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5/9/2023 - REMOVE FROM FINAL NEICVP1216E05 Replacement Report NEIC CIVIL INVESTIGATION REPORT Denka Performance Elastomer LaPlace, Louisiana Investigation Dates: May 9-11, 2023 Digitally signed by LAWRENCE LUTZ RICHARD Digitally signed by RICHARD HELMICH Date: 2023.08.17 10:21:32 -06'00' Craig Lutz HELMICH Date: 2023.08.16 15:30:20 -06'00' Richard Helmich Project Manager, NEIC Analytical Project Manager, NEIC Authorized for Release by: MICHAEL Digitally signed by MICHAEL ROACH ROACH Date: 2023.08.17 11:36:42 -06'00' Michael Roach, Acting Field Branch Manager, NEIC Report Prepared for: Office of Civil Enforcement Lynne Davies 1200 Pennsylvania Ave NW Washington, DC 20460 EPA Region 6 Jeffrey Yurk 1201 Elm Street Dallas, TX 75270 NATIONAL ENFORCEMENT INVESTIGATIONS CENTER P.O. Box 25227 Building 25, Denver Federal Center Denver, Colorado 80225 Page 1 of 9 CONTENTS INVESTIGATION OVERVIEW ............................................................................................................ 3 PROJECT OBJECTIVE .................................................................................................................... 3 FACILITY CONTACT INFORMATION ............................................................................................. 3 FACILITY OVERVIEW .................................................................................................................... 3 FIELD ACTIVITIES SUMMARY....................................................................................................... 4 Measurement and Sampling Activities ................................................................................... 4 LABORATORY ACTIVITIES SUMMARY.......................................................................................... 5 ANALYTICAL RESULTS.................................................................................................................. 6 TABLES Table 1. PROJECT TEAM MEMBERS ................................................................................................ 3 Table 2. FACILITY CONTACT INFORMATION ................................................................................... 3 Table 3. FIELD MEASUREMENT AND FIELD SAMPLING ACTIVITIES ................................................ 4 Table 4. ANALYTICAL OBJECTIVE, TECHNIQUE, AND METHOD; ANALYST; AND DATE PERFORMED ......................................................................................................................................................... 6 Table 5. SUMMARY OF ANALYTICAL RESULTS ................................................................................ 6 FIGURES Figure 1. The temperature of samples S01A, S04A, and S06A during testing in 100-mm cubes... 8 Figure 2. The temperature of sample S06A during testing in 25-mm cubes.................................. 9 APPENDICES (* NEIC GENERATED) A* Field Photographs (2 pages) B* Laboratory Receipt Photographs (6 pages) C* Laboratory Photographs (2 pages) This Contents page shows all the sections contained in this report and provides a clear indication of the end of this report. NEICVP1216E05 Page 2 of 9 Denka Performance Elastomer LaPlace, Louisiana INVESTIGATION OVERVIEW This report (NEICVP1216E05) replaces the following U.S. Environmental Protection Agency (EPA) National Enforcement Investigations Center (NEIC) report in its entirety: NEICVP1216E03 (June 2023). This replacement was necessary to correct the following issue: separately report confidential information. PROJECT OBJECTIVE U.S. Environmental Protection Agency (EPA) Office of Civil Enforcement (OCE) Waste Compliance and Enforcement Division (WCED) and EPA Region 6 (Region) requested EPA's National Enforcement Investigations Center (NEIC) to collect samples at Denka Performance Elastomer (Denka) located at 560 Highway 44, LaPlace, Louisiana. Samples were collected from the polymerization reactor strainers, also known as poly kettle strainers (PKS). The collected samples were analyzed to determine ignitability and reactivity properties. Table 1 lists the project team members. Team Member Craig Lutz Tanner Cheney Agustin Martinez Richard Helmich Kai Sinclair John Penland Mark Stead Table 1. PROJECT TEAM MEMBERS Organization NEIC NEIC NEIC NEIC NEIC REGIONAL AND OTHER CONTACTS EPA Region 6 EPA Region 6 Project Role Project manager (PM) Field team member Field team member Analytical project manager (APM), field and laboratory team member Laboratory team member Regional field team member Regional field team member FACILITY CONTACT INFORMATION Table 2 lists the primary facility contact. Name, Title Chris Meyers, Environmental Affairs Manager Table 2. FACILITY CONTACT INFORMATION Phone No. 995-536-7802 Email Address christopher-meyers@denka- pe.com FACILITY OVERVIEW Denka is listed with EPA Registry Identification No. 110067396669 and manufactures neoprene. Denka operates on property owned by E.I. DuPont de Nemours. The Region inspected the facility on April 18-22, 2022, and returned on May 5, 2022, to conduct an additional inspection and to collect samples. An administrative consent agreement was signed by EPA and Denka on December 22, 2022. The consent agreement required Denka to develop a waste determination plan for sampling and analysis of PKS waste for EPA's approval within 60 days. The Region and NEICVP1216E05 Page 3 of 9 Denka Performance Elastomer LaPlace, Louisiana WCED were on-site conducting another compliance inspection at the same time NEIC was sampling. FIELD ACTIVITIES SUMMARY Measurement and Sampling Activities The NEIC field team provided support to this investigation by sampling material from poly kettle strainers in the poly kettle building. The poly kettle reactors produce crude neoprene from chloroprene. The strainers remove unwanted solids from the product. Samples of the solids along with any entrained liquids were collected. Table 3 summarizes field measurement and field sampling activities. Photographs from the field activities are provided in Appendix A. All environmental measurement activities were performed in accordance with the NEIC quality system. All field sampling, monitoring, and laboratory flash point measurements described in this report are within the scope of NEIC's ISO/IEC 17025 accreditation issued by the ANSI National Accreditation Board (certificate No. FT-0303). The SW-846 Methods 1030 and 1050 results are not within the scope of NEIC's ISO/IEC 17025 accreditation. Denka was manufacturing product NPR-2008 at the time of the sampling. During the sampling event, the facility had an unplanned shutdown of the emission control device from approximately 10:00 a.m. on May 10, 2023, that extended into early morning May 11, 2023. This caused Denka to hold products in the poly kettle reactors overnight because the downstream processes had to be shut down until the emission controls were restarted. The samples collected on May 11, 2023, were from batches held overnight. This is longer than the usual holding time for the material in the poly kettle reactors. Table 3. FIELD MEASUREMENT AND FIELD SAMPLING ACTIVITIES Location Identifier Dates Method, and/or Procedure1, and Equipment MEASUREMENTS MSA Altair used to screen location for safety; May 1011, 2023 NEIC procedure: Safety and Sample Screening Instruments, NEICPROC/17-002 Instrument guide: MSA Altair 5X Multi-Gas Monitoring Equipment RadEye used additionally to screen samples for radiation May 1011, 2023 NEIC procedure: Safety and Sample Screening Instruments, NEICPROC/17-002 Instrument guide: RadEye B20-ER - Radiation Detection Equipment Measurer Name Craig Lutz Craig Lutz NEICVP1216E05 Page 4 of 9 Denka Performance Elastomer LaPlace, Louisiana Table 3. FIELD MEASUREMENT AND FIELD SAMPLING ACTIVITIES SAMPLING Station No. Appendix A Photo Nos. Dates and Sampling Time Technique Method, and/or Procedure1, and Equipment S01A, S01B1 P5100001.JPG P5100003.JPG 5/10/2023 Grab 09:35 a.m. sample Manually grabbed by hand with disposable gloves. S04A, S04B1 P5110006.JPG 5/11/2023 Grab 08:05 a.m. sample Manually grabbed by hand with disposable gloves. S06A, S06B2 P5110007.JPG 5/11/2023 Grab 08:30 a.m. sample Manually grabbed by hand with disposable gloves. 1 The current version of each procedure, at the time of the investigation, was followed. 2 Split samples left with the facility. Sampler Name Craig Lutz Craig Lutz Craig Lutz Samples collected during the field activities were stored on ice. The samples' temperature was monitored and recorded while driven by Tanner Cheney and Augustin Martinez to the NEIC laboratory in Denver, Colorado, for analysis. LABORATORY ACTIVITIES SUMMARY Richard Helmich received the samples from Tanner Cheney on May 15, 2023. The laboratory team analyzed the samples for properties of ignitability and reactive hazardous waste. Table 4 summarizes the analytical methods followed, as well as the analysts and dates of the analyses. Data quality summaries, including uncertainty measurements, for all laboratory measurements are maintained in the project files. NEICVP1216E05 Page 5 of 9 Denka Performance Elastomer LaPlace, Louisiana Table 4. ANALYTICAL OBJECTIVE, TECHNIQUE, AND METHOD; ANALYST; AND DATE PERFORMED Analytical Objective, Technique, and Method NEIC Analyst Samples Analyzed by Method (Station Nos.) Dates Performed Ignitability: Method 1020C, Standard Test Methods for Flash Point by Setaflash (Small Scale) Closed Cup Apparatus, December 2018, Third Edition of the Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, and EPA publication SW-846. Kai Sinclair S01A - liquid S04A - liquid S06A - liquid May 18-25, 2023 ASTM D3278-78, "Standard Test Methods for Flash Point for Liquids by Setaflash Closed Tester and Setaflash Method for Determining Ignitability of Liquids, NEICPROC/06-001 Burn Rate: Method 1030, Ignitability of Solids, Revision 1, July 2014, Final Update V to the Third Edition of the Test Methods for Evaluating Solid Waste, Richard Helmich S01A - solids S04A - solids S06A - solids May 17-22, 2023 Physical/Chemical Methods, EPA publication SW-846. Spontaneous Combustion and Self-Heating: Method 1050, Test Methods to Determine Substances Likely to Spontaneous Combust, Revision 0, February 2007, Final Update IV to the Third Edition of the Test Methods for Richard Helmich S01A S04A S06A May 25-June 7, 2023 Evaluating Solid Waste, Physical/Chemical Methods, EPA publication SW-846 ANALYTICAL RESULTS Table 5 summarizes the analytical results. Station No. S01A - liquid S01A - solid Station Location/ Description of Sample Location Poly Kettle #2 Strainer Table 5. SUMMARY OF ANALYTICAL RESULTS Appendix B Photo Nos. Laboratory Sample Physical Description Flash Point Results (C1) 101_5161.JPG 101_5162.JPG White, opaque, non-viscous, emulsion, liquid Brown, black, white, Clumps, Rubbery, Sticky, wet, soft, solid < 60 C N/A Burn Rate N/A2 Did not propagate combustion. Spontaneous Combustion Self-Heating Packing Group III NEICVP1216E05 Page 6 of 9 Denka Performance Elastomer LaPlace, Louisiana Station No. Station Location/ Description of Sample Location Table 5. SUMMARY OF ANALYTICAL RESULTS Appendix B Photo Nos. Laboratory Sample Physical Description Flash Point Results (C1) Burn Rate Spontaneous Combustion S04A - liquid Poly Kettle #1 Strainer S04A solid S06A liquid S06A solid Poly Kettle #3 Strainer 1 C: degrees Celsius 2 N/A: not analyzed. 101_5151.JPG 101_5152.JPG 101_5156.JPG 101_5157.JPG White, opaque, non-viscous, emulsion, liquid Brown, black, orange, Clumps, Rubbery, Sticky, wet, soft, solid White, opaque, non-viscous, emulsion, liquid Brown, black, orange, Clumps, Rubbery, Sticky, wet, soft, solid < 60 C N/A > 60 C N/A N/A Did not propagate combustion. Self-Heating Packing Group III N/A Did not propagate combustion. Self-Heating Packing Group III Samples S01A, S04A, and S06A were multiphasic and consisted of a soft, rubbery solid, and a liquid/emulsion. The liquid phase of samples S01A, S04A, and S06A separated from the solids by force of gravity upon standing during transport from Denka to the NEIC laboratory. The liquid was separated from the solids by decanting, with some residual liquid remaining in the jar with the solids. Only the liquid phase of samples S01A, S04A, and S06A were analyzed for flash point. Burn rate testing following SW-846 Test Method 1030 was performed only on the solid phase of samples S01A, S04A, and S06A. A clean piece of stretch film was placed over the mould for each sample to prevent them from sticking while filling the mould. Aliquots of solid sample were removed from the top of the jar, then cut with scissors into small, pea-sized pieces. The pieces were placed in the mould and pressure was applied using the ceramic plate to compress the pieces slightly, causing them to stick together. Some air spaces remained after loading and packing the material into the mould. None of the samples supported or propagated combustion. Spontaneous combustion of the samples was not tested. The samples were exposed to air during collection, storage, and handling, and no signs of spontaneous combustion were NEICVP1216E05 Page 7 of 9 Denka Performance Elastomer LaPlace, Louisiana observed. Self-heating tests following SW-846 Test Method 1050 were performed on samples S01A, S04A, and S06A. Each sample was tested in a 100-millimeter (mm) cube as a combination of solid and residual liquid/emulsion. The 100-mm test consumed all of samples S01A and S04A. All samples tested positive, i.e., self-heated > 200 C in the 100-mm cubes, qualifying as Department of Transportation (DOT) packing group III. Figure 1 shows the temperature of S01A, S04A, and S06A in 100 mm cubes during testing. Only sample S06A was tested in a 25-mm (Figure 2) cube, confirming DOT packing group III. Since samples S01A and S04A could not be tested in the 25-mm cube, a determination for DOT packing group II for these samples could not be performed. Temperature (degrees Celcius) Samples S01A, S04A, and S06A in 100-mm cube 500 Oven Temp Sample S01A Sample S06A 400 Sample S04A 300 200 100 0 6/4/23 2:09 PM 6/4/23 8:09 PM 6/5/23 2:09 AM 6/5/23 8:09 AM Time (MM/DD/YY HH:MM) 6/5/23 2:09 PM Figure 1. The temperature of samples S01A, S04A, and S06A during testing in 100-mm cubes. NEICVP1216E05 Page 8 of 9 Denka Performance Elastomer LaPlace, Louisiana Sample S06A Triplicate in 25-mm Cube 210 Oven Temperature S06A Rep 1 170 S06A Rep 2 S06A Rep 3 130 Temperature (degrees Celsius) 90 50 10 6/5/23 4:33 PM 6/5/23 10:33 PM 6/6/23 4:33 AM 6/6/23 10:33 AM Time (MM/DD/YY HH:MM) 6/6/23 4:33 PM Figure 2. The temperature of sample S06A during testing in 25-mm cubes. Laboratory sample descriptions, observations, method modifications, and notes are documented in the project file. Pertinent photographs from the laboratory activities are provided in Appendix B, additional photos are in the project file. Photographs of the samples after Method 1050 testing are provided in Appendix C. NEICVP1216E05 Page 9 of 9 Denka Performance Elastomer LaPlace, Louisiana