1 L/min, unless a 

slower sampling rate will yield 

detectable levels.

None ppmvd @ 3% O2

Speciated HAP listed 

in Table 1.43

Sample collection by SW-846

Method 0010, sample

preparation by SW-846 

Method 35425, and sample 

analysis by SW-846 Method

8270D4. Collect a minimum 

sample volume of 3 dscm per 

run. Use low resolution

GC/MS with the use of 

selected ion monitoring (SIM)

mode for the analytical finish.

None ppmvd @ 3% O2

Speciated HAP listed 

in Table 1.53

U.S. EPA Method 18 or 3206.

Minimum sample time of 1

hour per run. All compounds 

quantified by Method 320 

must be validated according to 

Section 13.0 of Method 320. 

All compounds quantified by 

Method 18 meet the recovery 

study specified in Section 8.4 

of Method 18.

None ppmvd @ 3% O2

O2 / CO2 U.S. EPA Method 3A. 

Simultaneous with each 

pollutant test run.

U.S. EPA Method 3B % volume, dry

Moisture U.S. EPA Method 4. 

Simultaneous with each 

pollutant test run.

None % volume

Flowrate U.S. EPA Method 2. 

Simultaneous with each 

pollutant test run.

U.S. EPA Method 2A, 2B, 2C, 

2D, 2F, or 2G, as appropriate.

ascfm and dscfm

1

 You must sample THC, vinyl chloride, and all speciated HAP concurrently.

2 You must include the results for the individual dioxin/furan congeners as specified in Table 1.2. 

3

 If any HAP other than those listed in Tables 1.3-1.5 could be emitted from the process, you must test for those 

HAP using US EPA Method 320, US EPA Method 18, SW-846 Method 0010, or an approved alternative test 

method, as applicable. 

4

 You must use all three SW-846 methods in combination to obtain a measurement result. The first method is the 

sampling method to be used at the stack. The second method is a preparatory method that readies for analysis the 

sample obtained from the first method. The third method is the analysis method. 

5 SW-846 Method 3542 replaces Section 8.1 of SW-846 Method 0010. 

Appendix C Page 27
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 5 

05/15/2014 

6

 The selection of technique [Method 320, Method 18 – Bag Sampling (Section 8.2.1), Method 18 – Direct 

Interface (Section 8.2.2), or Method 18 – Absorption Tube (Section 8.2.4)] must be made for each compound in 

Table 1.5 to achieve the lowest detection limit and meet method quality parameters. 

Table 1.2 Dioxin/Furan Congeners 

Dioxin/furan congener

2,3,7,8-tetrachlorodibenzo-p-dioxin.

1,2,3,7,8-pentachlorodibenzo-p-dioxin.

1,2,3,4,7,8-hexachlorodibenzo-p-dioxin.

1,2,3,7,8,9-hexachlorodibenzo-p-dioxin.

1,2,3,6,7,8-hexachlorodibenzo-p-dioxin.

1,2,3,4,6,7,8-heptachlorodibenzo-p-dioxin.

octachlorodibenzo-p-dioxin.

2,3,7,8-tetrachlorodibenzofuran.

2,3,4,7,8-pentachlorodibenzofuran.

1,2,3,7,8-pentachlorodibenzofuran.

1,2,3,4,7,8-hexachlorodibenzofuran.

1,2,3,6,7,8-hexachlorodibenzofuran.

1,2,3,7,8,9-hexachlorodibenzofuran.

2,3,4,6,7,8-hexachlorodibenzofuran.

1,2,3,4,6,7,8-heptachlorodibenzofuran.

1,2,3,4,7,8,9-heptachlorodibenzofuran.

Octachlorodibenzofuran.

Table 1.3 Target Analytes Using SW-846 Method 8260B 

Pollutant CAS Number Pollutant CAS Number

Benzene 71432 n-Hexane 110543

Chloroethane 75003 Methylene chloride 75092

Chloroform 67663 Toluene 108883

Chloroprene 126998 1,1,1-Trichloroethane 71556

1,1-Dichloroethane 75343 1,1,2-Trichloroethane 79005

1,2-Dichloroethane 107062 Vinylidene chloride 75354

Table 1.4 Target Analytes Using SW-846 Method 8270D 

Pollutant CAS Number Pollutant CAS Number

Acetophenone 98862 Hydroquinone 123319

Appendix C Page 28
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 6 

05/15/2014 

Pollutant CAS Number Pollutant CAS Number

Bis(2-ethylhexyl) phthalate 

(DEHP)

117817 Naphthalene 91203

1,4-Dichlorobenzene 106467 Phenol 108952

2,4-Dinitrophenol 51285 1,2,4-Trichlorobenzene 120821

Hexachlorobutadiene 87683

Table 1.5 Target Analytes Using US EPA Method 18 and 320 

Pollutant CAS Number Pollutant CAS Number

Acetaldehyde 75070 Formaldehyde 50000

1,3-Butadiene 106990 Methanol 67561

Chlorobenzene 108907 1,1,2,2-Tetrachloroethane 79345

Chloromethane 74873 2,2,4-Trimethylpentane 540841

Cumene 98828 Vinyl acetate 108054

Ethylbenzene 100414 Vinyl bromide 593602

Ethylene glycol 107211 Xylenes (isomers and mixtures) 1330207

1.3 Total Hydrocarbon 30-Day Monitoring 

You must conduct total hydrocarbon (THC) monitoring continuously for a 30-day period 

as specified in Table 1.6. You must also concurrently record the exhaust gas oxygen and 

moisture levels, the types and grades of PVC resin being produced and the control device 

temperature. Also indicate periods of abnormal operation for the control device and/or THC 

monitoring equipment. All the emissions testing required in Table 1.1 must be conducted during 

this 30-day monitoring period. 

Table 1.6 30-Day THC Monitoring 

Pollutant Recommended Method Alternative Method

Target Reported 

Units of Measure

THC U.S. EPA Method 25A 

continuously for 30 days.

Calibrate the measuring 

instrument with propane. The 

low level and high level 

calibration gases (see sections 

7.1.3 and 7.1.5 of Method 25A) 

must bracket the measured 

concentrations or a maximum 

high level calibration gas (see 

section 7.1.5 of Method 25A) of 

10 ppm propane must be used.

None ppmvd as propane @ 

3% O2

CH4 U.S. EPA Method 320 U.S. EPA Method 18 or 

instrument that uses 

chromatographic column to split

methane from all other organic 

compounds.

ppmvd @ 3% O2

O2 U.S. EPA Method 3A

continuously for 30 days. 

U.S. EPA Method 3B % volume, dry

Appendix C Page 29
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 7 

05/15/2014 

Pollutant Recommended Method Alternative Method

Target Reported 

Units of Measure

Moisture U.S. EPA Method 4 once per 

day for 30 days.

Where the exhaust stream is 

saturated (e.g. the outlet of a wet 

scrubber), you may measure the 

temperature by thermocouple 

and report the moisture at 

saturation levels. Where a stack 

is not saturated, moisture may 

be determined by wet/dry bulb 

psychrometry (ASTM E-337)

twice daily (at least one hour 

apart), by Method 320, or by 

ASTM D6348-12 (FTIR)

% volume

2.0 How to Report Data 

The method for reporting the results of testing and monitoring depends upon the methods 

used to complete the testing and monitoring requirements. This section discusses the 

requirements for reporting the collected data. 

2.1 Reporting stack test data 

For data collected using EPA Methods 23, 25/25A, and 26/26A, you must report the 

results of the performance test using the EPA’s Electronic Reporting Tool (ERT). You do not 

need to use the ERT to report the results of the 30-day THC monitoring; you only need to use the 

ERT to report the results of the Table 1.1 stack test. The ERT website (see 

http://www.epa.gov/ttn/chief/ert/index.html) contains the latest version of the ERT, as well as 

frequently asked questions and a user’s guide. The ERT is a Microsoft Access program that 

must be downloaded onto your computer prior to data entry. The file generated from the ERT 

must be submitted according to one of the methods specified in Section 3.0 of this Attachment. 

For data collected using all other test methods, you must report the results of the 

performance test(s) using Form P in the information collection request response forms Microsoft 

Excel workbook. You must also submit an electronic copy of the emission test report that 

includes all of the information specified in Section 2.2 of this Attachment (PDF format 

preferred). 

If you claim that some of the results of the performance test being submitted are 

confidential business information (CBI), you must submit the complete file including 

information claimed to be CBI. The submitted materials must be clearly marked as CBI 

submitted according to Section 3.0 of this Attachment. You must submit a separate copy of the 

file with all CBI data removed. Submit the non-CBI version of the file according to one of the 

options in Section 3.0 of this Attachment. 

2.2 Stack test data to be included in the report 

At a minimum, all performance test reports must include the following information: 

Appendix C Page 30
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 8 

05/15/2014 

 General identification information for the facility including a mailing address, the actual 

address, the owner or operator or responsible official (where they are applicable) or an 

appropriate representative and an email address for this person, and the appropriate 

Federal Registry System (FRS) number for the facility; 

 A brief process description, including a flow diagram clearly showing all process vent 

piping at the inlet to the first control device including manifolds and tie-in points for nonPVC process unit process vents (with those non-PVC process units identified), any 

piping that allows a process vent to bypass the control device(s), and the sampling site; 

 A complete unit description for PVC and non-PVC process units, including a description 

of emission streams and control devices, the appropriate source classification code 

(SCC), the latitude and longitude of the emission point being tested (to five decimal 

points), and the permitted maximum process rate (where applicable); 

 Sampling site description; description of sampling and analysis procedures and any 

modifications to standard procedures; quality assurance procedures; 

 Any process data and control device monitoring data required in this attachment; 

 Raw data sheets for field sampling; 

 Raw data sheets for field and laboratory analyses; 

 Chain-of-custody documentation; 

 Explanation of laboratory data qualifiers; 

 Example calculations of all applicable stack gas parameters, emission rates, percent 

reduction rates, and analytical results, as applicable; 

 Identification information for the company conducting the performance test including a 

contact person and his/her email address; and 

 Any other information required by the test method, a relevant standard, or the 

Administrator. 

Make clear, using the “Notes” section of the ERT or Form P, the correlation between 

emissions measurements and process data (e.g., identify Method 29, run 1 for the associated 

process data on the process data details tab of the ERT). 

2.3 Flagging data and handling data that is below the detection limit 

See Attachment C of this enclosure for information on how to flag data and on how to 

calculate and report values measured below the method detection limit. 

3.0 How to Submit Data 

You may submit your data in one of the three ways listed below. However, in order to 

avoid duplicate data and keep all data for a particular facility together, we request that you 

submit all non-CBI data requested from your facility in the same way. To submit your data: 

 E-mail an electronic copy of all requested files to CCG-PVC@epa.gov

Appendix C Page 31
Enclosure 1 

Attachment B 

PVC Section 114 Enclosure 1, Attachment B – Page 9 

05/15/2014 

 Mail a CD or DVD containing an electronic copy of all requested files to the EPA 

address shown in your section 114 letter. If no electronic copy is available, mail a hard 

copy of all requested files to the EPA address shown in your section 114 letter.

 If you are submitting Confidential Business Information (CBI), you must mail a separate 

CD or DVD containing only the CBI portion of your data to the EPA address shown in 

your section 114 letter. 

4.0 Contact Information for Questions 

For questions on how to report data using the ERT contact: 

Ron Myers 

(919) 541-5407 

myers.ron@epa.gov

For questions on the test methods contact: 

Jason DeWees 

(919) 541-9724 

dewees.jason@epa.gov

Stef Johnson 

(919) 541-4790 

johnson.steffan@epa.gov 

For all other questions contact: 

Jodi Howard 

(919) 541-4607 

howard.jodi@epa.gov 

Appendix C Page 32
Enclosure 1 

Attachment C 

PVC Section 114 Enclosure 1, Attachment C – Page 1 

5/15/2014 

Guidance for Calculating and Reporting Values Measured Below Method 

Detection Levels 

1.0 Identification of Detection Levels 

Identify the status of measured values relative to detection levels on the spreadsheet or in the 

ERT using the following descriptions: 

 BDL (below detection level) – all analytical values used to calculate and report an instack emissions value are less than the laboratory’s reported detection level(s); 

 DLL (detection level limited) – at least one but not all values used to calculate and report 

an in-stack emissions value are less than the laboratory’s reported detection level(s); or

 ADL (above detection level) – all analytical values used to calculate and report an instack emissions value are greater than the laboratory’s reported detection level(s). 

2.0 Reporting and Calculating Method Detection Limits 

For reporting and calculating individual test run data: 

 You must use the method specified approach for calculation and determination of the 

method detection limit (MDL). If the method does not specify the approach and 

calculation of the MDL, determine the MDL as follows: 

o For air sampling and analysis methods, you must determine the MDL in 

accordance with the procedures specified in Section 15 of Method 301 (located in 

Appendix A of 40 CFR part 63). 

o For water sampling and analysis, you must determine the MDL in accordance 

with the procedures specified in Appendix B of 40 CFR part 136. 

 For analytical data reported from the laboratory as above the MDL, include the ADL flag 

in the Form P columns labeled “Run #1 Detection”, “Run #2 Detection”, and/or “Run #3 

Detection” as appropriate or in the Comments line in the ERT. 

 For analytical data reported from the laboratory as “nondetect” or “below detection 

level;”

o Include a brief description of the procedures used to determine the analytical 

detection and in-stack detection levels: 

 In the Notes line of Excel spreadsheet template; or 

 In the Comments line of Lab Data tab in the Run Data Details in the ERT. 

o Describe these procedures completely in the full test report including the 

measurements made, the standards used, and the statistical procedures applied. 

o Calculate the in-stack emissions rate for any analytical result reported as below 

detection level using the relevant MDL, sampling volumes and other relevant run 

Appendix C Page 33
Enclosure 1 

Attachment C 

PVC Section 114 Enclosure 1, Attachment C – Page 2 

5/15/2014 

specific parameters (such as oxygen or flowrate). The reported value must 

assume that the analyte is present at the full MDL value. 

o Report the calculated emissions concentration or rate result: 

 As a detection level numerical value (i.e., no brackets or < symbol) in the 

Excel spreadsheet template (Form P; columns “Run 1”, “Run 2”, and/or 

“Run 3” as appropriate) and select the appropriate flag in the Form P 

columns labeled “Run #1 Detection”, “Run #2 Detection”, and/or “Run #3 

Detection” as appropriate; or 

 As a numerical value in the ERT with the appropriate flag in the 

Comments line. 

o Report as numerical values (i.e., no brackets or < symbol) any analytical data 

measured above the MDL, including any data between the MDL and a laboratoryspecific reporting or quantification level (i.e., flag as ADL). 

o Apply these reporting and calculation procedures to measurements made with 

Method 23: 

 Report data in the ERT for each of the D/F congeners measured with 

Method 23 below the detection level as [< detection level]; 

 Do not report emissions as zero, as described in the method. 

 For pollutant measurements composed of multiple components or fractions (e.g., Hg and 

other metals sampling trains) when the result for the value for any component is 

measured below the MDL: 

o Calculate in-stack emissions rate or concentrations as outlined above for each 

component or fraction; 

o Sum the measured values and/or calculated values (using the MDL as outlined 

above) for all of the components or fractions; and 

o Report the sum of all components or fractions: 

 As a detection level numerical value (i.e., no brackets or < symbol) in the 

Excel spreadsheet template (Form P; columns “Run 1”, “Run 2”, and/or 

“Run 3” as appropriate) and select the appropriate flag in the Form P 

columns labeled “Run #1 Detection”, “Run #2 Detection”, and/or “Run #3 

Detection” as appropriate; or 

 As a numerical value in the ERT with the appropriate flag in the 

Comments line. 

 If all components or fractions are BDL, the appropriate flag is BDL. If 

any component or fraction is ADL, the appropriate flag is DLL. 

o In addition to reporting the sum of the components or fractions, report the 

individual component or fraction values for each run if the Excel spreadsheet 

template or ERT format allows. 

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Enclosure 1 

Attachment C 

PVC Section 114 Enclosure 1, Attachment C – Page 3 

5/15/2014 

o If the Excel spreadsheet template or ERT format does not allow reporting of the 

individual components or factions (i.e., the format allows reporting only a single 

sum value): 

 For the Excel spreadsheet template, next to the sum reported as above 

report in the Notes line the appropriate flag along with the values for the 

measured or MDL value for each component or fraction as used in the 

calculations (e.g., 0.036, [<0.069], 1.239, [<0.945] for a four fraction 

sample) 

 For the ERT, next to the sum reported as above, report on the Comments

line the appropriate flag and the measured or MDL value for each 

component or fraction as used in the calculations (e.g., 0.036, [<0.069], 

1.239, [<0.945] for a four fraction sample) 

 For measurements conducted using instrumental test methods (e.g., Methods 3A, 6C, 7E, 

10, 25A): 

o Record gaseous concentration values as measured including negative values and 

flag as ADL; do not report as BDL 

o Calculate and report in-stack emissions rates using these measured values 

o Include relevant information relative to calibration gas values or other technical 

qualifiers for measured values in Comments line in the ERT or Notes line of the 

Excel spreadsheet. 

 For reporting and calculating average emissions rate or concentration for a test when 

some results are reported as BDL: 

o Sum all of the test run values including those indicated as BDL or DLL as 

numerical values 

o Calculate the average emissions rate or concentration (e.g., divide the sum by 3 

for a three-run test) 

o Report the average emissions rate or concentration average: 

 As a detection level numerical value (i.e., no brackets or < symbol) in the 

Excel spreadsheet template (Form P; columns “Run 1”, “Run 2”, and/or 

“Run 3” as appropriate) and select the appropriate flag in the Form P 

columns labeled “Run #1 Detection”, “Run #2 Detection”, and/or “Run #3 

Detection” as appropriate;

 As a numerical value in the ERT and include the appropriate flag in the 

relevant Comments line 

 If all test run values are BDL, the appropriate flag is BDL. If any test run 

value is ADL or DLL, the appropriate flag is DLL. 

Appendix C Page 35