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### November 6, 2012



# Summary of Test Procedures, Methods, And Reporting Requirements For Process Wastewater Sampling and Analysis at Polyvinyl

Chloride and Copolymer (PVC) 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

samp les from the outlet of process wastewater treatment system(s) which treat process wastewater streams originating from the affected source as defined in 40 CFR Part 63, Subpart HHHHHHH or DDDDDD.

All recipients must complete the sampling and analysis and s ubmit the results, reports, and documentation specified in Section 2.0 no later than May 1, 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) e missions from process wastewater in this source category. The document is organized as follows:

1.0 Process Wastewater Sampling Procedures and Analysis Methods 2.0 Data Reporting Procedures

3.0 Data Submission Procedures 4.0 Contact Information for Q uestions

5.0 Definitions



## 1.0 Process Wastewater Sampling Procedures and Analysis Methods

We are requiring sampling of each stream exiting the PVC process wastewater treatment system(s) at your facility. Sampling of each process wastewater treatment system is required for all HAP listed in Table 1, which can be detected by EPA methods listed

w ithin that same table. You must conduct sampling, sample preservation and sample storage in accordance with the specific methodology listed in Table 1 and Section 4.1.2

of SW

- 846 (Chapter 4

– Organic Analytes). You must collect one grab sample per PVC

pro cess wastewater treatment system for 30 consecutive operating days beginning no

later than January 7, 2013 . The samples must be taken during normal operating conditions. If you have a batch process wastewater treatment system that does not operate

continu ously, you must sample the outlet of that batch system at least once for each day

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### while it is operating such that at least 30 samples can be analyzed. [Note: Batch processes requiring multiple samples per batch should equally distribute the samples across the time taken for the effluent to discharge from the process to properly represent the concentration.] If you have more than one PVC process wastewater treatment system, the results must be reported separately for each day and for each treatment system (i .e., the results cannot be averaged). If you have identical water treatment systems that run in parallel and the outlet streams are not combined, you only need to sample one stream (however, include the combined flow rates for each stream). If you have ide ntical water treatment systems that run in parallel and the outlet streams are combined, then the sample must be taken after the streams are combined and the combined flow rate must be included. Each sample must be analyzed for the HAP listed in Table 1 an d for any other HAP expected to be present but not listed in Table 1.

Table 1. PVC Process Wastewater HAP

CAS No. HAP Analyte Category Analysis

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

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

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PVC Process Wastewater Sampling and Analysis Summary Page 3

11/06/12 75014 Vinyl Chloride VOC EPA Method 107

75354 Vinylidene Chloride (1,1

- Dichloroethylene) VOC SW

- 846

- 8260B

1330207 Xylenes (isomers and mixtures) VOC SW

- 846

- 8260B

SVOC

– semi

- volatile organic compound

VOC

– volatile organic compound



### 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

.



## 2.0 Data Reporting Procedures

Your facility’s submission in response to this request must include all of the following:

1. Completed copies of the Microsoft Excel 2007 spreadsheet workbooks that accompany this request. The workbooks are available for download at http://www2.ergweb.com/projects2/PVCSurvey/in dex.html

2. A report that includes all of the following:

a. A plot plan of the PVC process unit;

b. A schematic diagram of the process wastewater treatment system showing where the samples were taken and the sampling apparatus/configuration;

c. The flow rate for each stream (in gallons per minute) at the time of sampling. If there is a flow meter on a stream, you must report the measured flow rate. Otherwise, please specify that the reported flow rate is an engineering estimates and submit documentation of the calculat ion;

d. The temperature of each stream (in degrees Fahrenheit) at the time of sampling;

e. A description of process wastewater streams that are not treated prior to exiting the PVC production facility;

f. Any variations to the sampling procedures and/or analytical methods specified in this request;

g. The minimum detection limits (MDL) for each compound with each method used;

h. Quality assurance/quality control measures implemented during sampling and analysis.

3. A report from the entity (e.g., external or on

- site laboratory) analyzing samples associated with this request that contains all analytical procedures, results, and QA/QC measures. This report shall also include results of current proficiency samples ana lyses for all compounds and their appropriate method performed by the entity (e.g., external or on

- site laboratory) analyzing samples associated with this request. These analyses should have been performed in the last calendar year. If proficiency samples to cover all compounds and methodologies cannot be

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### procured, proof of analysis of a second source calibration standard during the sample analysis must be submitted.

4. The enclosed certification statement signed by a responsible official.

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

reas onable 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). I f 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.

Be aware that th ere 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 t o an enforcement action. We may use any information submitted in response to this request in an administrative, civil, or criminal action.



## 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 containin g 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 Confide ntial 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.

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## 4.0 Contact Information for Questions

For questions on the sampling procedures and a nalytical methods contact:

Jason DeWees (U.S. EPA)

919

- 541

- 9724 dewees.jason@epa.gov

For all other questions contact:

Andrea Siefers (U.S. EPA)

919.541.1185 siefers.andrea@epa.gov



## 5.0 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 wastewate r. 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 treatment system means a specific technique or collection of techniques that remove organic compounds from a process wastewater stream before the process wastewater stream exits the PVC production facility.

Wastewater means process wastewater and maintenance wast ewater. 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;

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### (7) Wastewater drips from procedures such as disconnecting hoses after cleaning lines; and (8) Noncontact cooling water.