Attachment A: PVC MACT Working Group Comments on CAA Section 114 Request
Memo for Summary of Test Procedures, Metho ds, and Reporting Requirements F or Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer Facili ties

, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo

- Pa ge 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 chlori de 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 c omplete 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 metho ds, 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) emissio ns 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 k noc k o ut pots instead of WW strippers

, can EPA confirm they

are o nly interested in effluent from the KO p ot 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, Metho ds, and Reporting Requirements F or Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer Facili ties

, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo

- Pa ge 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 collec t 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 m ust 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 fashi on 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 o r 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 trea tment 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 Sampl ing Data Tab in the Excel

w orkbook specifically excludes vinyl chloride analysis.Attachment A: PVC MACT Working Group Comments on CAA Section 114 Request
Memo for Summary of Test Procedures, Metho ds, and Reporting Requirements F or Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer Facili ties

, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo

- Pa ge 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 SW

846 Online website: http://www.epa.gov/waste/hazard/testmethods/sw846/index.htm

.

We believe tha t 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

re asonable 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 lig ht 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 a re 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 on

site laboratory) analyzing samples associated with this questionnaire. This analysis sho uld 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 fr om organic products or reactants; water used to cool or quench organic vapor streams through direct contact; water discarded from a control device; and condensedAttachment A: PVC MACT Working Group Comments on CAA Section 114 Request
Memo for Summary of Test Procedures, Metho ds, and Reporting Requirements F or Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer Facili ties

, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo

- Pa ge 4 10/3/12 steam from jet ejector systems pulling vacuum on vessels containing organics. Gasholder seal w ater 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 63.1 1965, 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 suc h 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 enf orcement 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 explai n 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 submi tted 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, Metho ds, and Reporting Requirements F or Process Wastewater Sampling and Analysis at Polyvinyl Chloride and Copolymer Facili ties

, Draft October 3, 2012”

Draft PVC Process Wastewater Sampling Procedures Memo

- Pa ge 5 10/3/12 1. Unit operation(s) of wastewater origination with latitude and longitude reported in decimal degrees to the 5 th decimal place; 2. Schematic diagram showing where the sample was taken and sampling configuration with latitude and longitude reported in d ecimal degrees to the 5 th 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 Det ection 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 submi tting 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 q uestions 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 pur pose 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.