### Attachment 2 – FGSARAN TTU



# Attachment 2

FGSARANTTU

40 CFR 63 MACT Performance Test Plan

The Dow Chemical Company Midland, Michigan

June 30, 2008

### Attachment 2 – FGSARAN TTU

Page 1 Table of Contents

MDEQ T EST 

### P LAN 

### C HECK 

### L IST

S ECTION D ESCRIPTION P AGE
1 Identification and Description of Source 2
2 Description of Air Pollution Control Equipment 4
3 Applicable Permit Number 5

4 Identification of Pollutants to be Measured 5
5 Description of Sampling Method 6
6 Detailed Sampling and Analytical Procedures 6
7 Sampling Conditions and Runs 9
8 Block Flow Diagrams 9

9 Estimated Flue Gas Condition 10
10 Projected Operation Conditions 11
11 Description of Process and Control Equipment to be Collected During Testing 11

12 Description of Any Monitoring Data to be Collected During the Test Period and Subsequently Reported 11
13 Chain-of-Custody Procedure 11
14 Field Quality Assurance and Quality Control Proc edures 12
15 Laboratory Quality Assurance and Quality Control Procedures 12

16 Test Personnel 14

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Introduction The Dow Chemical Company (Dow) is submitting this t est plan supporting performance testing to be conducted in order to demonstrate compliance with 4 0 CFR 63, Subpart GGG and FFFF standard requirements.

For consistency and to ensure that the proper test methods and procedures are implemented during testing, The Dow Chemical Company is submitting thi s test plan. The test plan is arranged according t o the Michigan Department of Environmental Quality (MDEQ) Air Quality (AQD) Format for Submittal of Source Emission Test Plans and Reports (February 20 08) guidance document.

http://www.michigan.gov/deq/0,1607,7-135-3310_4106_ 5778---,00.html

Sampling will be performed in strict accordance wit h 40 CFR 60, Appendix A test methods. There will be two variations. The inlet OHAP sample will not be corrected for spike recovery. This is a conservative measure because the inlet sample will not be corrected. This provides a worst cast denom inator
value for the DRE calculation. The inlet flow rate will be obtained by process instrumentation. EPA Methods 1 through 4 can not be safely performed on the inlet stream.

Section 1 – Identification and Description of Sourc e This section provides information pertaining to the identification and a brief description of the sour ce to be tested.

1 A

. C ONTACT I NFORMATION :

Jim McGee The Dow Chemical Company – Michigan Operations 1790 Building Midland, MI 48667 Phone: (989) 636-2435 Email: wmcgee@dow.com Jamie Dole The Dow Chemical Company – Michigan Operations 1790 Building Midland, MI 48667 Phone: (989) 636-5895 Email: jsdole@dow.com

1 B

. D ESCRIPTION OF I NDUSTRIAL P ROCESS The Dow Chemical Company operates a chemical manufa cturing facility in Midland, Michigan. This facility consists of numerous different chemic al manufacturing processes. These chemical manufacturing processes include the 827-Building Pr ocess Unit (FGRule290) that is subject to provision s of 40 CFR 63, Subpart GGG and the SARAN® Process Unit (EG35 & FGSARAN TTU) that is subject to the provision of Subpart FFFF.

The 827-Bldg pharmaceutical manufacturing facility located at 827-Building is subject to Subpart GGG. This facility uses the SARAN® thermal treatme nt unit (TTU) to control process vent emissions. T he

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SARAN® TTU incorporates a halogen/halide scrubbing system that includes a water scrubber column followed by a caustic scrubber column. The SARAN® TTU also controls streams from the SARAN® Resin manufacturing. Emissions include vinyl chloride mo nomer from one process train, which is subject to 4 0 CFR 41 Subpart F requirements, and vinylidene chlor ide monomer from the other process units, which wi ll be subject to the 40 CFR 63, Subpart FFFF – MON MAC T in 2008. Essentially all (99.9%) of the load to
the TTU comes from SARAN®.

For the purpose of conducting this performance test , the worst case emission scenario process vent emissions from both of the SARAN® manufacturing ope rations.

1 C

. T YPE AND Q UANTITY OF R AW AND F INISHED M ATERIALS USED IN P ROCESS The 827-Bldg pharmaceutical process unit can manufa cture a number of different pharmaceutical products on a batch campaign basis. The maximum ma ss loading of HAPs that 827-Bldg may generate and vent to the SARAN® TTU is insignificant compared to loading vented from SARAN® Resin manufacturing operations. Consequently, the worst case load to t his SARAN® TTU is based on the HAP and organicchlorine load from the SARAN® Resin manufacturing u nit. During testing, the worst case emission profi le will be based on vinylidene chloride manufacturing. Samples will be collected while operations are manufacturing vinylidene chloride resin products.

1 D

. D ESCRIPTION OF CYCLICAL OR BATCH OPERATIONS THAT IMP ACT EMISSION PROFILES : The SARAN® TTU is a leveraged control device. The 827-Building HAP and halogen/halide load is insignificant in comparison to the load from the SARAN® Resin manufacturing process. The load is l ess then 0.1% of the total HAP load to the TTU. The wo rst case emission profile will be based on SARAN® Resin manufacturing process.

The SARAN® Resin manufacturing uses the monomer vin ylidene chloride (1,1 dichloroethene:
C 2 H 2 Cl 2 ) and vinyl chloride (chloroethene: CH 2 CHCl). Worst case organic-halogen load to the TTU o ccurs during the recovery step. Sampling will be coordin ated so measurements are made during this step.

1 E

. O PERATING P ARAMETER R EQUIREMENTS : The table below outlines the basic operating parame ters used to regulate these process units.

Table 1.1 - Operating Parameter Summary Process Unit HAP Control Equipment Parameter Limit 827-Bldg PU HCl/Cl 2,

SARAN TM PU C 2 H 2 Cl 2 , CH 2 CHCl

HCl/Cl 2 SARAN® TTU

• firebox

• water scrubber

• caustic scrubber SARAN® TTU

• fire box: minimum temperature – 985 ° C

• scrubbing system: minimum flow rate – 35 gpm, minimum flow rate – 28 gpm minimum pH: 8

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1 F

. P ROCESS R ATE : The processing rate that results in the worst case emission profile occurs during the monomer recovery step. The worst case emission profile is discussed in greater detail in Attachment 3. Due t o the fact that the 827-Bldg PU makes up less than 0.1% of the HAP loading to the control device, only the SARAN®
Process Unit is considered.

Table 1.2 Processing Rate Summary Process Unit HAP Control Equipment Worst Case Emission Profile Scenario SARAN® PU HCl/Cl 2,

C 2 H 2 Cl 2 , CH 2 CHCl SARAN® TTU Vinylidene chloride SARAN® Resin manufacturing recovery step generates the worst case HCl/Cl 2 emission profile. Sampling to target 2 trains in this step.

Section 2 – Description of Air Pollution Control Eq uipment This section provides a brief description of air po llution control equipment associated with the process unit. The table below includes a brief des cription of the pollution control equipment used to comply with these standards. The description includes:

• control device description;

• operation parameters;

• rated capacity and efficiency; and

• maintenance history over the last 3 months.

Table 2 - Control Device Summary

Control Device Operating Parameter Capacity 3-Month Maintenance History SARAN® TTU – Burner minimum temperature = 985C 3 MM Btu/hr None

SARAN® TTU – water scrubber minimum flow rate = 35gpm 2000 CFM

SARAN® TTU – caustic scrubber minimum flow rate = 28 gpm

minimum pH = 8 2000 CFM A new blower is scheduled to be installed in June 2008. This blower should improve halogen scrubbing.

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Section 3 – Applicable Permit Number & Emission Sta ndards The table, below summarize the applicable SARAN® TT U permit citations.

Table 3 - Renewable Operating Permit: List of facil ities that vent to the SARAN® TTU
Permit Numbers: MI-ROP-A4033 Facility ROP Table Number Applicable Emission Standard 827-Building Table F-1.18

FGPHARMA Halide/Halogen Mass Removal Efficiency > 95% demonstrated during worst case emission profile conditions. 827-Building Table F-1.7 FGRule290 827-Buiding oper ates in compliance with Michigan Air Rule R 336.1290 (Rule 290). There is no applicable halide/halogen emission or removal standard specifi c to the SARAN® TTU process vents. 564-Building Table E-1.25 EG35 564-Building SARAN® Resin manufacturing operations has no applicable halide/halogen emission or remova l standard specific to the SARAN® TTU process vents. 564-Building Table F-1.4

FGSARANTTU 564-Building manages the SARAN® TTU in compliance with the provisions of FGSARANTTU. This table has no applicable halide/halogen emission or removal stand ard specific to the SARAN® TTU process vents. 564- Building Table F-1.9

FGVinylchloride 564 and 684-Buildings comply with 40 CFR 61, Subpar t A, Subpart F, and Subpart V; and 40 CFR 63, Subpart J – Polyvinyl Chloride MACT. These regulations have no applicable halide/halogen emission or removal stand ard specific to the SARAN® TTU process vents. 564-Building Table F-1.30 (proposed)

FGMON Halide/Halogen Mass Removal Efficiency > 99% & HAP >98% demonstrated during worst case emission profil e conditions.

Section 4 – Identification of Pollutants to be Meas ured The table below lists all the pollutants to be meas ured during this performance test.

Ta ble 4

- Pollutants to be Measured Control Device Pollutants SARAN® TTU • Hydrogen Chloride: HCl

• Chlorine: Cl 2

• 1,1-Dichloroethene (Vinylidene Chloride): C 2 H 2 Cl 2

• Chloroethene (Vinyl Chloride): CH 2 CHCl

• Methyl Propenoate (Methyl Acrylate): C 4 H 6 O 2

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Section 5 – Description of Sampling Method The table below provides a description of the sampl ing trains to be used to collect measurements and samples during the performance test. These methods will be performed according to the protocol listed in the appropriate Appendix A, 40 CFR 60 EPA Reference Test Method. Schematic diagrams can be found in
the EPA Reference Test Methods.

Table 5 - Sampling Method

Regulation Control

Device Sample/

Measurement Sampling

Location Sampling Method Water Scrubber Inlet EPA Method 26

Caustic Scrubber Inlet EPA Method 26 HCl, Cl 2

Caustic Scrubber

Outlet EPA Method 26A

EPA Method 1 - 4 Firebox Inlet EPA Method 18 – bag dilution

method. Flow by process instrumentation. C 2 H 2 Cl 2 , CH 2 CHCl, C 4 H 6 O 2 Caustic Scrubber

Outlet EPA Method 18 and Method 25A

– direct interface continuous sample extraction method. Subpart GGG & Subpart FFFF SARAN®

TTU

Flow Rate Caustic Scrubber Outlet EPA Methods 1, 2, 3 or 3A, and 4.

Measurements will be collected during Method 26A sampling.

Section 6 – Detailed Sampling and Analytical Proced ures The sampling and analytical procedure to be followe d during the performance test is designed to demonstrate compliance with the process vent standa rd requirement

As described in Section 1, the worst case emission profile with respect to OHAP & halogen/halide mass loading to the SARAN® TTU occurs during the SA RAN® Resin monomer recovery step. The performance test will be conducted while the proces s unit is in the operating step that generates the worst case emission profile. The sampling procedure incl udes the following steps:

1. Documenting the sample location dimensions and usin g the EPA Reference Method 1 Duct Dimension and Flow Disturbance Chart to determine t raverse points.

2. Collection volumetric flow rate measurements using EPA Reference Methods 1 thru 4 during Method 26A sampling at the caustic scrubber outlet location. Firebox inlet volumetric flow rate will be measured using process instrumentation. Safety concerns make using EPA Reference Methods 1 through 4 not possible.

3. For Method 26 and 26A sampling, one sampling train per location, per run, will be collected. A minimum of 3 runs will be collected. Each run will be a minimum of one hour in duration. Sampling trains per location will be coordinated so that col lection is simultaneous.

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4. For Method 18 inlet sampling, one sampling train pe r location, per run, will be collected in TedlarTM Bags diluted with nitrogen to prevent condensation. EPA Method 40 CFR 60, Appendix A, Method 18 paragraph 8.2.1 Integrated Bag Sampling and Anal ysis, will be followed during sample collection. A minimum of 3 runs will be collected. Each run will be a minimum of one hour in duration. Sampling trains per location will be coor dinated so that collection is simultaneous.

5. For Method 18 and 25A outlet sampling, exhaust gas will be continuously extracted from the stack and transported through a heat-traced sample line t o a mobile analytical laboratory. Sample gas will be routed to a gas chromatography system to measure 1,1-dichloroethylene and a flame ionization detector to measure total hydrocarbons.

The methods provided in the table below will be use d to collect samples for demonstration of compliance. Samples will be collected by an indepe ndent contractor.

Table 6 - Sampling and Analytical Plan 1 Sampling Location Sampling

Method Sampling Plan Analytical Method Analytical Plan Firebox Inlet Method 18 Single point sampling with TedlarTM bags nitrogen. Method 18 – Gas Chromatography

Method 18 Method 18 – Gas Chromatography Caustic Scrubber Exit Method

25A Sample gas will be routed

from the stack to a gas chromatography system and TOC CEMS located in a mobile laboratory located near the base of the stack. Method 25A – Total Hydrocarbons OHAP and MA stack gas concentration measurements will be made on-site using gas chromatography.

TOC concentration measurements will be made using an FID CEMS. Firebox Exit Method 26 Single point sampling with standard impingers to compensate for condensate. Method 26 – Ion Chromatography

Water Scrubber Exit Method 26 Single point sampling with standard impingers to compensate for condensate. Method 26A – Ion Chromatography

Method 26A Method 26A – Ion Chromatography Samples will be shipped off site to independent laboratories for analysis.

Caustic Scrubber Exit Methods 1,

2, 3, & 4 Isokinectic sample

collection. Method 1, 2, 3, & 4 Flow Rate Measurements will be collected and summarized by the sampling firm.

1 June 30, 2008 – Page Revised. Table 6 Sampling Lo cation description updated for the second and fifth rows to clarify the sampling location, and the Analytical Plan entr y for the first row was updated to read “OHAP” inst ead of “HAP”.

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Bag Dilution Technique Method 18, "Measurement of Gaseous Organic Compound Emissions by Gas Chromatography" will
be used to determine the concentrations of OHAP in the sample gas. Method 18 uses a gas chromatograph equipped with a flame ionization detector (GC/FID) to measure hydrocarbon compounds. Inlet samples wi ll be measured using the Tedlar bag sampling procedure s describe in Method 18 Section 8.2.1.4.2, Integrat ed Bag Sampling and Analysis, Second Alternative Proce dure. This procedure involves collecting an integr ated sample in a Tedlar bag that has been pre-filled wit h a known amount of nitrogen. A known amount of sample to be metered into the bag. This procedure will provide the desired dilution over the 1-hour p eriod test run period. The bags will be analyzed on-site using a GC/FID.

The GC to be used for the incinerator sampling will be equipped with a appropriate column and a flame ionization detector (FID). The FID signals will be processed using a PeakSimple chromatography data system (or equivalent system) operated out of a Win dow 2000 based PC system. The GC column ovens will be operated using a temperature program to provide adequate separation of the compounds of interest an d timely elution of heavier compounds. Nitrogen will be used as the carrier gas. All instrument compon ents in contact with the sample gas will be made of stainle ss steel, Teflon, or glass and will be heated to pr event condensation. The contents of the sample loop will be injected onto the GC columns and the sample ana lysis will be initiated approximately every 14 minutes. Certified compressed gas standards will be used to
calibrate the GC.

The calibration gases will provide information to b e used to speciate, identify specifically and quant itate compounds in the samples. The GC will be calibrate d directly using these gases to establish linearity across the ranges of concentrations found in the stack gas . Linearity of the FID response will be determined using three different calibration gas concentrations. A least-squares equation (y = mx + b) will be calcula ted from
this calibration.

The mid-level gas for each compound will be analyze d after the bags are analyzed. If this post-test c heck is not within 5% of the initial calibration curve, the three-point calibration will be repeated and the c ombined pre and post-test calibration data will be used to calculate concentrations. If this post-test check is within 5% of the initial calibration curve, the initial calib ration curve will be used to calculate concentratio ns. Due to the high level of the sample, spiking of the bags w ill not be performed. A low spike recovery would a llow a correction to increase the sample results and thus increase the inlet loading, therefore assuming 100 percent recovery is a conservative approach for the inlet s amples and DRE determinations. The concentrations of hydrocarbons in the samples will be corrected to a dry basis for reporting purposes.

Calibration gas certification sheets, sample chroma tograms, the sample run log, and calibration QA/QC will be included in the appendix of the report.

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Section 7 – Sampling Conditions and Runs The table below summarizes the number and length of sampling runs which will constitute a complete test.

Table 7

- Test Condition Summary 2

Control Device Condition

Number Runs Operating Condition Summary SARAN® TTU 1 3 Samples will be collected during max imum SARAN® Resin recovery step – target 2 units in step. A ru n will consist of one sampling train. One sampling train will be located at each of the four sampling locations.

Section 8 – Block Flow Diagrams The following figures illustrate block flow diagram for this process unit. Dimensioned sketches showing all sampling ports in relation to breeching and upstream and downstream gas flow disturbances are illustrated in Figure 8. Flow rate measurements wi ll be made at traverse points according to the duct diagram grid below.

2 June 30, 2008 – Page Revised. Table 7 Operating C ondition Summary column heading and information was updated to correct two typographical errors. Heading on la st column changed from “Condition Operation Conditi ons Summary” to “Operating Condition Summary,” and the number of samples taken in this column was changed from “thr ee” to “four”.

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Page 10 Figure 8 - SARAN® TTU Schematic Diagram

Fire Tube

Flow Caustic Scrubber Sampling Ports

Quench

HCl/Cl2 Inlet Sample Port Outlet Sample Point Data: Diameter = 8.5 in Velocity ~ 34.7 ft/sec Flow Rate ~ 49,000 acfhr Flow Rate ~ 49,000 scfhr Temp ~ 70 F H2O ~ 2 % CO2 ~ 3% O2 ~ 15% N2~ 82% Water Scrubber

Packing

OHAP Inlet Sample Port

SARAN® Resin Production 827-Bldg Process Unit SARAN® TTU 827-Close Vent System water scrubber caustic

scrubber atmosphere

quench column

Section 9 – Estimated Flue Gas Condition The Table below summarized the flue gas conditions.

Table 9 - Estimated Flue Gas Conditions Process Stack ID Flue Gas Parameter FGSARAN TTU SV35101 Gas velocity ~ 2000 afpm Flow rate ~ 49,000 acfhr & scfhr (note, minimum sta ndard correction) Temperature ~ 70 ° F Major gas stream component concentrations: ~2% H 2 O, ~4% CO 2 , ~ 15% O 2 , and ~ 81% N 2

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Page 11 Section 10 – Process Operation Conditions The projected process operating conditions during w hich the performance test will be run are
summarized in the table below.

Table 10 - Projected Process Operation Conditions Process Projected Process Operating Condition FGSARANTTU Samples collection will coincide with wo rst case the halide/halogen worst case emission profile. SARAN® Resins recovery step – target 2 units in step for w orst case HAP load

Section 11 – Description of Process and Control Equ ipment to be Collected During

Testing A description of process and control equipment to b e collected during the performance test is
summarized in the table below.

Table 11 - Process Data Collected During Testing Operating Parameters Process Parameter Unit minimum or maximum Note 827-Bldg (SARAN® TTU) process step

SARAN®-TTU temperature SARAN®-TTU quench flow SARAN®-TTU water flow SARAN®-TTU caustic flow SARAN®-TTU pH NA

° F
gpm gpm gpm NA NA minimum NA minimum minimum minimum Process step disclosure

may be confidential business information requiring separate cover disclosure

Section 12 – Description of Any Monitoring Data to be Collected During the Test

Period and Subsequently Reported (e.g., CEMS) This section is not applicable to this performance test. This process unit is not required to incorporate any monitoring data collection such as continuous emission monitoring systems (CEMS) into unit operations.

Section 13 – Chain-of-Custody Procedure The independent firm contracted to manage and execu te sample collection, sample analysis, and report generation will manage Chain-of-Custody (COC ) procedure use. Samples will be logged prior to shipment. A copy of the Chain of Custody will rema in with Dow and a copy will be sent with the sample s, to the analytical laboratory. Copies of the COCs w ill be provided in the test report appendix.

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Page 12 Section 14 – Field Quality Assurance and Quality Co ntrol Procedures Specific data quality objectives for each measureme nt are presented in the table below. The sampling and analytical procedures to be used are s tandard EPA Methods. Each method has minimum quality control checks. Adherence to the prescribe d QC procedures will ensure data quality meets appl icable
method standards.

Table 14 - Process Field QAQC Summary Sample Matrix Target

Compound EPA Method Field QAQC Methodology HAP (C 2 H 2 Cl 2 , CH 2 CHCl) & VOC (C 4 H 6 O 2 ) Method 18

THC Method 25A System Calibration Line Bias checks Response time

Method 26 Gas

HCl/Cl 2 Method 26A Filed Blanks:

• HCl: H 2 SO 4 Impinger Solution;

• Cl 2 : NaOH Impinger Solution

Section 15 – Laboratory Quality Assurance and Quali ty Control Procedures

Laboratory QAQC Personnel performing field and laboratory activitie s will be responsible for continually monitoring compliance with the quality assurance objectives ou tlined in the applicable EPA Method.

All sampling and analytical procedures are EPA or A STM published methods. Calibration of analytical instrumentation to acceptable limits wil l be in accordance with the applicable EPA or ASTM method. Calibration and sample spike analytical re cords and associated log notes will be supplied in the appendix to the final test report.

The TRC project manager will be responsible for con ducting a review to determine whether all requirements for analytical activities have been fu lfilled and that complete records exist. Each anal ytical data set will be peer reviewed and then checked by a QA/QC officer. A summary of applicable QAQC checks will be supplied in the final test report. This summary will include:

• Test Method;

• Calibration Results;

• QA Spike Recovery Results;

• Field Blank Results; and

• Duplicate Analysis Results.

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Page 13 To ensure accurate results, strict quality assuranc e and control measures will be followed. All testi ng will be performed following standard EPA protocols as outlined in Title 40 Code of Federal Regulations Part 60 Appendix A. The test data will be thoroughly do cumented and checked for completeness.

Method 18 Inlet - Certified compressed gas standard s will be used to calibrate the GC. The calibration gases provided information used to sepa rate-, identify specifically and quantitate compoun ds in the samples. The GC will be calibrated directly us ing these gases to establish linearity across the r anges of concentrations found in the stack gas. Linearity o f the FID response will be determined using three d ifferent calibration gas concentrations. A least-squares eq uation (y = mx + b) will be calculated from this ca libration. The mid-level gas will be analyzed before and after each test run. If this post-test check is not wit hin 5% of the initial calibration curve, the three-point cali bration will be repeated and the combined pre and p ost-test
calibration data will be used to calculate concentr ations. The concentrations of hydrocarbons in the samples will be corrected to a dry basis for reporting purp oses. If this post-test check is within 5% of the initial calibration curve, the initial calibration curve wi ll be used to calculate concentrations.

Due to the high level of the sample, spiking of th e inlet bags will not be performed. A low spike recovery would allow a correction to increase the s ample results and thus increase the inlet loading, therefore assuming 100 percent recovery is a conservative app roach for the inlet samples and DRE determinations. All other bags will be spiked per Method requirements.

Corrective Action Any error, deficiency, deviation, or QC result that falls outside EPA Method established acceptance criteria will be investigated. The investigation o f the issue and any corrective actions will be docu mented and reported to the project management.

Data Acceptance To assess overall data quality, the completed data set for a compliance burn will be reviewed by the project manager. The project manager will review a nalytical data for completeness and preparing a QAQ C summary report for submittal in the final test repo rt.

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Page 14 Section 16 – Test Personnel Dow will contract TRC Environmental to perform this test. TRC will manage and execute sample collection, sample analysis, QAQC, and report gener ation. Dow’s internal stack sampling resource is managed by Chuck Glenn. Mr. Glenn is a subject mat ter expert and will assist Dow in overseeing the execution of this test program.

Chuck Glenn The Dow Chemical Company Texas Operations 2301 Brazosport Bldg Freeport, TX 77541 Phone: (979) 238-9109 Email: CEGlenn@dow.com Mike Krall TRC Environmental 2100 Kramer Lane, Suite 800 Austin, TX 78758 Phone: (512) 684-3417 Email: mkrall@trcsolutions.com