### POLYCYCLIC AROMATIC HYDROCARBONS AND MERCURY EMISSION SUMMARY REPORT EAF No. 12 SCRUBBER EAF No. 1 MAIN BAGHOUSE ERAMET MARIETTA , INC. MARIETTA, OHIO

Prepared for:

Eramet Marietta, Inc. P.O. Box 299 State Route 7 South Marietta, Ohio 45750

- 0299

Prepared by:

Environmental Quality Management, Inc. 1800 Carillon Boulevard Cincinnati, Ohio 45240 (513) 825

- 7500 Fax (513) 825

- 7495
www.eqm.com

EQ PN: 050352.0031

November 2014

### ii CONTENTS Section Page

1. Introduction

................................ ................................ ................................ ...................... 1

- 1

2. Summary of Test Results

................................ ................................ ................................ . 2

- 1 2.1 EAF No. 12 Scrubber

................................ ................................ .............................. 2

- 1 2.1.1 Stack Gas Conditions and Pollutant Emissions

................................ .......... 2

- 1 2.1.1.1 Mercury

................................ ................................ ........................ 2

- 1 2.1.1.2 PAHs

................................ ................................ ............................ 2

- 2 2.2 Furnace 1 Main Baghouse

................................ ................................ ...................... 2

- 4 2.2.1 Stack Gas Conditions and Pollutant Emissions

................................ .......... 2

- 5 2.2.1. 1 Mercury

................................ ................................ ........................ 2

- 5 2.2.1.2 PAHs

................................ ................................ ............................ 2

- 5

3. Sampling and Analytical Procedures

................................ ................................ ............... 3

- 1 3.1 Location of Measurement Sites

................................ ................................ .............. 3

- 1 3.2 Stack Gas Volumetric Flow Rate

................................ ................................ ............ 3

- 1 3.3 Stack Gas Dry Molecular Weight

................................ ................................ ........... 3

- 1 3.4 Stack Gas Moisture Content

................................ ................................ ................... 3

- 2 3.5 Mercury

................................ ................................ ................................ ................... 3

- 2 3.6 PAHs

................................ ................................ ................................ ....................... 3

- 3

4. Process Operation/Sampling Locations

................................ ................................ ........... 4

- 1

5. Quality Assurance and Quality Control

................................ ................................ ........... 5

- 1 5.1 Calibration Procedures and Frequency

................................ ................................ ... 5

- 1 5.2 Field Blanks

................................ ................................ ................................ ............ 5

- 1

### iii APPENDICES

Appendix A Calculations Appendix B Field Data Appendix C Analytical Data Appendix D Process Data Appendix E Quality Assurance and Quality Control

FIGURES

No. Page

Figure 3

- 1

. EPA Method 30B

................................ ................................ ................................ .... 3

- 3 Figure 3

- 2

. CARB Method 429 Sampling Train

................................ ................................ ....... 3

- 4 Figure 4

- 1. Sampling Locations

................................ ................................ ................................ 4

- 1

TABLES

No. Page

Table 1

- 1. General Scope Of Work

................................ ................................ .......................... 1

- 1 Table 2

- 1. Summary of Furnace Exhaust Conditions Furnace 12 Sc rubber

– Mercury

.......... 2

- 2 Table 2

- 2. Summary of Furnace Exhaust Cond itions Furnace 12 Scrubber

– PAH

................ 2

- 3 Table 2

- 3

. Summary of Furnace Exhaust Conditions Furnace 1 Main Baghouse

– Mercury

. 2

- 5 Table 2

- 4

. Summary of Furnace Exhaust Conditions Furnace 1 Main Baghouse

– PAHs

...... 2

- 6 Table 4

- 1. Sampling Location Parameters

................................ ................................ ............... 4

- 2 Table 4

- 2

. Furnace No. 12 Process Operations

................................ ................................ ........ 4

- 2 Table 4

- 3

. Furnace No. 1 Process Operations

................................ ................................ .......... 4

- 2 Table 5

- 1. Field Equipment Calibration Summary

................................ ................................ .. 5

- 2 Table 5

- 2. Field Checks of Sampling Equipment

................................ ................................ .... 5

- 2

### 1

- 1 1. INTRODUCTION

Eramet Marietta Inc. (EMI) conduc ted a n emission measurement program to characterize
polycyclic aromatic hydrocarbon ( PAH) and mercury emissions from electric arc furnace 1
(main baghouse outlet) during the production of ferromanganese (FeMn) and furnace 12
(scrubber outlet) during the production of silicomanganese (SiMn). Emission measurements
were collected October 15 and 16, 2014 at the Marietta, Ohio facility

.

The overall goal of the tests wa s to supplement data from previous tests and thereby gain
a better understanding of the range and variability of actual emissions during production , using

test measurement method 30B for Hg as specified by US EPA and method 429 for PAHs as
specified in Cali fornia Air Resources Board (CARB). The methodology follows a prior
Information Collection Request (ICR) by USEPA.

Environmental Quality Management, Inc. (EQ) was contracted by EMI to obtain the
emission measurement data and coordinate the analysis and re porting of the results . A summary
of the general scope of work as indicated is provided in Table 1

- 1.

Table 1

- 1

. General Scope Of Work

Source Sampling

Location Target Analyte USEPA Reference Method EAF No. 12 Scrubber Outlet PAH s CARB Method 429

Outlet Flow, O 2 

### /CO 2 

### 1, 2, 3 Outlet Moisture 4 Outlet Hg 30B EAF No. 1 Main Baghouse Outlet PAH s CARB Method 429

Outlet Flow, O 2 

### /CO 2 

### 1, 2, 3 Outlet Moisture 4 Outlet Hg 30B

### 2

- 1 2. SUMMARY OF TEST RESU LTS

2.1 EAF No. 12 Scrubber

On October 16, 2014, the EAF No. 12 scrubber exhaust was sampled to determine the
emission profile for Hg and PAHs. Furnace 12 is a continuous furnace that was operating in a
double tap scenario where tapping occurred approximately every 80 min utes. Each test run
encompassed approximately 7 0 minute s . Since this is a continuous furnace, raw material is
added to the mix throughout the melting process and is tapped at the appropriate time. Each run
incorporated a tap as well as the same amount m elting time and raw material addition.
Furnace No. 12 scrubber was sampled at the outlet stack for all pollutants , flow, and

O 2 

### /CO 2 

### concentrations during the production of SiMn . The outlet sampling location was located

in a circular duct downstream of the scrubber

.

2.1 .1 Stack Gas Conditions and Pollutant Emissions

2.1.1.1 Mercury

Table 2

- 1 details the furnace exhaust conditions measured under each mercury (Hg) test run. Results are summarized for stack gas velocity (feet per second), volumetric flow rate
(actual and dry standard cubic feet per minute), stack temperature, moisture, and composition
(carbon dioxide and oxygen percentages). Stack gas conditions we re consistent for each

condition on a run

- by

- run basis. Paired mercury sorbent tubes were run

, and t he second tube was
spiked for each run for QA analysis. Results for t he unspiked tube are p rovided. The mercury
results are reported in the following unit s : μg/dscm, lb/hr

, and lb/ton of metal produced.
Recovery efficiency for all runs met method QA requirements.

### 2

- 2 Table 2

- 1

. Summary of Furnace Exhaust Conditions

Furnace 12 Scrubber

– Mercury

Date: October 16, 2014 Eramet

– Marietta, Ohio
Run No. Average FCE12

- US

- 1 FCE12

- US

- 2 FCE12

- US

- 3 FCE12

- US

- 4 Date Oct. 16, 2014 Oct. 16, 2014 Oct. 16, 2014 Oct. 16, 2014 Time 1010

- 1120 1158

- 1308 1341

- 1451 1510

- 1620 Stack Gas Velocity, fps a 59 60 59 59 56 Volumetric Flow Rate, acfm b 175,370 177,425 174,399 174,156 175,731 Volumetric Flow Rate, dscfm c 142,579 144,279 143,841 142,969 143,566 Temperature, °F 127 128 127 130 128 Moisture, % 6.8 6.7 5.5 5.5 6.3 CO 2 , % 0 0 0 0 0 O 2 , % 20.8 20.8 20.8 20.8 20.8 Mercury
μg /dscm lbs/hr lbs/ton Metal 10.11 5.78 E

- 03 6.09 E

- 0 4 10. 27

5.94 E

- 03 6.25E

- 04 9.05

5.15 E

- 03 5.42E

- 04 9.58

5.42E

- 03 5.70E

- 04 9 .7 5

5.57 E

- 03 5.87E

- 04

a Feet per second.
b Actual cubic feet per minute.

c Dry standard cubic feet per minute.

.



### 2.1.1.2 PAHs

Table 2

- 2 details the furnace exhaust conditions measured under each CARB

Method 429 for PAHs. Results are summarized for stack gas velocity (feet per second),
volumetric flow rate (actual and dry standard cubic feet per minute), stack temperature, moisture,

and c omposition (carbon dioxide and oxygen percentages). Stack gas conditions were consistent

for each condition on a run

- by

- run basis. Gas composition for O 2 

### and CO 2 

### were analyzed during

each run via Method 3A. The results are reported in : ng/ dscm, lb/hr an d lb/ton of metal
produced

.

### 2

- 3 Table 2

- 2. Summary of Furnace Exhaust Conditions

Furnace 12 Scrubber

– PAHs

Date: October 16, 2016 Eramet

– Marietta, Ohio
Site/Run No. Average 12

- 429

- 1 12

- 429

- 2 12

- 429

- 3 12

- 429

- 4 Date Oct. 16, 2014 Oct. 16, 2014 Oct. 16, 2014 Oct. 16, 2014 Time 1010

- 1123 1157

- 1311 1332

- 1445 1509

- 1622 Stack Gas Velocity, fps a 58.9 59. 7 58.6 58.7 58.9 7 Volumetric Flow Rate, acfm b 175,354 177,474 174,420 174,697 175,486 Volumetric Flow Rate, dscfm c 142,702 144,255 143,914 141,110 142,995 Temperature, °F 127 128 127 130 128 Moisture, % 6.7 6.7 5.5 7.0 6.49 CO 2 , % 0 0 0 0 0 O 2 , % 20.5 20.5 20.5 20.5 20.5 Naphthalene ng/dscm d 2.14E+04 1.69E+04 2.28E+

- 04 2.26E+

- 4 2.09E+04

1

– Methylnaphthalene ng/dscm 4.92E+

- 3 8.68E+03 6.82E+

- 3 6.03E+03 6.61E+03

2

– Methylnaphthalene ng/dscm 7.22E+03 1.16E+04 9.45E+

- 3 8.45+03 9.18E+03
Acenaphthylene ng/dscm 7.58E+03 3.06E+03 7.75E+03 9.84E+03 7.06E+03
Acenaphthene ng/dscm 9.11E+02 1.35E+03 1.20E+03 1.06E+03 1.13E+03

Fluorene ng/dscm 1.40E+03 1.98E+03 1.81E+03 1.59E+03 1.69E+03

Phenanthrene ng/dscm 1.86E+04 1.85E+04 3.82E+04 2.24E+04 2.44E+04

Anthracene ng/dscm 4.41E+03 3.01E+03 6.82+03 5.41E+03 4.91E+03

Fluoranthene ng/dscm 1.88E+04 9.85E+03 3.33E+04 1.57E+04 1.94E+04
Pyrene ng/dscm 1.37E+04 6.63E+03 2.42E+04 1.19E+04 1.41E+04
Benzo (a) Anthracene ng/dscm 1.81E+03 2.79E+03 1.81E+03 1.69E+03 2.03E+03
Chrysene ng/dscm 7.07E+03 8.33E+03 5.47E+03 2.68+03 5.89E+03
Benzo (b) Fluoranthene ng/dscm 2.65E+03 4.41E+03 2.61E+ 03 1.63E+03 2.83E+03
Benzo (k) Fluoranthene ng/dscm 9.98E+02 2.19E+03 9.71E+02 6.44E+02 1.20 E+03
Benzo (e) Pyrene ng/dscm 1.30E+03 2.31E+03 1.11E+03 8.55E+02 1.39 E+03

### 2

- 4

Table 2

- 2

. (continued)
Site/Run No. Average 12

- 429

- 1 12

- 429

- 2 12

- 429

- 3 12

- 429

- 4 Benzo (a) Pyrene ng/dscm 4.25E+02 3.81E+02 2.63E+02 3.51E+02 3.55 E+02
Perylene ng/dscm 5.48E+01 7.33E+01 3.12E+01 6.85E+01 5.69 E+01
Indeno (1, 2, 3

– cd) Pyrene ng/dscm 5.43E+02 9.76E+02 3.36E+02 5.05E+02 5.90 E+02
Dibenzo (a, h) Anthracene ng/dscm 1.06E+02 2.70E+02 6.66E+01 1.05E+02 1.37 E+02
Benzo (ghi) Perylene ng/dscm 4.20E+02 6.27E+02 2.73E+02 4.16E+02 4.34 E+02

Total PAHs ng/dscm lbs/hr lbs/ton Metal 1.14 E+05 6.11 E

- 02 0.01 1.04 E+05

5.61 E

- 02 0.01 1.65 E+05

8.90 E

- 02 0.01 1.14 E+05

6.01 E

- 02 0.01 1.24 E+05

6.66 E

- 02 0.01 19

- PAH d ng/dscm lbs/hr lbs/ton Metal 1.09 E+05 5.84 E

- 02 0.01 9.52E+04

5.14E

- 02 0.01 1. 59E+05

8.54E

- 02 0.01 1. 08E+05

5.70E

- 02 0.01 1 .18E+05

6.30 E

- 02 0.01

a Feet per second.
b Actual cubic feet per minute.

c Dry standard cubic feet per minute.
d 19

- PAH Excludes 1

- Methylnaphthalene



### 2. 2 Furnace 1 Main Baghouse

O n October 15, 2014 , the Main Baghouse (MB 1 ) controlling emissions from the No. 1

EAF was sampled while producing FeMn to determine the emission profile for PAHs and Hg

. Furn ace 1 is a continuous furnace that was operating in a double tap scenario where tapping
occurred approximately every 120 minutes. Each test run encompassed a 90 minute period.
Since this is a continuous furnace, raw material is added to the mix throughou t the melting
process and is tapped at the appropriate time. Each run incorporated a tap as well as the same
amount of time of melting and raw material addition.

The Furnace 1 MB was sampled at the outlet stack for all pollutants, flow, and O 2 

### /CO 2 

### concentrations. The outlet sampling location was located in a circular duct downstream of the
baghouse. Data was not corrected for detected blank amounts . The blank detected quantity was

well below the analytical result.

### 2

- 5

2.2.1 Stack Gas Conditions an d Pollutant Emissions

2. 2.1 .1 Mercury

Table 2

- 3 details the furnace exhaust conditions measured under each mercury (Hg) test
run. Results are summarized for stack gas velocity (feet per second), volumetric flow rate
(actual and dry standard cubic feet p er minute), stack temperature, moisture, and composition
(carbon dioxide and oxygen percentages). Stack gas conditions were consistent for each

condition on a run

- by

- run basis. Paired mercury sorbent tubes were run , and t he second tube was
spiked for eac h run for QA analysis. Results for t he unspiked tube are provided. All runs met
the recovery efficiency QA requirements.

Table 2

- 3

. Summary of Furnace Exhaust Conditions Furnace 1 Main Baghouse

– Mercury

Date: October 15, 2014 Eramet

– Marietta, Ohio
Run No. Average MB

- US

- 1 MB

- US

- 2 MB

- US

- 3 MB

- US

- 4 Date Oct.15, 2014 Oct.15, 2014 Oct.15, 2014 Oct.15, 2014 Time 0820

- 0950 1020

- 1150 1220

- 1350 1420

- 1550 Stack Gas Velocity, fps a 49.5 48.3 46.9 48.4 48.3 56 Volumetric Flow Rate, acfm b 233,394 227,807 221,163 227,892 227,455 Volumetric Flow Rate, dscfm c 185,008 172,103 166,240 177,086 174,450 Temperature, °F 170.8 200.5 206.6 184.8 191 Moisture, % 2.5 2.7 2.3 2.3 2.5 CO 2 , % 0 0 0 0 0 O 2 , % 20.8 20.8 20.8 20.8 20.8 Mercury μg/dscm lbs/hr lbs/ton Metal 92.75 6.58 E

- 02 6.04E

- 03 135.4 1

8.95 E

- 02 8.21E

- 03 105.70

6.72 E

- 02 6.17E

- 03 69.38

4.70 E

- 02 4.31.03 100.81

6.74E

- 02 6.18

- 03

a Feet per second.
b Actual cubic feet per minute.

c Dry standard cubic feet per minute.
d Run 2 did not meet the m e thod QA requirements and is not included in the average.



### 2.2

. 1. 2 PAHs

Table 2

- 4 details the furnace exhaust conditions measured under each CARB Method 429
for PAHs. Results are summarized for stack gas velocity (feet per second), volumetric flow rate

### 2

- 6

(actual and dry standard cubic feet per minute), stack temperature, moisture, and composition
(carbon dioxide and oxygen percentages). Stack gas conditions were consistent for each

condition on a run

- by

- run basis. Gas composition for O 2 

### and CO 2 

### were analyzed dur ing each run

via Method 3A. The results are reported in the units specified in : ng/dscm, lb/hr and lb/ton of
metal produced. All test runs met the minimum sample volume requirement of 1 m 3



### .

Table 2

- 4

. Summary of Furnace Exhaust Conditions

Furnace 1 Main Baghouse

– PAHs Date : October 15, 2014 Eramet

– Marietta, Ohio

Site/Run No. Average MB

- 429

- 1 MB

- 429

- 2 MB

- 429

- 3 MB

- 429

- 4 Date Oct. 15, 2014 Oct. 15, 2014 Oct. 15, 2014 Oct. 15, 2014 Time 0820

- 0954 1020

- 1155 1220

- 1355 1420

- 1553 Stack Gas Velocity, fps a 48.8 47.6 46.2 47.6 47.5 Volumetric Flow Rate, acfm b 229,839 224,327 217,779 224,270 224,054 Volumetric Flow Rate, dscfm c 187,907 174,827 168,899 180,391 178,006 Temperature, °F 171 201 207 185 191 Moisture, % 2.5 2.7 2.3 2.0 2.4 CO 2 , % 0.00 0.00 0.00 0.00 0.00 O 2 , % 20.5 20.5 20.5 20.5 20.5 Naphthalene ng/dscm d 2.78E+05 3.00E+05 2.30E+05 2.29E+05 2.59E+05

1

– Methylnaphthalene ng/dscm 3 .26E +04 4.89E+04 2.89E+04 3.29E+04 3.58E+04

2

– Methylnaphthalene ng/dscm 4.42E+04 6.74E+04 3.78E+04 4.69E+04 4.91E+04
Acenaphthylene ng/dscm 9.04E+04 1.23E+05 5.28E+04 8.50E+04 8.78E+04
Acenaphthene ng/dscm 1.89E+04 2.84E+04 1.37E+04 1.38E+04 1.87E+04

Fluorene ng/dscm 4.15E+04 7.92E+04 2.92E+04 4.62+04 4.90E+04

Phenanthrene ng/dscm 1.19E+06 1.04E+06 1.12E+06 9.03E+05 1.06E+06

Anthracene ng/dscm 2.03E+05 1.33E+05 1.47E+05 1.10E+05 1.48E+05

Fluoranthene ng/dscm 2.14E+06 3.13E+06 2.89E+06 1.36E+06 2.38E+06
Pyrene ng/dscm 1.54E+06 2.32E+06 2.11E+06 9.42E+05 1.73E+06
Benzo (a) Anthracene ng/dscm 1.58E+05 3.73E+05 4.98E+05 1.17E+05 2.86E+05
Chrysene ng/dscm 2.79E+05 8.18E+05 1.04E+06 3.04E+05 6.11E+05
Benzo (b) Fluoranthene ng/dscm 8.33E+04 2.74E+05 4.33E+05 1.17E+05 2.27E+05
Benzo (k) Fluoranthene ng/dscm 2.43E+04 7.33E+04 1.46E+05 3.91E+04 7.06E+04

### 2

- 7 Site/Run No. Average MB

- 429

- 1 MB

- 429

- 2 MB

- 429

- 3 MB

- 429

- 4 Benzo (e) Pyrene ng/dscm 3.07E+04 9.75E+04 164E+05 4.94E+04 8.54E+04
Benzo (a) Pyrene ng/dscm 1.34E+04 3.95E+04 8.52E+04 1.98E+04 3.95E+04
Perylene ng/dscm 2.41E+03 5.76E+03 145E+04 4.10E+03 6.69E+03
Indeno (1, 2, 3

– cd) Pyrene ng/dscm 4.95E+03 1.50E+04 2.84E+04 7.38E+03 1.39E+04
Dibenzo (a, h) Anthracene ng/dscm 7.03E+02 2.70E+03 4.15E+03 1.30E+03 2.21E+03
Benzo (ghi) Perylene ng/dscm 4.33E+03 1.16E+04 1.94E+04 5.54E+03 1.02E+04

Total PAHs ng/dscm lbs/hr lbs/ton Metal 6.18E+06 4.35 0.40 8.99E+06

5.88 0.54 9.09E+06

5.74 0.53 4.44E+06

3.00 0.27 7.17E+06

4.74 0.44 19

- P AH d ng/dscm lbs/hr lbs/ton Metal 6.15E+06 4.32 0.40 8.94E+06

5.85 0.54 9.06E+06

5.73 0.53 4.40E+06

2.97 0.27 7.14E+06

4.72 0.43

a Feet per second.
b Actual cubic feet per minute.

c Dry standard cubic feet per minute.
d 19

- PAH Excludes 1

- Methylnaphthalene

### 3

- 1 3. SAMPLING AND ANALYTI CAL PROCEDURES

The sampling and analytical procedures used in this test program conformed to the prior

USEPA ICR , the test protocol and the EPA Reference Methods as published in the Federal
Register . A brief description of each method follows.

3.1 Location of Measurem ent Sites

EPA Method 1, “ Sample Velocity Traverses for Stationary Sources

, ” was used to select
representative measurement sites at each sampling location

. The s ampling locations are

described in Section 4.

3.2 Stack Gas Volumetric Flow Rate

EPA Method 2, “Determination of Stack Gas Velocity and Volumetric Flow Rates,” was
used at each location to determine stack gas v olumetric flow rates. Type “S” pitot tubes meeting
the EPA specifications and an inclined manometer were used to measure velocity pressu res. A calibrated Type “K” thermocouple attached directly to the pitot tube was used to measure stack
gas temperature. The stack gas velocity was calculated from the average square root of the stack
gas velocity pressure, average stack gas temperature, s tack gas molecular weight, and absolute
static pressure. The volumetric flow rate is the product of velocity and stack cross

- sectional

area.

3.3 Stack Gas Dry Molecular Weight

EPA Reference Method 3 , “Determination of Oxygen and Carbon Dioxide

Concentr ations in Emissions was used to determine oxygen and carbon dioxide content of the
stack gas. Integrated tedlar bag samples were collected at each exhaust during each test run and
analyzed with the Fyrite analyzer.

### 3

- 2

3.4 Stack Gas Moisture Content

EPA R eference Method 4, “Determination of Moisture Content in Stack Gases,” was
used to determine stack gas moisture content. T his method was conducted in conjunction with

each Carb 429 sampling run . The initial and final contents of all impingers were measu red
gravimetrically.

3. 5 Mercury

Mercury concentrations and emissions were sampled and analyzed for following Method 30B, “Determination of Total Vapor Phase Mercury Emissions From Coal

- Fired Combustion Sources Using Carbon Sorbent Traps.” This method is designed to measure the mass
concentration of total vapor phase Hg in flue gas, including elemental Hg (Hg o ) and oxidized
forms of Hg (Hg +2 ), in micrograms per dry standard cubic meter. The sampling system used
two paired sorbent tubes; one tube was s piked (3,800 nanograms for FCE 1 and 1,000 ng for

FCE 12 ) to determine recovery efficiencies. Each pair of tubes was sampled simultaneously,
with a similar sample target flow rate, at approximately 1 liter per minute. Leak checks were
performed before an d after each sampling run. After each sampling run, the sorbent traps were
properly labeled, sealed in plastic tubes, and prepared for shipment to the lab. Cold Vapor
Atomic Absorption (CVAA) was used to perform sample analyses. Figure 3

- 1 is a schemati c of
the sampling system.

### 3

- 3 Figure 3

- 1

. EPA Method 30B

3. 6 PAH s

C alifornia Air Resources Board (CARB) Method 429, “Determination of Polycyclic
Aromatic Hydrocarbon (PAH) Emissions from Stationary Sources, was used to measure PAHs

from the scrubber and baghouse exhausts. The particulate and gaseous phase PAH are extracted
isokinetically from the stack and collected on the XAD

- 2 resin in impingers or in upstream
sampling train components (filter, probe, nozzle). Only the total amounts of each PAH in the
stack emissions can be determined with this method. The analytical method is isotope dilution
mass spectrometry combined with high resolution gas chromatography (HRGC ). Selected
targets from selected samples have been reported from the analysis of di luted extracts that have

been re

- spiked with quantification standard. As a result, these data are not calculated by isotope
dilution and are not inherently recovery

- corrected. Reported extraction standard recoveries for
these targets are not indicative of extraction efficiency as they have been spiked after extraction.
This modification was submitted to USEPA in the test pr otocol and approved via email. Figure

3

- 2 is a schematic of the sampling system.

### 3

- 4 Figure 3

- 2

. CARB Method 429 Sampling Train

### 4

- 1 4. PROCESS OPERATION/SA MPLING LOCATIONS

Eramet Marietta, Inc., operates a facility in Marietta, Ohio. The No. 12 Furnace and No.
1 Furnace were tested at the facility as part of this test program. The No. 12 Furnace, a
submerged arc continuous furnace, is rated at 22 MW and utilizes two wet scrubbers to control
primary and secondary emissions. The scrubbers operate simultaneously and exhaust through a
sing le stack. The No. 1 Furnace, a continuous electric arc continuous furnace, is rated at 31 MW
and a maximum production rate of 35 tons per hour.
The Electrode consumption rate and Safety Data Sheet (SDS) are provided in Appendix
D. The raw material feed to each furnace is also provided in Appendix D.

Table 4

- 1 presents a summary of the sampling site location. Figure 4

- 1 is a general
schematic of the testing locations.

Table 4

- 2 presents Furnace No. 12 process operations, and Table 4

- 3 presents Furnace
No. 1 process operations.

Figure 4

- 1. Sampling Locations

### 4

- 2 Table 4

- 1. Sampling Location Parameters

Stack Identification Stack I.D., Inches (C) Distance from Nearest Disturbance No. of Sampling Points Required, Total Upstream, Inches (A) Downstream,

Inches (B)

Furnace No. 12 Scrubber 95.35” >194.0 368.0 24

Furnace No. 1 Main Baghouse 120” 480.0” 480.0” 24



### Table 4

- 2

. Furnace No. 12 and Process Operations

Date: October 16, 2014 Plant: Eramet

- Marietta, Ohio

Run No. Time Process Throughput , t ons/hr at furnace load (MW) Pressure Drop, inches of water 12

- 1 1010

- 1123 9.5 at 19.55 MW 53.8 east 53.4 west 12

- 2 1157

- 1311 9.5 at 19.02 MW 53.8 east 53.4 west 12

- 3 1332

- 1445 9.5 at 18.82 MW 53.8 east 53.3 west 12

- 4 1509

- 1622 9.5 at 19.17 MW 53.7 east 53.2 west

Average 9.5 at 19.14 MW 53.8 east 53.3 west



### Table 4

- 3

. Furnace No. 1 Process Operations Date: October 15, 2014 Plant: Eramet

– Marietta, Ohio

Run No. Time Process Throughput , t ons/hr at furnace load (MW) Pressure Drop, inches of water Compartments
1 2 3 4 5 6 7 8 Furnace No. 1 Main Baghouse
MB

- 5

- 1 0820

- 0950 10.9 at 24.85 MW 10.58 6.42 6.58 6.27 8.17 6.44 6.43 9.12
MB

- 5

- 2 1020

- 1150 10 .9 at 26.13 MW 10.27 6.85 6.42 6.38 8.17 6.58 6.61 8.99

MB

- 5

- 3 1220

- 1350 10 .9 at 25.88 MW 10.59 6.38 6.75 6.29 8.54 6.54 6.86 9.04

MB

- 5

- 3 1420

- 1550 10.9 at 24.11 MW 10.26 6.78 6.24 6.59 8.06 6.53 6.48 8.46 Average 10.9 at 25.24 MW 10.43 6.61 6.50 6.38 8.26 6.53 6.60 8.90

95.35” I.D.

### 5

- 1 5. QUALITY ASSURANCE AN D QUALITY CONTROL

The field sampling quality assurance for this project included the use of calibrated source
sampling equipment, reference test methods, and traceability protocols for recording and
calculating data . The analytical quality assurance included use of validated analytical
procedures, calibration of analytical instruments, and analysis of control samples and blanks.
The calibration and quality control procedures used for this test program are described in the
following subsection.

5.1 Calibration Procedures and Frequency

All manual stack gas sampling equipment was calibrated before the test program in
accordance with the procedures outlined in the Quality Assurance Handbook for Air Pollution

Measurem ent Systems, Volume 111, EPA

- 600/4

- 72

- 027B. Summarized in Table 5

- 1 are the
stack gas sampling equipment calibrations that were performed in preparation for this project.

The meter box was re

- calibrated after the test.

Table s 5

- 2 and 5

- 3 list the additio nal calibration checks that were performed on the
sampling equipment on site, just prior to the testing, to ensure that equipment was not damaged
during transport. Analyzer checks are conducted directly to the instrument initially and then
through the samp ling system.

5.2 Field Blanks

A field blank of the PAH sampling train was collected. After sample collection and

recovery , the sampling train was assembled, leak checked, recovered

, and submitted to the
laboratory for analysis. The field blank results were subtracted from the sample analyte results
where applicable. Reagent and media blanks were also submitted for analysis.

### 5

- 2 Table 5

- 1. Field Equipment Calibration Summary a Equipment Calibrated Against Allowable E rror Method 5 meter box Reference test meter Y  0.02 Y ∆H @  0.15 post

- test Y  0.05 Orsat Certified cylinder gas  0.5% Pitot tube Geometric specifications See EPA Method 2 Thermocouple ASTM

- 3F thermometer  1.5% Impinger (or condenser thermometer) ASTM

- 3F  2° F

Dry gas thermometer ASTM

- 3F  5° F Probe nozzles Caliper  0.004 in. Barometer NBS traceable barometer  0.1 in. Hg

a As recommended in the Quality Assurance Handbook for Pollution Measurement Systems: Volume III. Stationary Source

Specific Methods. EPA

- 600/4

- 77

- 027b, August 1997.



### Table 5

- 2. Field Checks of Sampling Equipment Equipment Checked Against Allowable Differences Pitot tube Inspection No visible damage Thermocouples ASTM 2F or 3F  1.5% Probe Nozzles Caliper  0.004 in.

### APPENDIX A

CALCULATIONS

### NOMENCLATURE

1

- B ws 

### Dry Mole Fraction
A Cross

- sectional area of stack , ft 2



### acfm Actual Cubic Feet Per Minute

A n 

### Cross

- sectional area of sampling nozzle , ft 2



### A s 

### Cross

- sectional area of stack, in 2



### B ws 

### Moisture, % by volume

B ws(sat) 

### Moisture (at saturation), % by volume
CO 2 

### Carbon Dioxide content, % by volume
C metals 

### Metals concentration, μg/dscm
C p 

### Pitot Tube Coefficient
C pm 

### Particulate matter concentration, grains/dscf
C pmlb 

### Particulate matter concentration, lb/dscf
dscf Dry standard cubic feet
dscfm Dry Standard Cubic Feet Per Minute
dscmm Dry standard cubic meter per minute
DH Avg Meter Orifice Pressure, in. H 2 

### O

D n 

### Nozzle Diameter, inches Dp 1/2 

### Average Square Root Dp, (in. H 2 

### O) 1/2



### E metals 

### Metals mass emission rate, lb/hr

E pm 

### Particulate mass emission rate, lb/hr I Isokinetic Sampling Ratio, % La Maximum acceptable leakage check rate; equal to 0.020 ft 3 

### /min

or 4% of the average sampling rate, whichever is less M catch 

### Metal sample collected, μg
M d 

### Molecular Weight (d.b.), lb/lb•mole

M s 

### Molecular Weight (w.b.), lb /lb•mole

N 2 

### Nitrogen content, % by volume
O 2 

### Oxygen content, % by volume

P bar 

### Barometric Pressure, inches Hg
P s 

### Absolute Stack Pressure, inches Hg

P static 

### Stack Static Pressure, inches H 2 

### O

### PM Particulate matter collected during the test, mg

Q Sample Run Duration, minutes Q a Stack Gas Volumetric flow, acfm Q m Average Sampling Rate, dscfm Q s Stack Gas Volumetric flow, dscfm Q sm Stack Gas Volumetric flow, dscmm T m Average Meter Temperature, °F T s Average Stack Temperature, °F

V lc Volume of Condensate Collected in Impingers and Silica Gel

,

ml V m Sample Volume, ft 3 V m(std) Standard Meter Volume, ft 3 V s Stack Gas Velocity, ft/s V wstd Standard Water Vapor Volume, ft 3
y Meter Box Correction Facto r

### EXAMPLE CALCULATIONS FOR POL LUTANT EMISSIONS

1. Volume of dry gas sampled corrected to standard conditions, ft 3



### . Note: Vm must be corrected for leakage if any leakage rates exceed La.

2. Volume of water vapor at standard conditions, ft 3



### .

Vwstd = 0.04707 x Vlc

3. Moisture content in stack gas, dimensionless.

4. Dry molecular weight of stack gas, lb/lb

- mole.

Md = 0.44 (% CO 2 

### ) + 0.32 (% O 2 

### ) + 0.28 (% N 2 

### + % CO)

5. Molecular weight of stack gas, lb/lb

- mole.

Ms = Md(1

- Bws) + 18Bws

6. Stack velocity at stack conditions, f/s.

7. Stack gas volumetric flow rate at stack conditions, cfm.

Qs = 60 x Vs x As

8. Dry stack gas volumetric flow rate at standard conditions, cfm.

### EXAMPLE CALCULATIONS FOR POLLUTANT EMISSI ONS (CONTINUED)

9. Concentration in gr/dscf.

10. Pollutant mass emission rate, lb/h.

11. Pollutant mass emission rate, lb/MM Btu.

12. F

- factor (Fd).

13. F

- factor, pollutant mass emission rate, lb/MM Btu (O 2 

### - based).

14. Heat input, MM Btu/hr fuel.

15. Heat input, MM Btu/hr, F

- factor.

### EXAMPLE CALCULATIONS FOR GASEOUS POLLUTAN TS MEASURED BY CONTINUO US EMISSION MONITORS (CEMS)

1) Concentrations, parts per million, dry basis:

2) Pollutant Mass Emission Rate, pounds per hour.

PMR , lb/hr =

Molecular Weights of Target Compounds

TGO = Total Gaseous Organics 16.01 (Methane); 44.01 (Propane) SO 2 

### = Sulfur Dioxide 64.05 NO 2 

### = Nitrogen Oxides 46.00 CO = Carbon Monoxide 28.01 HCL = Hydrogen Chloride 36.47 HF = Hydrogen Fluoride 20.01 BWS = Proportion by Volume of Water Vapor in the Gas Stream PMR = Pollutant Mass Emission Rate, pounds per hour DSCFM = Dry standard cubic feet per minute SCF/mol = 385.3

### FURNACE 1 MAIN BAGHOUSE CALCULATIONS

### APPENDIX B

FIELD DATA

### FURNACE 12

### PAH

### MERCURY

### FURNACE 1

### PAH

### MERCURY

### APPENDIX C

ANALYTICAL DATA

### PAHs5420 Mainway Drive, Unit 5, Burlington ON, L7L 6A4 Phone: 905-331-3111, FAX: 905-331-4567

ALS Project Contact: Ron McLeod Client Name: Environmental Quality Management Inc ALS Project ID: EQM100 Client Address: 1800 Carillon Boulevard
ALS WO#: L1535265 Cincinnati, OH 45240 Date of Report: 18-Nov-14 Date of Sample Receipt: 20-Oct-14 Client Contact: Tom Gerstle Client Project ID: 050352.0031 Eramet

COMMENTS: PAH via modified CARB 42 9

The method blank was lost during laboratory processing and has not been reported. The field blank serves as an indication that the sample data are not impacted by significant laboratory background.

Selected targets from selected samples have been reported from the analysis of diluted extracts that have been re-spiked with q uantification standard. As a result, these data are not calculated by isotope dilution and are not inherently recovery-corrected. Reported ex traction standard recoveries for these targets are not indicative of extraction efficiency as they have been spiked after extraction. S.Kennedy 18-Nov-1 4

Certified by: Whitney Davis Account Manager
Results in this certificate relate only to the samples as submitted to the laboratory. This report shall not be reproduced, except in full, without the written permission of ALS Canada Ltd. 

## Certificate of Analysis

ALS Canada Ltd L1535265 141118 Page 1 of 16Sample Name BLANK ACETONE/ HEXANE/METH.
BLANK FIELD BLANK MAIN BAGHOUSE RUN#1 MAIN BAGHOUSE RUN#2

ALS Sample ID L1535265-11 L1535265-4 L1535265-3 L1535265-1 L1535265-2
Sample Size 11111 Sample units sample train train train train

Moisture Content n/a n/a n/a n/a n/a

Matrix XAD Trap Stack Stack Stack Stack Sampling Date 22-Oct-14 14-Oct-14 14-Oct-14 15-Oct-14 15-Oct-14

Extraction Date 28-Oct-14 28-Oct-14 28-Oct-14 28-Oct-14 28-Oct-14

Target Analytes ng ng ng ng ng

Naphthalene 103 2260 9270 471000 458000 2-Me-Naphthalene 12.3 4860 17900 74800 103000 1-Me-Naphthalene 10.2 3910 13600 55200 74800

Acenaphthylene 1.55 157 395 153000 188000

Acenaphthene 1.42 450 1180 32000 43400
Fluorene 6.27 648 1620 70200 121000
Phenanthrene 13.5 3380 12200 2020000 1590000

Anthracene 3.04 140 556 343000 203000
Fluoranthene 1.92 118 554 3620000 4790000 Pyrene 2.97 69.2 522 2600000 3550000 Benz[a]anthracene 4.46 7.33 96.8 268000 570000 Chrysene/Triphenylene 3.33 29.9 225 473000 1250000

Benzo[b]fluoranthene 4.90 614 187 141000 419000 Benzo[k]fluoranthene 2.88 524 51.7 41100 112000 Benzo[e]pyrene 1.74 4.47 109 51900 149000 Benzo[a]pyrene 2.59 <1.8 45.3 22600 60300 Perylene 1.55 <1.3 5.05 4080 8800 Indeno[1,2,3-cd]pyrene 7.92 4.63 30.0 8370 22900 Dibenzo[a,h]anthracene 7.65 1.66 12.4 1190 4120

Benzo[g,h,i]perylene 6.20 3.17 57.1 7330 17700

Field Spike Standards % Rec % Rec % Rec % Rec % Rec

Fluorene-d10 76 n/s 96 111 145 p-Terphenyl-d14 48 n/s 106 73 65

Extraction Standards % Rec % Rec % Rec % Rec % Rec

Naphthalene-d8 72 83 80 100 83 2-Me-Naphthalene-d10 63 84 78 99 67 Acenaphthylene-d8 49 85 81 113 60
Phenanthrene-d10 38 83 85 73 94

Anthracene-d10 40 71 71 78 95
Fluoranthene-d10 45 90 87 81 95 Benz[a]anthracene-d12 20 101 122 66 78 Chrysene-d12 22 75 93 71 79 Benzo[b]fluoranthene-d12 36 103 98 70 94 Benzo[k]fluoranthene-d12 34 77 71 74 99 Benzo[a]pyrene-d12 36 74 66 71 90 Perylene-d12 36 75 69 74 92 Indeno[1,2,3-cd]pyrene-d12 27 88 97 66 92 Dibenzo[a,h]anthracene-d14 25 89 100 64 91

Benzo[g,h,i]perylene-d12 30 86 89 73 101 

### ALS Environmental

Sample Analysis Summary Report

ALS Canada Ltd L1535265 141118 Page 2 of 16Sample Name MAIN BAGHOUSE RUN#3 MAIN BAGHOUSE RUN#4 FURNACE 12 RUN#1 FURNACE 12 RUN#2 FURNACE 12 RUN#3 FURNACE 12 RUN#4

ALS Sample ID L1535265-5 L1535265-6 L1535265-7 L1535265-8 L1535265-9 L1535265-10
Sample Size 111111 Sample units train train train train train train
Moisture Content n/a n/a n/a n/a n/a n/a

Matrix Stack Stack Stack Stack Stack Stack Sampling Date 15-Oct-14 15-Oct-14 16-Oct-14 16-Oct-14 16-Oct-14 16-Oct-14

Extraction Date 28-Oct-14 28-Oct-14 28-Oct-14 28-Oct-14 28-Oct-14 28-Oct-14

Target Analytes ng ng ng ng ng ng

Naphthalene 326000 347000 41700 20200 44100 43900 2-Me-Naphthalene 53700 71100 14100 13900 18300 16400 1-Me-Naphthalene 41000 49900 9600 10400 13200 11700

Acenaphthylene 75000 129000 14800 3670 15000 19100

Acenaphthene 19400 20900 1780 1620 2330 2050
Fluorene 41500 70100 2740 2370 3500 3080
Phenanthrene 1590000 1370000 36400 22200 74000 43500

Anthracene 208000 167000 8620 3610 13200 10500
Fluoranthene 4100000 2070000 36800 11800 64500 30400 Pyrene 2990000 1430000 26800 7950 46900 23100 Benz[a]anthracene 707000 177000 3530 3350 3510 3290 Chrysene/Triphenylene 1480000 461000 13800 9990 10600 5200

Benzo[b]fluoranthene 614000 178000 5170 5290 5060 3160 Benzo[k]fluoranthene 207000 59300 1950 2630 1880 1250 Benzo[e]pyrene 233000 75000 2540 2770 2150 1660 Benzo[a]pyrene 121000 30000 831 457 510 681 Perylene 20600 6220 107 87.8 60.4 133 Indeno[1,2,3-cd]pyrene 40300 11200 1060 1170 651 980 Dibenzo[a,h]anthracene 5890 1980 207 324 129 204

Benzo[g,h,i]perylene 27600 8400 821 751 528 807

Field Spike Standards % Rec % Rec % Rec % Rec % Rec % Rec

Fluorene-d10 104 125 118 109 114 104 p-Terphenyl-d14 87 85 115 85 113 85

Extraction Standards % Rec % Rec % Rec % Rec % Rec % Rec

Naphthalene-d8 97 103 68 90 105 95 2-Me-Naphthalene-d10 116 90 71 91 70 71 Acenaphthylene-d8 104 92 75 88 72 68
Phenanthrene-d10 81 81 108 81 105 77

Anthracene-d10 84 86 103 99 109 81
Fluoranthene-d10 84 87 120 103 102 87 Benz[a]anthracene-d12 71 73 108 64 103 44 Chrysene-d12 73 78 71 48 74 35 Benzo[b]fluoranthene-d12 79 80 96 87 95 67 Benzo[k]fluoranthene-d12 86 81 72 57 94 54 Benzo[a]pyrene-d12 82 78 73 78 72 56 Perylene-d12 81 80 76 81 74 57 Indeno[1,2,3-cd]pyrene-d12 70 76 92 90 97 58 Dibenzo[a,h]anthracene-d14 72 73 95 91 101 56

Benzo[g,h,i]perylene-d12 80 85 92 91 95 55 

### ALS Environmental

Sample Analysis Summary Report

ALS Canada Ltd L1535265 141118 Page 3 of 16Sample Name Laborator y Control Sample

ALS Sample ID WG1980014-2
Sample Size 1 Sample units n/a
Moisture Content n/a

Matrix QC Sampling Date n/a

Extraction Date 28-Oct-14

Target Analytes % Rec

Naphthalene 123 2-Me-Naphthalene 1-Me-Naphthalene

Acenaphthylene 98

Acenaphthene 103
Fluorene 105
Phenanthrene 99

Anthracene 101
Fluoranthene 102 Pyrene 92 Benz[a]anthracene 103 Chrysene/Triphenylene 97

Benzo[b]fluoranthene 109 Benzo[k]fluoranthene 103 Benzo[e]pyrene Benzo[a]pyrene 89 Perylene Indeno[1,2,3-cd]pyrene 111 Dibenzo[a,h]anthracene 104

Benzo[g,h,i]perylene 104

Field Spike Standards % Rec

Fluorene-d10 n/s p-Terphenyl-d14 n/s

Extraction Standards % Rec

Naphthalene-d8 85 2-Me-Naphthalene-d10 81 Acenaphthylene-d8 84
Phenanthrene-d10 80

Anthracene-d10 74
Fluoranthene-d10 91 Benz[a]anthracene-d12 56 Chrysene-d12 50 Benzo[b]fluoranthene-d12 85 Benzo[k]fluoranthene-d12 79 Benzo[a]pyrene-d12 75 Perylene-d12 79 Indeno[1,2,3-cd]pyrene-d12 79 Dibenzo[a,h]anthracene-d14 80

Benzo[g,h,i]perylene-d12 81 

### ALS Environmental

Sample Analysis Summary Report

ALS Canada Ltd L1535265 141118 Page 4 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265-11 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1

Filename 4-141115A1 5 Run Date Final Volume 1000 u L Dilution Factor 1 Anal y sis Units n g Instrument - Column HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Tar g et Anal y tes Time n g n g

Naphthalene 7:33 103 1.3 M 2-Me-Naphthalene 8:44 12.3 0.25 M J 1-Me-Naphthalene 8:54 10.2 0.26 M J

Acenaphthylene 10:10 1.55 0.072 M J

Acenaphthene 10:27 1.42 0.22 J
Fluorene 11:18 6.27 0.48 M J
Phenanthrene 12:51 13.5 0.40 M J

Anthracene 12:56 3.04 0.52 M J
Fluoranthene 14:47 1.92 0.38 M J Pyrene 15:09 2.97 0.36 M J Benz[a]anthracene 17:32 4.46 0.22 M J Chrysene/Triphenylene 17:37 3.33 0.22 M J

Benzo[b]fluoranthene 19:44 4.90 0.64 M J Benzo[k]fluoranthene 19:47 2.88 0.69 M J Benzo[e]pyrene 20:14 1.74 0.75 M J Benzo[a]pyrene 20:21 2.59 0.78 M J Perylene 20:30 1.55 0.60 M J Indeno[1,2,3-cd]pyrene 22:22 7.92 1.4 M J Dibenzo[a,h]anthracene 22:26 7.65 1.3 M J

Benzo[g,h,i]perylene 22:46 6.20 0.74 M J

Field Spike Standards % Rec Limits

Fluorene-d10 11:15 76 50-150 p-Terphenyl-d14 15:34 48 50-150

Extraction Standards % Rec Limits

Naphthalene-d8 7:31 72 20-150 2-Me-Naphthalene-d10 8:40 63 20-150 Acenaphthylene-d8 10:08 49 20-150
Phenanthrene-d10 12:48 38 30-150

Anthracene-d10 12:53 40 30-150
Fluoranthene-d10 14:45 45 30-150 Benz[a]anthracene-d12 17:29 20 30-150 Chrysene-d12 17:33 22 30-150 Benzo[b]fluoranthene-d12 19:41 36 30-150 Benzo[k]fluoranthene-d12 19:44 34 30-150 Benzo[a]pyrene-d12 20:17 36 30-150 Perylene-d12 20:27 36 30-150 Indeno[1,2,3-cd]pyrene-d12 22:20 27 30-150 Dibenzo[a,h]anthracene-d14 22:23 25 30-150

Benzo[g,h,i]perylene-d12 22:44 30 30-150

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated.

J indicates that a tar g et anal y te was detected below the LQL. XAD Trap 10 BLAN K

CARB 429 Modified sam p le n/a 1 Sample Analysis Report

15-Nov-14 20:44 

# ALS Environmental

22-Oct-14 28-Oct-14 Approved: Ella Gd y cz y nski --e-si g nature--

17-Nov-2014

Flags

ALS Canada Ltd L1535265 141118 Page 5 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 4 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1

Filename 4-141115A1 6 Run Date Final Volume 1000 u L Dilution Factor 1 Anal y sis Units n g Instrument - Column HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Tar g et Anal y tes Time n g n g

Naphthalene 7:33 2260 16 M 2-Me-Naphthalene 8:42 4860 7.2 1-Me-Naphthalene 8:52 3910 7.6

Acenaphthylene 10:09 157 1.4 M

Acenaphthene 10:26 450 3.4 M
Fluorene 11:17 648 1.6 M
Phenanthrene 12:50 3380 2.2 M

Anthracene 12:55 140 2.6 M
Fluoranthene 14:46 118 0.92 M Pyrene 15:09 69.2 0.86 M J Benz[a]anthracene 17:32 7.33 0.40 M J Chrysene/Triphenylene 17:35 29.9 0.43 M J

Benzo[b]fluoranthene 19:45 614 1.3 M Benzo[k]fluoranthene 19:47 524 1.6 M Benzo[e]pyrene 20:15 4.47 1.7 M J Benzo[a]pyrene NotFnd <1.8 1.8 M U Perylene NotFnd <1.3 1.3 M U Indeno[1,2,3-cd]pyrene 22:22 4.63 0.90 M J Dibenzo[a,h]anthracene 22:26 1.66 0.45 M J

Benzo[g,h,i]perylene 22:46 3.17 0.55 M J

Field Spike Standards % Rec Limits

Fluorene-d10 11:14 n/s p-Terphenyl-d14 15:34 n/s

Extraction Standards % Rec Limits

Naphthalene-d8 7:31 83 20-150 2-Me-Naphthalene-d10 8:39 84 20-150 Acenaphthylene-d8 10:08 85 20-150
Phenanthrene-d10 12:47 83 30-150

Anthracene-d10 12:52 71 30-150
Fluoranthene-d10 14:44 90 30-150 Benz[a]anthracene-d12 17:29 101 30-150 Chrysene-d12 17:32 75 30-150 Benzo[b]fluoranthene-d12 19:40 103 30-150 Benzo[k]fluoranthene-d12 19:44 77 30-150 Benzo[a]pyrene-d12 20:17 74 30-150 Perylene-d12 20:27 75 30-150 Indeno[1,2,3-cd]pyrene-d12 22:19 88 30-150 Dibenzo[a,h]anthracene-d14 22:22 89 30-150

Benzo[g,h,i]perylene-d12 22:44 86 30-150

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated. U Indicates that this com p ound was not detected above the MDL. n/s Indicates that this standard has not been s p iked. J indicates that a tar g et anal y te was detected below the LQL. Flags 10 ACETONE/HEXANE/METH. BLANK

15-Nov-14 21:18 Ella Gd y cz y nski --e-si g nature-- 1 

# ALS Environmental

14-Oct-14 28-Oct-14 Approved: Sample Analysis Report

17-Nov-2014 Stack CARB 429 Modified train n/a

ALS Canada Ltd L1535265 141118 Page 6 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 3 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1

Filename 4-141115A1 7 Run Date Final Volume 1000 u L Dilution Factor 1 Anal y sis Units n g Instrument - Column HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Tar g et Anal y tes Time n g n g

Naphthalene 7:35 9270 39 M 2-Me-Naphthalene 8:43 17900 2.5 1-Me-Naphthalene 8:53 13600 2.6

Acenaphthylene 10:10 395 1.4 M

Acenaphthene 10:27 1180 6.5 M
Fluorene 11:17 1620 2.9 M
Phenanthrene 12:50 12200 8.3 M

Anthracene 12:55 556 10 M
Fluoranthene 14:47 554 1.8 M Pyrene 15:09 522 1.7 M Benz[a]anthracene 17:32 96.8 1.2 M J Chrysene/Triphenylene 17:36 225 1.3 M

Benzo[b]fluoranthene 19:43 187 0.61 M Benzo[k]fluoranthene 19:46 51.7 0.70 M J Benzo[e]pyrene 20:14 109 0.85 M Benzo[a]pyrene 20:20 45.3 0.89 M J Perylene 20:30 5.05 0.61 M J Indeno[1,2,3-cd]pyrene 22:22 30.0 2.1 M J Dibenzo[a,h]anthracene 22:26 12.4 0.98 M J

Benzo[g,h,i]perylene 22:47 57.1 1.4 M J

Field Spike Standards % Rec Limits

Fluorene-d10 11:14 96 50-150 p-Terphenyl-d14 15:34 106 50-150

Extraction Standards % Rec Limits

Naphthalene-d8 7:33 80 20-150 2-Me-Naphthalene-d10 8:40 78 20-150 Acenaphthylene-d8 10:08 81 20-150
Phenanthrene-d10 12:48 85 30-150

Anthracene-d10 12:53 71 30-150
Fluoranthene-d10 14:45 87 30-150 Benz[a]anthracene-d12 17:29 122 30-150 Chrysene-d12 17:32 93 30-150 Benzo[b]fluoranthene-d12 19:40 98 30-150 Benzo[k]fluoranthene-d12 19:44 71 30-150 Benzo[a]pyrene-d12 20:17 66 30-150 Perylene-d12 20:27 69 30-150 Indeno[1,2,3-cd]pyrene-d12 22:19 97 30-150 Dibenzo[a,h]anthracene-d14 22:22 100 30-150

Benzo[g,h,i]perylene-d12 22:43 89 30-150

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated.

J indicates that a tar g et anal y te was detected below the LQL. Stack 10 FIELD BLAN K

CARB 429 Modified train n/a 1 Sample Analysis Report

15-Nov-14 21:52 

# ALS Environmental

14-Oct-14 28-Oct-14 Approved: Ella Gd y cz y nski --e-si g nature--

17-Nov-2014

Flags

ALS Canada Ltd L1535265 141118 Page 7 of 16Sample Name Samplin g Date ALS Sample ID L1535265-1 Extraction Date Analysis Method Sample Size Ana l ysis Type Samp l e Moisture Conten t Sample Matrix Split Ratio

Run Information Run 1 Run 2 Run 3

Filename 4-141115B17 4-141115B04 4-141115A19 Run Date Final Volume 1000 u L 1000 u L 1000 u L Dilution Facto r 1 10 100 Analysis Units n g n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Ret. Conc. EDL Tar g et Analytes Time n g n g Time. n g n g Time. n g n g

Naphthalene 7:33 471000 390 7:34 604000 1400 7:34 686000 5800 M 2-Me-Naphthalene 8:43 74800 58 M 8:43 117000 170 8:43 141000 4100 J 1-Me-Naphthalene 8:52 55200 60 M 8:52 94800 180 8:52 126000 4300 J

Acenaphthylene 10:10 153000 19 M 10:10 255000 360 M 10:09 238000 1800 M J

Acenaphthene 10:27 32000 130 M 10:27 53700 530 M 10:27 44400 2500 M J
Fluorene 11:18 70200 110 M 11:19 102000 450 M 11:18 104000 2400 M J
Phenanthrene 12:50 1130000 93 M E 12:50 2020000 130 M 12:50 1970000 2600 M

Anthracene 12:55 129000 96 M 12:55 343000 150 M 12:55 385000 3300 M J
Fluoranthene 14:47 2000000 260 M E 14:47 3620000 1600 M 14:46 3810000 3600 M Pyrene 15:10 1670000 250 M E 15:09 2600000 1500 M 15:09 2780000 3300 M Benz[a]anthracene 17:33 153000 99 M 17:32 268000 1200 M 17:32 220000 3700 M J Chrysene/Triphenylene 17:36 314000 100 M 17:36 473000 1100 M 17:36 470000 3200 M J

Benzo[b]fluoranthene 19:44 79700 90 M 19:44 141000 340 M 19:44 116000 1100 M J Benzo[k]fluoranthene 19:47 36200 92 M 19:46 41100 380 M J 19:46 51100 1100 M J Benzo[e]pyrene 20:15 10800 26 M 20:14 51900 390 M 20:14 53600 1200 M J Benzo[a]pyrene 20:21 5150 28 M 20:21 22600 410 M J 20:21 23300 1200 M J Perylene 20:31 2500 48 M J 20:30 4080 300 M J 20:31 6630 710 M J Indeno[1,2,3-cd]pyrene NotFnd <34000 34000 M U 22:22 8370 380 M J 22:22 8760 3000 M J Dibenzo[a,h]anthracene 22:27 885 220 M J 22:26 1190 250 M J 22:28 3790 2300 M J

Benzo[g,h,i]perylene 22:48 4620 120 M J 22:46 7330 190 M J 22:47 7050 1500 M J

Field Spike Standards % Rec Limits % Rec % Rec

Fluorene-d10 11:15 111 50-150 11:15 141 11:15 222 p-Terphenyl-d14 15:34 73 50-150 15:34 158 15:34 59

Extraction Standards % Rec Limits % Rec % Rec

Naphthalene-d8 7:32 100 20-150 7:32 77 7:32 80 2-Me-Naphthalene-d10 8:40 99 20-150 8:40 70 8:40 68 Acenaphthylene-d8 10:08 113 20-150 10:08 75 10:08 80
Phenanthrene-d10 12:48 119 30-150 12:48 73 12:48 64

Anthracene-d10 12:53 128 30-150 12:53 78 12:53 63
Fluoranthene-d10 14:45 131 30-150 14:45 81 14:45 67 Benz[a]anthracene-d12 17:30 66 30-150 17:29 66 17:29 52 Chrysene-d12 17:33 57 30-150 17:32 71 17:33 73 Benzo[b]fluoranthene-d12 19:41 121 30-150 19:41 70 19:40 67 Benzo[k]fluoranthene-d12 19:44 100 30-150 19:44 74 19:44 67 Benzo[a]pyrene-d12 20:18 316 30-150 20:17 71 20:18 73 Perylene-d12 20:28 147 30-150 20:27 74 20:27 70 Indeno[1,2,3-cd]pyrene-d12 22:15 76 30-150 22:20 66 22:20 65 Dibenzo[a,h]anthracene-d14 22:25 37 M 30-150 22:23 64 22:24 61

Benzo[g,h,i]perylene-d12 22:45 105 30-150 22:44 73 22:44 83

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sample. M Indicates that a peak has been manually inte g rated. U Indicates that this compound was not detected above the MDL. E Indicates that this compound was detected above the calibrated ran g e. J indicates that a tar g et analyte was detected below the LQL

. Flags Flags 16-Nov-14 03:35 15-Nov-14 23:01 500 MAIN BAGHOUSE RUN#1

16-Nov-14 11:01 Ella Gdyczynski --e-si g nature-- 1 

## ALS Environmental

15-Oct-14 28-Oct-14 Approved:

Flags Sam p le Anal y sis Re p or t

17-Nov-2014 Stack CARB 429 Modified train n/a

ALS Canada Ltd L1535265 141118 Page 8 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 2 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1 Run 2 Run 3

Filename 4-141115B1 8 4-141115B0 5 4-141115A2 0 Run Date Final Volume 1000 u L 1000 u L 1000 u L Dilution Factor 1 10 100 Anal y sis Units n g n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Ret. Conc. EDL Tar g et Anal y tes Time n g n g Time. n g n g Time. n g n g

Naphthalene 7:34 458000 240 M 7:34 437000 700 7:35 570000 4400 M 2-Me-Naphthalene 8:43 103000 36 8:43 79900 180 8:44 107000 2800 J 1-Me-Naphthalene 8:52 74800 38 8:53 65500 190 8:53 83800 2900 J

Acenaphthylene 10:10 188000 110 M 10:10 156000 500 M 10:09 147000 830 M J

Acenaphthene 10:27 43400 52 M 10:27 32900 120 J 10:28 32700 1100 M J
Fluorene 11:19 121000 140 M 11:19 57300 120 M 11:18 71300 1900 M J
Phenanthrene 12:50 2480000 220 M E 12:50 1590000 790 M 12:51 1600000 2300 M

Anthracene 12:55 205000 250 M 12:55 203000 970 M 12:55 261000 3300 M J
Fluoranthene 14:47 5300000 450 M E 14:47 4790000 1900 M 14:47 4050000 570 M Pyrene 15:10 4720000 420 M E 15:10 3550000 1700 M 15:09 3210000 530 M Benz[a]anthracene 17:32 1120000 670 M E 17:32 570000 370 M 17:32 466000 2500 M J Chrysene/Triphenylene 17:36 2400000 600 M E 17:36 1250000 350 M 17:32 536000 2800 M

Benzo[b]fluoranthene 19:44 776000 180 M E 19:44 419000 440 M 19:44 400000 3700 M J Benzo[k]fluoranthene 19:47 152000 120 M 19:47 112000 480 M 19:47 126000 4300 M J Benzo[e]pyrene 20:15 88000 41 M 20:14 149000 540 M 20:15 142000 4000 M J Benzo[a]pyrene 20:21 38700 43 M 20:20 60300 560 M 20:21 71400 4200 M J Perylene 20:31 16200 95 M 20:30 8800 440 M J 20:30 5550 3100 M J Indeno[1,2,3-cd]pyrene 22:23 46800 150 M 22:22 22900 620 M J 22:22 26600 3600 M J Dibenzo[a,h]anthracene 22:27 8480 210 M 22:27 4120 200 M J 22:27 5290 2200 M J

Benzo[g,h,i]perylene 22:48 29100 140 M 22:46 17700 320 M J 22:46 18000 1600 M J

Field Spike Standards % Rec Limits % Rec % Rec

Fluorene-d10 11:15 175 50-150 11:15 145 11:16 60 p-Terphenyl-d14 15:35 173 50-150 15:35 65 15:36 186

Extraction Standards % Rec Limits % Rec % Rec

Naphthalene-d8 7:32 83 20-150 7:32 94 7:32 97 2-Me-Naphthalene-d10 8:40 67 20-150 8:40 98 8:40 87 Acenaphthylene-d8 10:08 60 20-150 10:08 88 10:08 93
Phenanthrene-d10 12:48 54 30-150 12:48 94 12:48 78

Anthracene-d10 12:53 52 30-150 12:53 95 12:53 84
Fluoranthene-d10 14:45 52 30-150 14:45 95 14:45 102 Benz[a]anthracene-d12 17:29 27 30-150 17:29 78 17:30 80 Chrysene-d12 17:33 28 30-150 17:32 79 17:30 48 Benzo[b]fluoranthene-d12 19:41 47 M 30-150 19:40 94 19:41 79 Benzo[k]fluoranthene-d12 19:44 68 M 30-150 19:44 99 19:44 85 Benzo[a]pyrene-d12 20:18 136 M 30-150 20:17 90 20:18 86 Perylene-d12 20:28 50 M 30-150 20:27 92 20:27 88 Indeno[1,2,3-cd]pyrene-d12 22:21 33 M 30-150 22:19 92 22:20 87 Dibenzo[a,h]anthracene-d14 22:25 33 M 30-150 22:23 91 22:23 81

Benzo[g,h,i]perylene-d12 22:45 39 M 30-150 22:44 101 22:44 111

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated.

E Indicates that this com p ound was detected above the calibrated ran g e. J indicates that a tar g et anal y te was detected below the LQL. Stack 500 MAIN BAGHOUSE RUN#2

CARB 429 Modified train n/a 1 Sample Analysis Report

16-Nov-14 11:36 

# ALS Environmental

15-Oct-14 28-Oct-14 Approved: Ella Gd y cz y nski --e-si g nature--

17-Nov-2014

Flags Flags Flags 16-Nov-14 04:10 15-Nov-14 23:35

ALS Canada Ltd L1535265 141118 Page 9 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 5 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1 Run 2 Run 3

Filename 4-141115B1 9 4-141115B0 6 4-141115A21 Run Date Final Volume 1000 u L 1000 u L 1000 u L Dilution Factor 1 10 100 Anal y sis Units n g n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Ret. Conc. EDL Tar g et Anal y tes Time n g n g Time. n g n g Time. n g n g

Naphthalene 7:34 326000 97 7:33 445000 860 7:34 530000 11000 2-Me-Naphthalene 8:44 53700 19 8:43 88100 440 8:44 106000 2900 J 1-Me-Naphthalene 8:53 41000 20 8:52 65400 460 8:53 93800 3100 J

Acenaphthylene 10:11 75000 59 10:09 125000 270 M 10:10 120000 1900 M J

Acenaphthene 10:27 19400 19 M 10:26 26600 340 M J 10:27 25900 2000 M J
Fluorene 11:18 41500 65 M 11:18 58100 310 M 11:19 60300 2200 M J
Phenanthrene 12:50 1090000 97 M E 12:49 1590000 130 M 12:51 1570000 7600 M

Anthracene 12:55 95500 110 M 12:54 208000 160 M 12:55 358000 12000 M J
Fluoranthene 14:47 2300000 140 M E 14:46 4100000 620 M 14:47 3340000 7500 M Pyrene 15:10 1940000 130 M E 15:09 2990000 580 M 15:10 2600000 7000 M Benz[a]anthracene 17:32 584000 51 M 17:31 707000 200 M 17:33 640000 2000 M Chrysene/Triphenylene 17:37 1290000 47 M E 17:35 1480000 190 M 17:36 1640000 1800 M

Benzo[b]fluoranthene 19:44 481000 89 M E 19:44 614000 320 M 19:44 634000 4400 M Benzo[k]fluoranthene 19:47 164000 86 M 19:45 207000 320 M 19:47 206000 5000 M J Benzo[e]pyrene 20:15 72900 35 M 20:14 233000 380 M 20:15 245000 5600 M J Benzo[a]pyrene 20:21 38500 36 M 20:20 121000 390 M 20:21 126000 5800 M J Perylene 20:31 16800 82 20:30 20600 290 M J 20:31 23900 3900 M J Indeno[1,2,3-cd]pyrene 22:23 27200 310 M 22:21 40300 490 M J 22:23 30300 4500 M J Dibenzo[a,h]anthracene 22:27 5510 200 M 22:26 5890 260 M J 22:28 7220 3400 M J

Benzo[g,h,i]perylene 22:48 16000 200 M 22:46 27600 250 M J 22:47 25500 2000 M J

Field Spike Standards % Rec Limits % Rec % Rec

Fluorene-d10 11:15 104 50-150 11:14 131 11:15 142 p-Terphenyl-d14 15:35 87 50-150 15:34 176 15:37 67

Extraction Standards % Rec Limits % Rec % Rec

Naphthalene-d8 7:32 97 20-150 7:31 85 7:32 94 2-Me-Naphthalene-d10 8:40 116 20-150 8:40 86 8:40 78 Acenaphthylene-d8 10:09 104 20-150 10:08 81 10:09 84
Phenanthrene-d10 12:48 119 30-150 12:47 81 12:48 75

Anthracene-d10 12:53 105 30-150 12:53 84 12:54 69
Fluoranthene-d10 14:45 109 30-150 14:44 84 14:45 93 Benz[a]anthracene-d12 17:29 80 30-150 17:28 71 17:30 69 Chrysene-d12 17:33 71 30-150 17:32 73 17:33 81 Benzo[b]fluoranthene-d12 19:41 105 M 30-150 19:40 79 19:41 73 Benzo[k]fluoranthene-d12 19:44 99 M 30-150 19:44 86 19:45 80 Benzo[a]pyrene-d12 20:17 233 M 30-150 20:17 82 20:18 80 Perylene-d12 20:23 90 M 30-150 20:27 81 20:28 83 Indeno[1,2,3-cd]pyrene-d12 22:21 87 30-150 22:19 70 22:20 76 Dibenzo[a,h]anthracene-d14 22:25 70 30-150 22:22 72 22:24 70

Benzo[g,h,i]perylene-d12 22:45 121 30-150 22:43 80 22:44 85

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated.

E Indicates that this com p ound was detected above the calibrated ran g e. J indicates that a tar g et anal y te was detected below the LQL. Flags Flags 16-Nov-14 04:44 16-Nov-14 00:09 500 MAIN BAGHOUSE RUN#3

16-Nov-14 12:10 Ella Gd y cz y nski --e-si g nature-- 1 

# ALS Environmental

15-Oct-14 28-Oct-14 Approved:

Flags Sample Analysis Report

17-Nov-2014 Stack CARB 429 Modified train n/a

ALS Canada Ltd L1535265 141118 Page 10 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 6 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1 Run 2

Filename 4-141115B2 0 4-141115B0 7 Run Date Final Volume 1000 u L 1000 u L Dilution Factor 1 10 Anal y sis Units n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Tar g et Anal y tes Time n g n g Time. n g n g

Naphthalene 7:33 347000 200 7:34 487000 820 2-Me-Naphthalene 8:43 71100 31 8:44 88700 190 1-Me-Naphthalene 8:52 49900 33 8:52 67900 190

Acenaphthylene 10:09 129000 28 M 10:09 188000 360 M

Acenaphthene 10:27 20900 120 M 10:27 29500 170 M J
Fluorene 11:18 70100 39 M 11:19 83400 230 M
Phenanthrene 12:50 1320000 100 M E 12:51 1370000 260 M

Anthracene 12:54 104000 120 M 12:55 167000 330 M
Fluoranthene 14:47 1820000 74 M E 14:47 2070000 810 M Pyrene 15:09 1460000 69 M E 15:09 1430000 750 M Benz[a]anthracene 17:32 176000 92 M 17:32 177000 230 M Chrysene/Triphenylene 17:36 394000 79 M 17:36 461000 220 M

Benzo[b]fluoranthene 19:44 158000 440 M 19:44 178000 240 M Benzo[k]fluoranthene 19:46 59100 510 M 19:46 59300 250 M Benzo[e]pyrene 20:14 35200 240 M 20:15 75000 270 M Benzo[a]pyrene 20:21 14500 240 M 20:21 30000 280 M J Perylene 20:30 3510 340 M J 20:30 6220 220 M J Indeno[1,2,3-cd]pyrene 22:23 12800 120 M 22:22 11200 280 M J Dibenzo[a,h]anthracene 22:28 1900 97 M J 22:26 1980 240 J

Benzo[g,h,i]perylene 22:48 9830 68 M 22:47 8400 140 M J

Field Spike Standards % Rec Limits % Rec

Fluorene-d10 11:15 125 50-150 11:16 159 p-Terphenyl-d14 15:34 85 50-150 15:34 34

Extraction Standards % Rec Limits % Rec

Naphthalene-d8 7:31 103 20-150 7:32 86 2-Me-Naphthalene-d10 8:40 90 20-150 8:40 84 Acenaphthylene-d8 10:08 92 20-150 10:08 81
Phenanthrene-d10 12:48 92 30-150 12:48 81

Anthracene-d10 12:53 92 30-150 12:53 86
Fluoranthene-d10 14:44 95 30-150 14:45 87 Benz[a]anthracene-d12 17:29 52 30-150 17:29 73 Chrysene-d12 17:32 53 30-150 17:33 78 Benzo[b]fluoranthene-d12 19:41 81 M 30-150 19:41 80 Benzo[k]fluoranthene-d12 19:44 74 M 30-150 19:44 81 Benzo[a]pyrene-d12 20:20 142 M 30-150 20:17 78 Perylene-d12 20:27 104 M 30-150 20:27 80 Indeno[1,2,3-cd]pyrene-d12 22:21 52 30-150 22:19 76 Dibenzo[a,h]anthracene-d14 22:24 51 30-150 22:23 73

Benzo[g,h,i]perylene-d12 22:45 57 30-150 22:44 85

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated.

E Indicates that this com p ound was detected above the calibrated ran g e. J indicates that a tar g et anal y te was detected below the LQL. Stack 500 MAIN BAGHOUSE RUN# 4

CARB 429 Modified train n/a 1 Sample Analysis Report

16-Nov-14 12:44 

# ALS Environmental

15-Oct-14 28-Oct-14 Approved: Ella Gd y cz y nski --e-si g nature--

17-Nov-2014

Flags Flags 16-Nov-14 05:18

ALS Canada Ltd L1535265 141118 Page 11 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 7 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1 Run 2

Filename 4-141115B1 2 4-141115B0 8 Run Date Final Volume 1000 u L 1000 u L Dilution Factor 1 50 Anal y sis Units n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Tar g et Anal y tes Time n g n g Time. n g n g

Naphthalene 7:34 41700 41 M 7:33 37700 61 M 2-Me-Naphthalene 8:43 14100 17 8:43 14500 11 1-Me-Naphthalene 8:53 9600 18 8:52 12700 11

Acenaphthylene 10:10 14800 2.9 M 10:10 12100 26 M

Acenaphthene 10:27 1780 1.5 M 10:27 1950 34 M J
Fluorene 11:18 2740 15 M 11:19 2540 49 M J
Phenanthrene 12:50 30000 6.6 M E 12:51 36400 15 M

Anthracene 12:55 4750 7.3 M 12:56 8620 21 M
Fluoranthene 14:47 38100 7.9 M E 14:47 36800 26 M Pyrene 15:10 31400 7.4 M E 15:09 26800 24 M Benz[a]anthracene 17:32 3530 3.7 M 17:33 2190 53 M J Chrysene/Triphenylene 17:36 13800 4.0 M 17:33 2520 61 M J

Benzo[b]fluoranthene 19:44 5170 1.4 M 19:45 4060 18 M J Benzo[k]fluoranthene 19:47 1950 1.5 M 19:47 2940 24 M J Benzo[e]pyrene 20:15 2540 1.8 M 20:15 842 5.5 M J Benzo[a]pyrene 20:21 831 1.8 M 20:22 108 5.7 M J Perylene 20:31 107 1.4 M 20:30 85.2 12 M J Indeno[1,2,3-cd]pyrene 22:22 1060 0.62 M 22:25 1040 26 M J Dibenzo[a,h]anthracene 22:26 207 0.83 M 22:27 216 28 M J

Benzo[g,h,i]perylene 22:47 821 0.36 M 22:48 579 14 M J

Field Spike Standards % Rec Limits % Rec

Fluorene-d10 11:15 118 50-150 11:15 94 p-Terphenyl-d14 15:34 115 50-150 15:35 78

Extraction Standards % Rec Limits % Rec

Naphthalene-d8 7:32 68 20-150 7:31 119 2-Me-Naphthalene-d10 8:41 71 20-150 8:40 100 Acenaphthylene-d8 10:09 75 20-150 10:08 108
Phenanthrene-d10 12:48 79 30-150 12:48 108

Anthracene-d10 12:53 69 30-150 12:53 103
Fluoranthene-d10 14:45 82 30-150 14:45 120 Benz[a]anthracene-d12 17:29 108 30-150 17:30 67 Chrysene-d12 17:33 71 30-150 17:30 41 Benzo[b]fluoranthene-d12 19:41 96 30-150 19:42 103 M Benzo[k]fluoranthene-d12 19:44 72 30-150 19:46 74 M Benzo[a]pyrene-d12 20:17 73 30-150 20:17 354 M Perylene-d12 20:27 76 30-150 20:28 101 M Indeno[1,2,3-cd]pyrene-d12 22:20 92 30-150 22:21 67 M Dibenzo[a,h]anthracene-d14 22:23 95 30-150 22:24 26

Benzo[g,h,i]perylene-d12 22:44 92 30-150 22:45 113

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated.

E Indicates that this com p ound was detected above the calibrated ran g e. J indicates that a tar g et anal y te was detected below the LQL. Flags 16-Nov-14 05:52 10 FURNACE 12 RUN#1

16-Nov-14 08:10 Ella Gd y cz y nski --e-si g nature-- 1 

# ALS Environmental

16-Oct-14 28-Oct-14 Approved:

Flags Sample Analysis Report

17-Nov-2014 Stack CARB 429 Modified train n/a

ALS Canada Ltd L1535265 141118 Page 12 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 8 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1 Run 2

Filename 4-141115B1 3 4-141115B0 9 Run Date Final Volume 1000 u L 1000 u L Dilution Factor 1 50 Anal y sis Units n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Tar g et Anal y tes Time n g n g Time. n g n g

Naphthalene 7:34 26400 63 E 7:33 20200 200 2-Me-Naphthalene 8:44 13900 3.4 8:43 13200 18 1-Me-Naphthalene 8:53 10400 3.5 8:52 12600 19

Acenaphthylene 10:10 3670 3.2 M 10:09 3480 18 M J

Acenaphthene 10:28 1620 1.9 10:26 1630 16 M J
Fluorene 11:18 2370 5.3 M 11:17 2860 34 M J
Phenanthrene 12:51 22700 7.8 M E 12:51 22200 63 M

Anthracene 12:55 1820 9.8 M 12:54 3610 76 M J
Fluoranthene 14:47 11800 4.1 M 14:47 10700 4.5 Pyrene 15:10 7950 3.8 M 15:10 8380 4.2 M Benz[a]anthracene 17:32 3350 4.7 M 17:34 3330 11 M J Chrysene/Triphenylene 17:37 9990 5.0 M 17:37 9600 8.7 M

Benzo[b]fluoranthene 19:44 5460 3.2 M E 19:44 5290 34 M Benzo[k]fluoranthene 19:47 1600 3.6 M 19:48 2630 39 M J Benzo[e]pyrene 20:15 2770 4.9 M 20:14 1560 8.0 M J Benzo[a]pyrene 20:21 457 5.1 M 20:21 132 8.3 M J Perylene 20:31 87.8 3.6 M J 20:30 163 17 M J Indeno[1,2,3-cd]pyrene 22:23 1170 3.8 M 22:24 816 52 M J Dibenzo[a,h]anthracene 22:26 324 1.3 M 22:26 95.0 54 J

Benzo[g,h,i]perylene 22:48 751 2.2 M 22:48 856 37 M J

Field Spike Standards % Rec Limits % Rec

Fluorene-d10 11:15 109 50-150 11:14 117 p-Terphenyl-d14 15:34 85 50-150 15:34 93

Extraction Standards % Rec Limits % Rec

Naphthalene-d8 7:32 84 20-150 7:31 90 2-Me-Naphthalene-d10 8:41 91 20-150 8:40 83 Acenaphthylene-d8 10:09 88 20-150 10:08 91
Phenanthrene-d10 12:48 91 30-150 12:48 81

Anthracene-d10 12:53 76 30-150 12:53 99
Fluoranthene-d10 14:45 103 30-150 14:45 100 Benz[a]anthracene-d12 17:29 64 30-150 17:30 40 Chrysene-d12 17:33 48 30-150 17:33 56 Benzo[b]fluoranthene-d12 19:41 104 30-150 19:42 87 Benzo[k]fluoranthene-d12 19:44 93 30-150 19:42 57 Benzo[a]pyrene-d12 20:18 78 30-150 20:18 158 M Perylene-d12 20:27 81 30-150 20:27 46 M Indeno[1,2,3-cd]pyrene-d12 22:20 90 30-150 22:21 53 M Dibenzo[a,h]anthracene-d14 22:23 91 30-150 22:27 49 M

Benzo[g,h,i]perylene-d12 22:44 91 30-150 22:45 60 M

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated.

E Indicates that this com p ound was detected above the calibrated ran g e. J indicates that a tar g et anal y te was detected below the LQL. Stack 10 FURNACE 12 RUN#2

CARB 429 Modified train n/a 1 Sample Analysis Report

16-Nov-14 08:44 

# ALS Environmental

16-Oct-14 28-Oct-14 Approved: Ella Gd y cz y nski --e-si g nature--

17-Nov-2014

Flags Flags 16-Nov-14 06:27

ALS Canada Ltd L1535265 141118 Page 13 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265- 9 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1 Run 2

Filename 4-141115B1 5 4-141115B1 4 Run Date Final Volume 1000 u L 1000 u L Dilution Factor 1 50 Anal y sis Units n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Tar g et Anal y tes Time n g n g Time. n g n g

Naphthalene 7:35 42000 51 E 7:33 44100 190 M 2-Me-Naphthalene 8:43 18300 2.9 8:43 16000 19 1-Me-Naphthalene 8:53 13200 3.0 8:52 13700 19

Acenaphthylene 10:10 15000 3.8 M 10:09 12700 10 M

Acenaphthene 10:27 2330 1.4 M 10:27 2570 31 M J
Fluorene 11:18 3500 8.0 M 11:18 4220 32 M J
Phenanthrene 12:50 36200 4.3 M E 12:50 74000 25 M

Anthracene 12:55 5970 4.6 M 12:56 13200 31 M
Fluoranthene 14:47 43800 12 M E 14:47 64500 58 M Pyrene 15:10 37700 11 M E 15:09 46900 54 M Benz[a]anthracene 17:33 3510 1.3 M 17:33 2180 20 M J Chrysene/Triphenylene 17:36 10600 1.5 M 17:36 9520 18 M

Benzo[b]fluoranthene 19:44 5080 1.2 M E 19:45 5060 60 M Benzo[k]fluoranthene 19:47 1310 1.3 M 19:47 1880 50 M J Benzo[e]pyrene 20:15 2150 1.5 M 20:14 959 59 M J Benzo[a]pyrene 20:21 510 1.5 M 20:22 189 62 M J Perylene 20:31 60.4 1.1 M J 20:31 <220 220 M U Indeno[1,2,3-cd]pyrene 22:22 651 0.74 M 22:23 597 44 M J Dibenzo[a,h]anthracene 22:26 129 1.2 M 22:28 198 57 M J

Benzo[g,h,i]perylene 22:47 528 0.45 M 22:48 505 22 M J

Field Spike Standards % Rec Limits % Rec

Fluorene-d10 11:15 114 50-150 11:15 135 p-Terphenyl-d14 15:34 113 50-150 15:34 103

Extraction Standards % Rec Limits % Rec

Naphthalene-d8 7:32 65 20-150 7:31 105 2-Me-Naphthalene-d10 8:40 70 20-150 8:40 110 Acenaphthylene-d8 10:09 72 20-150 10:08 104
Phenanthrene-d10 12:48 77 30-150 12:48 105

Anthracene-d10 12:54 69 30-150 12:53 109
Fluoranthene-d10 14:45 80 30-150 14:45 102 Benz[a]anthracene-d12 17:29 103 30-150 17:29 72 Chrysene-d12 17:33 74 30-150 17:33 81 Benzo[b]fluoranthene-d12 19:41 85 30-150 19:41 95 M Benzo[k]fluoranthene-d12 19:45 69 30-150 19:45 94 M Benzo[a]pyrene-d12 20:18 72 30-150 20:16 268 M Perylene-d12 20:27 74 30-150 20:27 115 M Indeno[1,2,3-cd]pyrene-d12 22:20 97 30-150 22:21 91 M Dibenzo[a,h]anthracene-d14 22:23 101 30-150 22:25 56

Benzo[g,h,i]perylene-d12 22:44 95 30-150 22:44 116 M

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated. U Indicates that this com p ound was not detected above the MDL. E Indicates that this com p ound was detected above the calibrated ran g e. J indicates that a tar g et anal y te was detected below the LQL. Flags 16-Nov-14 09:18 10 FURNACE 12 RUN#3

16-Nov-14 09:53 Ella Gd y cz y nski --e-si g nature-- 1 

# ALS Environmental

16-Oct-14 28-Oct-14 Approved:

Flags Sample Analysis Report

17-Nov-2014 Stack CARB 429 Modified train n/a

ALS Canada Ltd L1535265 141118 Page 14 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID L1535265-1 0 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e Sam pl e Moisture Content Sample Matrix Split Ratio

Run Information Run 1 Run 2

Filename 4-141115B1 6 4-141115B11 Run Date Final Volume 1000 u L 1000 u L Dilution Factor 1 50 Anal y sis Units n g n g Instrument - Column HRMS-4 Rxi5Sil1117926 HRMS-4 Rxi5Sil1117926

Ret. Conc. EDL Ret. Conc. EDL Tar g et Anal y tes Time n g n g Time. n g n g

Naphthalene 7:34 43100 43 E 7:33 43900 93 M 2-Me-Naphthalene 8:44 16400 3.9 M 8:42 15100 38 M 1-Me-Naphthalene 8:54 11700 4.0 M 8:52 13500 40 M

Acenaphthylene 10:10 19100 2.9 M 10:09 14900 28 M

Acenaphthene 10:27 2050 5.8 M 10:27 2350 30 M J
Fluorene 11:18 3080 2.0 M 11:17 3650 15 M J
Phenanthrene 12:50 34100 11 M E 12:50 43500 56 M

Anthracene 12:55 6300 11 M 12:55 10500 71 M
Fluoranthene 14:47 38400 14 M E 14:46 30400 78 M Pyrene 15:10 25600 13 M E 15:09 23100 72 M Benz[a]anthracene 17:32 3290 1.1 M 17:35 4350 86 M J Chrysene/Triphenylene 17:36 5200 1.1 M 17:35 5000 99 M

Benzo[b]fluoranthene 19:44 3160 2.8 M 19:45 3470 160 M J Benzo[k]fluoranthene 19:47 1250 3.2 M 19:47 1470 170 M J Benzo[e]pyrene 20:15 1660 3.7 M 20:14 1140 42 M J Benzo[a]pyrene 20:21 681 3.8 M 20:23 160 43 M J Perylene 20:31 133 2.9 M 20:31 <40 40 M U Indeno[1,2,3-cd]pyrene 22:22 980 1.7 M 22:24 707 81 M J Dibenzo[a,h]anthracene 22:27 204 2.7 M 22:29 <140 140 M U

Benzo[g,h,i]perylene 22:47 807 1.0 M 22:48 868 48 M J

Field Spike Standards % Rec Limits % Rec

Fluorene-d10 11:15 104 50-150 11:14 113 p-Terphenyl-d14 15:34 85 50-150 15:34 85

Extraction Standards % Rec Limits % Rec

Naphthalene-d8 7:32 69 20-150 7:31 95 2-Me-Naphthalene-d10 8:40 71 20-150 8:40 87 Acenaphthylene-d8 10:09 68 20-150 10:08 87
Phenanthrene-d10 12:48 66 30-150 12:48 77

Anthracene-d10 12:54 59 30-150 12:53 81
Fluoranthene-d10 14:45 69 30-150 14:44 87 Benz[a]anthracene-d12 17:29 44 30-150 17:30 36 Chrysene-d12 17:33 35 30-150 17:30 22 Benzo[b]fluoranthene-d12 19:41 67 30-150 19:41 56 Benzo[k]fluoranthene-d12 19:45 54 30-150 19:45 43 Benzo[a]pyrene-d12 20:18 56 30-150 20:21 111 Perylene-d12 20:28 57 30-150 20:27 151 Indeno[1,2,3-cd]pyrene-d12 22:20 58 30-150 22:22 37 M Dibenzo[a,h]anthracene-d14 22:23 56 30-150 22:27 25 M

Benzo[g,h,i]perylene-d12 22:44 55 30-150 22:45 42 M

ED L Indicates the Estimated Detection Limit, based on the measured back g round noise for this tar g et in this sam p le. M Indicates that a p eak has been manuall y inte g rated. U Indicates that this com p ound was not detected above the MDL. E Indicates that this com p ound was detected above the calibrated ran g e. J indicates that a tar g et anal y te was detected below the LQL. Stack 10 FURNACE 12 RUN# 4

CARB 429 Modified train n/a 1 Sample Analysis Report

16-Nov-14 10:27 

# ALS Environmental

16-Oct-14 28-Oct-14 Approved: Ella Gd y cz y nski --e-si g nature--

17-Nov-2014

Flags Flags 16-Nov-14 07:35

ALS Canada Ltd L1535265 141118 Page 15 of 16Sam p le Name Sam p lin g Date ALS Sam p le ID WG1980014- 2 Extraction Date Anal y sis Method Sam p le Size Ana ly sis T yp e LCS Moisture Content Sample Matrix Split Ratio

Run Information Run 1

Filename 4-141115A1 0 Run Date Final Volume 1000 u L Dilution Factor 1 Anal y sis Units % Instrument - Column HRMS-4 Rxi5Sil1117926

Ret. Tar g et Anal y tes Time % Rec Limit s

Naphthalene 7:34 123 50-150 2-Me-Naphthalene 1-Me-Naphthalene

Acenaphthylene 10:10 98 50-150

Acenaphthene 10:27 103 50-150
Fluorene 11:18 105 50-150
Phenanthrene 12:50 99 50-150

Anthracene 12:55 101 50-150
Fluoranthene 14:47 102 50-150 Pyrene 15:10 92 50-150 Benz[a]anthracene 17:32 103 50-150 Chrysene/Triphenylene 17:36 97 50-150

Benzo[b]fluoranthene 19:43 109 50-150 Benzo[k]fluoranthene 19:47 103 50-150 Benzo[e]pyrene Benzo[a]pyrene 20:20 89 50-150 Perylene Indeno[1,2,3-cd]pyrene 22:21 111 50-150 Dibenzo[a,h]anthracene 22:26 104 50-150

Benzo[g,h,i]perylene 22:46 104 50-150

Field Spike Standards % Rec Limits

Fluorene-d10 11:15 n/s p-Terphenyl-d14 15:34 n/s

Extraction Standards % Rec Limits

Naphthalene-d8 7:32 85 20-150 2-Me-Naphthalene-d10 8:40 81 20-150 Acenaphthylene-d8 10:08 84 20-150
Phenanthrene-d10 12:48 80 30-150

Anthracene-d10 12:53 74 30-150
Fluoranthene-d10 14:45 91 30-150 Benz[a]anthracene-d12 17:29 56 30-150 Chrysene-d12 17:33 50 30-150 Benzo[b]fluoranthene-d12 19:40 85 30-150 Benzo[k]fluoranthene-d12 19:44 79 30-150 Benzo[a]pyrene-d12 20:17 75 30-150 Perylene-d12 20:27 79 30-150 Indeno[1,2,3-cd]pyrene-d12 22:19 79 30-150 Dibenzo[a,h]anthracene-d14 22:22 80 30-150

Benzo[g,h,i]perylene-d12 22:44 81 30-150

n/s Indicates that this standard has not been s p iked. Flags 1 Laborator y Control Sam p l e

15-Nov-14 17:53 Ella Gd y cz y nski --e-si g nature-- 1 

# ALS Environmental

n/a 28-Oct-14 Approved: Laboratory Control Sample Analysis Report

17-Nov-2014 QC CARB 429 Modified n/a

ALS Canada Ltd L1535265 141118 Page 16 of 16

### MERCURY

### APPENDIX D

PROCESS DATA

### Furnace 1

### Furnace 12

### Hi Tom,

We calculated the rate that each furnace consumed electrode in lbs/hr , specifically, how many pounds of electrode were consumed during each stack test run in October. We don’t track individual electrodes, just the rate at which continuous electrode is consumed, which depends on various factors during a specific test. For percent composition, please see the attached SDS.

Fce 1, 10/15

Run Time (min) Run Time (hrs) Electrode Consumed (lbs) Rate (lbs/hr)

94 1.567 1789 1142 95 1.583 1953 1234 95 1.583 1463 924.2 93 1.550 1270 819.4

Fce 12, 10/16

Run Time (min) Run Time (hrs) Electrode Consumed (lbs) Rate (lbs/hr)

73 1.22 106 86.9 74 1.23 348 283 73 1.21 622 514 73 1.21 655 541

### Electrode Paste Safety Data Sheet

### APPENDIX E

QUALITY ASSURANCE/QUALITY CO NTROL

### CALIBRATION PROCEDUR ES AND RESULTS

All of the equipment used is calibrated in accordance with the procedures outlined in the
Quality Assurance Handbook for Air Pollution Measurement Systems, Volume III ( EPA

- 600/4

-
77

- 027b). The following pages describe these procedures and include the data sheets.

### STACK THERMOCOUPLES

Each thermocouple is calibrated by comparing it with an ASTM

- 3F thermometer at
approximately 32°F, ambient temperature, 212°F, and 500°F. The thermocouple reads within
1.5 percent of the reference thermometer throughout the entire range when expressed in degrees
Rankine. The thermocouples may be checked at ambient temperature at the test site to verify the

calibration. Calibrat ion data are included in the following Thermocouple Calibration Data
Sheet(s).

### TEMPERATURE SENSOR CALIBRATION DATA FORM FOR SAMPLE HEADS

12/23/2013
Reference point number Source a

(Specify) Reference

Thermometer Temperature, o F Thermocouple

Potentiometer Temperature, o F Temperature

Difference, b

o F Sample Head No. 1 1 Ambient Air 72 70 2 

### ACCEPT 2 Cold Bath 34 34 0 Sample Head No. 2 1 Ambient Air 71 70 1 

### ACCEPT 2 Cold Bath 34 34 0 Sample Head No. 3 1 Ambient Air 71 70 1 

### ACCEPT 2 Cold Bath 34 34 0 Sample Head No. 4 1 Ambient Air 72 70 2 

### ACCEPT 2 Cold Bath 34 34 0 Sample Head No. 5 1 Ambient Air 71 70 1 

### ACCEPT 2 Cold Bath 34 33 1 Sample Head No. 6 1 Ambient Air 72 70 2 

### ACCEPT 2 Cold Bath 34 34 0 Sample Head No. 7 1 Ambient Air 71 70 1 

### ACCEPT 2 Cold Bath 34 33 1 Sample Head No. 8 1 Ambient Air 71 69 2 

### ACCEPT 2 Cold Bath 34 33 1 Sample Head No. 9 1 Ambient Air 71 69 2 

### ACCEPT 2 Cold Bath 34 35 1 Sample Head No. 10 1 Ambient Air 72 72 0 

### ACCEPT 2 Cold Bath 34 33 1 Sample Head No. 11
1 

### ACCEPT 2

a Type of calibration used. Calibrated By: BF
b Allowable tolerance + 2 o F

### En vironmental Quality Management, Inc.

Dry Gas Meter and Orifice Meter.doc

DRY GAS METER AND ORIFICE METER

Dry gas meters and orifices are calibrated in accordance with Section 3.3.2 of the QA
Handbook. This procedure involves direct comparison of the dry gas meter to a reference dry
test meter. The reference dry test mete r is routinely calibrated using a liquid displacement
technique. Before its initial use in the field, the metering system is calibrated over the entire
range of operation. After each field use, the metering system is calibrated at a single

intermediate s etting based on the previous field test. Acceptable tolerances for the initial and
final gas meter factors and orifice calibration factors are  0.02 and  0.20 from average,
respectively.

### En vironmental Quality Management, Inc.

PitotTubeCalibration .doc

### En vironmental Quality Management, Inc.

PITOTS 2014.doc ENVIRONMENTAL QUALITY MANAGEMENT PITOT TUBE CALIBRATIONS

### En vironmental Quality Management, Inc.

PITOTS 2014.doc ENVIRONMENTAL QUALITY MANAGEMENT PITOT TUBE CALIBRATIONS

### En vironmental Quality Management, Inc.

Trip Balance .doc TRIP BALANCE

The trip balance is calibrated by comparing it with Class

- S standard weights, and it
agreed within 0.5g. Calibration data are shown in the following Trip Balance Calibration Data
Sheet(s).

### En vironmental Quality Management, Inc.

Barometer .doc BAROMETER

The field barometer is calibrated to within 0.1 in. Hg of an NBS

- traceable mercury

- in

glass barometer before the test series. It is checked against the reference barometer after each
test series to determine if it reads within 0.2 in. Hg. The barometer reads within the allowable
limits each time. Calibration data are included in the following Barometer Calibration Log(s).

### Quality Assurance Checks

Furnace 1

### Furnace 12

### APPENDIX F

TEST PROTOCOL

### SUMMARY OF ERAMET VOLUNTARY PAH AND MERCURY EMISSIONS TEST PLAN TO

SUPPORT FERROMANGANESE AND SILICOMANGANESE NESHAP RULEMAKING

SEPTEMBER 23, 2014; REVISI ON 0 Page 1 of 3

Eramet Marietta Inc. (EMI) is planning to conduct a voluntary test program during the week of October 13, 2014 to characterize polycyclic aromatic hydrocarbon (PAH) and mercury emissions from electric arc furnaces 1 (main baghouse outlet) and 12 (scrubber outlet) during production of silicomanganese and ferromanganese alloys at its facility in Marietta, Ohio.

The overall goal of the tests is to supplement very limited data from previous tests and thereby gain a better understanding of the range and variabi lity of actual emissions during production, using test measurement methods specified by EPA in the proposed NESHAP.

Environmental Quality Management, Inc. (EQ) will perform the measurements, with laboratory analysis support from ALS in Burlington, Ontario (Canada). This summary outlines key aspects of the tests.

1. The objectives of the tests are:

1.1. To obtain at least three valid PAH and mercury emissions measurements at each exhaust;

1.2. To determine and document measurement data quality, and achieve measurement d ata quality acceptable for rulemaking purposes;

1.3. To document emissions from Furnace 12 scrubber during silicomanganese production;

1.4. To document emissions from Furnace 1 main baghouse during ferromanganese production;

1.5. To document furnace feeds and operating c onditions during the tests.

2. Following is a summary of planned PAH sampling and analysis activities:

2.1. EQ will conduct four test runs (sampling and analysis) at each location in order to assure at least three valid test runs.

2.2. The tests will be conducted under the direction of a Qualified Source Test Individual (QSTI).

2.3. Each PAH sampling run will attempt to encompass one entire furnace heat cycle (tap to tap). It is anticipated that each sample run time will be approximately 70

- 90 minutes. The sampling duration and sample gas volume will be less than in the 2012 tests. Based on the PAH amount (~1

- 160 milligrams) encountered in those tests, shorter runs are expected to provide sufficient PAH for analysis.

2.4. EQ will follow the procedures specified in California Air Resources Board (CARB) Method 429 to collect and analyze the samples. The method will be used as published, except the analytical procedure will be adjusted to accommodate potentially higher PAH concentrations based on the results of earlier tests.

### SUMMARY OF ERAMET VOLUNTARY PAH AND MERCURY EMISSIONS TEST PLAN TO

SUPPORT FERROMANGANESE AND SILICOMANGANESE NESHAP RULEMAKING

SEPTEMBER 23, 2014; REVISI ON 0 Page 2 of 3

2.4.1. High re solution gas chromatography and high resolution mass spectroscopy will be used for sample analysis.

2.4.2. Laboratory analysis will be expedited to the extent possible for fastest available turnaround consistent with data quality objectives. For high resolution analyses, a three

- week turnaround is the shortest period provided by ALS.

2.4.3. Instrument Calibration range will be 0.002 to 2 ug/mL. The upper range will be expanded by dilutions and by increasing the labeled spiking levels (i.e. the Split Factor).

2.4.4. XAD

- 2 re sin cartridges will be spiked based on the historic sampling results. A spike of 1000 ng per target compound will be used based on a split design of 10 and 100 ng per split.

2.4.5. The initial labeled internal standard spiking levels were selected to provide mea surable quantities anticipating that the sample may need to be diluted prior to analysis. The spiking levels are designed to provide measurable spike recoveries at over an analytical dilution factor range of 1 to 50 ng total PAH. At this dilution range and the planned spiking levels, the minimum quantifiable total PAH will range from 2.5 to 4000 ng. For a sample volume of approximately 1 dscm, the in

- stack equivalent of the minimum analytical quantification limit corresponds to a total PAH concentration of 2.5 to 4000 ng/dscm.

2.4.6. If higher dilutions are required beyond the level at which the labeled internal standards can be measured, the dilute will be fortified with the labeled internal standards. While this represents a compromise over selecting higher initi al spiking levels by increasing measurement uncertainty, it provides a means of correcting the samples for spike recoveries at higher PAH concentrations characteristic of the single 7/2012 test while also providing reasonably low quantification minimums in the event PAH levels are lower, based on the 10/2012 tests.

3. Following is a summary of mercury sampling and analysis activities:

3.1. EQ will conduct four test runs (sampling and analysis) at each location in order to assure at least three valid test runs.

3.2. The tests will be conducted under the direction of a Qualified Source Test Individual (QSTI).

3.3. Each mercury sampling run will attempt to encompass an entire furnace heat cycle. It is anticipated that the sample run time will be approximately 70

- 90 minutes.

3.4. Mer cury test runs will be conducted during the PAH sampling runs.

### SUMMARY OF ERAMET VOLUNTARY PAH AND MERCURY EMISSIONS TEST PLAN TO

SUPPORT FERROMANGANESE AND SILICOMANGANESE NESHAP RULEMAKING

SEPTEMBER 23, 2014; REVISI ON 0 Page 3 of 3

3.5. Measurements will be made following USEPA Method 30B (sorbent tube approach).

3.5.1. The method will be performed as published.

3.5.2. Paired sampling tubes operated in parallel will be used during each tes t

run. 1 tube will be spiked with a known quantity of mercury for quality assurance purposes, as specified in the test method, and the second will be unspiked.

4. With expedited lab turnaround it is anticipated that a final report will be available for EPA

r eview by November 24, 2014.. 1280 Arrowhead Ct., Suite 2,
. Crown Point, Indiana 46308
. (219) 661-9900/ FAX (219) 661-9902