Attachment A: PVC MACT Working Group Comments on CAA Section 114 Request 

Memo for Summary of Test Procedures, Methods, and Reporting Requirements For 

Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer 

Facilities, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo - Page 1

10/3/12

DRAFT

October 3, 2012

 

Summary of Test Procedures, Methods, 

And Reporting Requirements

For Process Wastewater Sampling and Analysis at Polyvinyl 

Chloride and Copolymer Facilities 

Under the authority of Section 114 of the Clean Air Act, EPA is requesting process 

wastewater sampling and analysis for facilities which produce polyvinyl chloride and 

copolymers (PVC). This sampling program requires you to collect process wastewater 

samples from the process wastewater treatment system(s) which originates from the 

affected source in 40 CFR Part 63, Subpart HHHHHHH or DDDDDD.

All recipients must complete the sampling and submit a test report with the results no 

later than XX/XX/2013. Any submissions made after this date will be in violation of this 

Section 114 request.

This document provides an overview of approved sampling and analytical methods, 

target pollutants, and reporting requirements for PVC production facilities required to 

provide process wastewater sampling data based on this section 114 request. The 

purpose for this testing is to gather data on hazardous air pollutant (HAP) emissions from 

process wastewater in this source category. The document is organized as follows:

1.0 Process Wastewater Sampling Procedures and Methods

2.0 Data Reporting Procedures

3.0 Data submission Procedures

4.0 Contact Information for Questions on Test Plan and Reporting

1.0 Process Wastewater Procedures and Methods

1.1 How to Select Sample Location

We are requiring sampling of the effluent for each of the process wastewater treatment 

systems (i.e. base of the wastewater stripper, or if there is no wastewater stripper then at 

each individual wastewater stream as it exits the process) which originate from your PVC 

production facilities. Sampling of each process wastewater treatment system is required 

Comment [RK1]: The due date needs to consider 

that some PVC Units may be shut down or at a low 

production rate during the Nov/Dec ’12 holidays. 

Propose May 1, 2013 per attached schedule. 

Comment [RK2]: It would be best to reword to 

indicate this phrase was intended to capture a site 

that does not have a wastewater stripper so it is clear 

that sampling is only being requested for the effluent 

of process wastewater systems.

Comment [RK3]: Can EPA confirm that only the 

effluent from the “process wastewater treatment 

system” or alternative process wastewater treatment 

system is required to be sampled?

Comment [RK4]: For sites that use knock out 

pots instead of WW strippers, can EPA confirm they

are only interested in effluent from the KO pot which 

is considered an alternative WW treatment system?
Attachment A: PVC MACT Working Group Comments on CAA Section 114 Request 

Memo for Summary of Test Procedures, Methods, and Reporting Requirements For 

Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer 

Facilities, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo - Page 2

10/3/12

for all HAP listed in Table 1.1, which can be detected by EPA procedures listed within 

that same table. You must conduct sampling, sample preservation and sample storage 

and transport according to the instructions in Section 8 of EPA Method 107. You must 

collect one grab or composite sample per process wastewater treatment system for 30 

consecutive days beginning XX/XX/201X. The samples must be taken during normal 

operating conditions. If you have more than one water treatment system, the results must 

be reported separately for each day (cannot be averaged). The samples must be analyzed 

for the following HAP and any other HAP expected to be present but not listed in Table 

1.1:

Table 1.1: PVC Process Wastewater HAP

CAS No. HAP Analyte

category Test method

107211 Ethylene glycol. Alcohol. SW-846-8015C.

67561 Methanol. Alcohol. SW-846-8015C.

75070 Acetaldehyde. Aldehyde. SW-846-8315A.

50000 Formaldehyde. Aldehyde. SW-846-8315A.

51285 2,4-Dinitrophenol. SVOC. SW-846-8270D.

98862 Acetophenone. SVOC. SW-846-8270D.

117817 Bis(2-Ethylhexyl) Phthalate 

(DEHP).

SVOC. SW-846-8270D.

123319 Hydroquinone. SVOC. SW-846-8270D.

108952 Phenol. SVOC. SW-846-8270D.

79345 1,1,2,2-Tetrachloroethane. VOC. SW-846-8260B.

106990 1,3-Butadiene. VOC SW-846-8260B.

540841 2,2,4-Trimethylpentane. VOC. SW-846-8260B.

71432 Benzene. VOC. SW-846-8260B.

108907 Chlorobenzene. VOC. SW-846-8260B.

67663 Chloroform. VOC. SW-846-8260B.

126998 Chloroprene. VOC. SW-846-8260B.

98828 Cumene. VOC. SW-846-8260B.

75003 Ethyl Chloride (Chloroethane). VOC. SW-846-8260B.

100414 Ethylbenzene. VOC. SW-846-8260B.

107062 Ethylene Dichloride (1,2-

Dichloroethane).

VOC. SW-846-8260B.

75343 Ethylidene Dichloride (1,1-

Dichloroethane).

VOC. SW-846-8260B.

74873 Methyl Chloride (Chloromethane). VOC. SW-846-8260B.

75092 Methylene Chloride. VOC. SW-846-8260B.

110543 n-Hexane. VOC. SW-846-8260B.

108883 Toluene. VOC. SW-846-8260B.

Comment [RK5]: The 24 hour analysis 

timeframe which is required by S8 of M107 is 

impractical for this sampling which must be sent to 

an offsite lab for analysis. That requirement is 

specific the M107 test methodology. Can EPA revise 

the requirement in a fashion whereby sampling, 

preservation, storage, and transport either must 

conform to practices required in EPA SW 846 or the 

method specified? 

Comment [RK6]: Some plants run batch WW 

stripping operations and as a result do not operate the 

WW stripper every day. Does EPA want 30 samples

or 30 operating days? Are more than one sample 

allowed per day if batch operations preclude 30 

consecutive days? Should it read 30 days of 

representative samples during normal operation? 

Are a minimum of 30samples required?

Comment [RK7]: Beginning on or before 

January 7, 2013.

Comment [RK8]: Should a different sampling 

plan be prepared for batch stripping (stripping unit 

operates every 3-7days) vs. continuous operations 

(stripping unit operates every day)?

Comment [RK9]: To be consistent, this should 

read “process wastewater treatment system or 

alternative process WW treatment system”.

Comment [RK10]: A batch treatment system that 

samples 1 /wk in effect is a 7 day average result (this 

may mean their data must be evaluated differently 

from continuous stripping systems) – may want to 

discuss in the call.

Comment [RK11]: Please insert: (excluding 

Vinyl Chloride). Reasoning: Vinyl chloride is 

expected in the samples but since it is handled by its 

own limit, it should be specifically excluding from 

this TOHAP determination. Also, instruction 

number 6 of the Sampling Data Tab in the Excel 

workbook specifically excludes vinyl chloride 

analysis.
Attachment A: PVC MACT Working Group Comments on CAA Section 114 Request 

Memo for Summary of Test Procedures, Methods, and Reporting Requirements For 

Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer 

Facilities, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo - Page 3

10/3/12

71556 Methyl Chloroform (1,1,1-

Trichloroethane)

VOC. SW-846-8260B.

79005 1,1,2-Trichloroethane VOC. SW-846-8260B.

108054 Vinyl Acetate. VOC. SW-846-8260B.

593602 Vinyl Bromide. VOC. SW-846-8260B.

75354 Vinylidene Chloride (1,1-

Dichloroethylene).

VOC. SW-846-8260B.

1330207 Xylenes (isomers and mixtures). VOC. SW-846-8260B.

For copies of the recommended U.S. EPA SW-846 methods, please refer to EPA’s SW846 Online website: http://www.epa.gov/waste/hazard/testmethods/sw846/index.htm. 

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 Clean Air Act to provide 

data sufficient for decisions, we can and will request additional measurements requiring 

the use of improved testing procedures.

Further, you are required to submit the results of a current proficiency sample analysis for 

all compounds and their appropriate method performed by the entity (e.g., external or onsite laboratory) analyzing samples associated with this questionnaire. This analysis 

should have been performed in the last calendar year. If a proficiency sample to cover all 

compounds and methodologies cannot be procured, proof of analysis of a second source 

calibration standard during the sample analysis must be submitted.

1.2 Definitions

For the purposes of this section 114 request, the following definitions apply:

Process wastewater means 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 
Attachment A: PVC MACT Working Group Comments on CAA Section 114 Request 

Memo for Summary of Test Procedures, Methods, and Reporting Requirements For 

Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer 

Facilities, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo - Page 4

10/3/12

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 treatment system means a specific technique or collection of 

techniques that remove or destroy the organics in a process wastewater stream to comply 

with 40 CFR 63.11965, 63.11970, and 63.11975. 

Wastewater means 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 used;

(6) Equipment leaks;

(7) Wastewater drips from procedures such as disconnecting hoses after cleaning 

lines; and

(8) Noncontact cooling water.

2.0 Reports

All process wastewater sampling reports must contain the enclosed certification statement 

signed by a responsible official.

Be aware that there are significant penalties for submitting false information, including 

the possibility of fines and imprisonment as explained in Section 113 of the Clean Air 

Act (42 USC §7413). Failure to comply fully with this request for information may 

subject you to an enforcement action. We may use any information submitted in response 

to this request in an administrative, civil, or criminal action.

Process Wastewater sampling report

You must complete the Excel worksheets that accompany this sampling summary along 

with a sampling report. A blank spreadsheet workbook can be downloaded from the 

following website:

http://www2.ergweb.com/projects2/PVCSurvey/index.html

The following items must be included in the process wastewater sampling report:

Comment [RK12]: . Can EPA explain why they 

included these sections in this definition? This has 

the potential to pick up process equipment that has 

water as a component.

Comment [RK13]: Does EPA intend to include 

this certification statement in the official S114 letter?

Comment [RK14]: Does EPA want lab reports 

submitted and if so, at which time should they be 

submitted?
Attachment A: PVC MACT Working Group Comments on CAA Section 114 Request 

Memo for Summary of Test Procedures, Methods, and Reporting Requirements For 

Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer 

Facilities, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo - Page 5

10/3/12

1. Unit operation(s) of wastewater origination with latitude and longitude reported in 

decimal degrees to the 5th decimal place;

2. Schematic diagram showing where the sample was taken and sampling 

configuration with latitude and longitude reported in decimal degrees to the 5th

decimal place

3. Flow rate for each stream (in gal/min);

4. Wastewater stream temperature; 

5. Description of streams that are controlled (e.g. not exposed to atmosphere);

6. Any variations of test methods used during testing; 

7. Minimum Detection Limit (MDL) for each compound with each method used; 

and

8. Quality assurance/quality control measures implemented during testing and 

analysis.

3.0 Data Submission Procedures

To avoid duplicate data and to keep all data for a particular facility together, we request 

that you submit all of the data requested from your facility in the same way. You may 

submit your data using one of the following options:

 

• E-mail an electronic copy of all requested files to siefers.andrea@epa.gov; or

• 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 on Test Plan and Reporting 

For questions on the test methods contact:

Jason DeWees (U.S. EPA)

919-541-9724

dewees.jason@epa.gov

For questions on the PVC production section 114 process wastewater sampling 

contact:

Andrea Siefers (U.S. EPA)

919.541.1185

siefers.andrea@epa.gov

Comment [RK15]: This is unclear and is an 

overly burdensome request. What is the purpose of 

listing unit operations?

Comment [RK16]: What is the purpose of 

including latitude and longitude coordinates and why 

is it necessary?

Comment [RK17]: Can the diagrams that were 

submitted previously be used to ID these points 

(some identified wastewater streams). Note some of 

these were classified as CBI.

Comment [RK18]: What is the purpose of 

including latitude and longitude coordinates and why 

is it necessary?

Comment [RK19]: All production data is 

confidential and should be listed in a separate 

workbook so that emissions information can be 

reported non-confidentially. Industry prefers to 

avoid having its confidential production volumes 

declared public just because it is included in the 

same workbook as public emissions information.