# Results of the April 12-13, 2011 Sulfuric Acid

Mist and Sulfur Dioxide Performance Tests at the United Taconite, LLC Facility Located in Forbes, Minnesota

Line 2 Waste Gas Stack 2A (SV048) Line 2 Waste Gas Stack 2B (SV049)



# MPCA AQD File No. 869A Air Emissions Permit No. 13700113-005 Barr Project No. 23/69-1092.06

Prepared for United Taconite, LLC Forbes, Minnesota

April 2011

### i



# Results of the April 12-13, 2011 Sulfuric Acid Mist and Sulfur Dioxide Performance Tests at the United Taconite, LLC Facil ity Located in Forbes, Minnesota

Table of Contents

Report Certification...............................

................................................... ................................................... . iii
Executive Summary .................................

................................................... .................................................. v

Introduction ......................................

................................................... ................................................... ....... 1
Results Summary ...................................

................................................... ................................................... . 2
Process Description ...............................

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

Stack Test Procedures and Methods .................

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

Tables Figures Appendices23691092.06 

### ii List of Tables

Table 1 EPA Method 8 Test Results – Line 2 Waste Ga s Stack – 2A (SV048)-Gas
Table 2 EPA Method 8 Test Results – Line 2 Waste Ga s Stack – 2B (SV049)-Gas
Table 3 EPA Method 8 Test Results – Line 2 Waste Ga s Stack – 2A (SV048)-Solid Fuel
Table 4 EPA Method 8 Test Results – Line 2 Waste Ga s Stack – 2B (SV049)-Solid Fuel
Table 5 Derivation of SAM to SO 2 

### Ratios – Line 2 (SV048 and SV049)

List of Figures
Figure 1 Test Port Locations – Line 2A Waste Gas St ack (SV048, EU042) Figure 2 Traverse Point Location – Line 2A Waste Ga s Stack (SV048, EU042) Figure 3 Test Port Locations – Line 2B Waste Gas St ack (SV049, EU042) Figure 4 Traverse Point Location – Line 2B Waste Ga s Stack (SV049, EU042)

List of Appendices
Appendix A Report Calculations and Nomenclature Appendix B Field Data Sheets Appendix C Laboratory Reports and Sample Chain of C ustody Appendix D Calibration Data Appendix E Cylinder Gas Certifications Appendix F Process Operating Data Appendix G Stack Test Plan Appendix H Project Participants and Contact Informa tion23691092.06


### v 

# Executive Summary

Barr Engineering Company conducted sulfuric acid mi st (SAM) and sulfur dioxide (SO 2 

### ) emissions performance tests on the Line 2 kiln (Emission Unit 042) 2A (SV048) and 2B (SV049) waste gas stacks at the United Taconite, LLC taconite production fac ility located in Forbes, Minnesota. The two waste gas stacks were tested simultaneously on April 12, 2011 while the Line 2 kiln was burning natural gas and again on April 13, 2011 while furnace was firin g on solid fuel.

The purposes of these tests were to determine the r atio of SAM to SO 2 

### emissions to use with Line 2 SO 2 

### continuous emissions monitors (CEM) data to demonst rate ongoing compliance with 30 day rolling average SAM limit and to verify the ratio of SAM to SO 2 

### used in the permit application. The testing was completed prior to commencement of construction for modifications to Line 1 furnace (EU040) to burn solid fuel as authorized by Air Emission Permi t No. 13700113-005. Results of the tests performed are summarized in the Executive Summary Table.23691092.06 

### vi 

# Executive Summary Tables

EPA Method 8 - Gas Condition Average Test Results

Source Line 2 WGS – 2A Line 2 WGS – 2B Stack Vent No. SV048 SV049 Emission Unit EU042 Test Date 4/12/2011 Volumetric Airflow Rate, DSCFM 305,000 309,000 Concentration Sulfuric Acid Mist, lb/dscf 2.3 x 10 -7 

### 2.8 x 10 -7 

### Sulfur Dioxide, lb/dscf 1.2 x 10 -6 

### 6.8 x10 -6


### Emission Rates Sulfuric Acid Mist, lb/hr 4.2 5.1 Sulfur Dioxide, lb/hr 21.9 12.6 Sulfuric Acid Mist Combined Emissions, lb/hr 9.3 Sulfur Dioxide Combined Emissions, lb/hr 34.5 Ratio Sulfuric Acid Mist : Sulfur Dioxide 0.300

EPA Method 8 – Solid Fuel Condition Average Test Re sults
Source Line 2 WGS – 2A Line 2 WGS – 2B Stack Vent No. SV048 SV049 Emission Unit EU042 Test Date 4/13/2011 Volumetric Airflow Rate, DSCFM 312,000 317,000 Concentration Sulfuric Acid Mist, lb/dscf 4.9 x 10 -7 

### 6.4 x 10 -7 

### Sulfur Dioxide, lb/dscf 2.1 x 10 -5 

### 1.8 x 10 -5


### Emission Rate Sulfuric Acid Mist, lb/hr 9.1 12.2 Sulfur Dioxide, lb/hr 391 342 Sulfuric Acid Mist Combined Emissions, lb/hr 21.3 Sulfur Dioxide Combined Emissions, lb/hr 734 Ratio Sulfuric Acid Mist : Sulfur Dioxide 0.02923691092 

### 1 

# Introduction

Barr Engineering Company conducted sulfuric acid mi st (SAM) and sulfur dioxide (SO 2 

### ) emissions performance tests at the Line 2 kiln (Emission Unit 042) 2A (SV048) and 2B (SV049) waste gas stacks at the United Taconite, LLC (UTAC) taconite product ion facility located in Forbes, Minnesota. The two waste gas stacks were tested simultaneously on April 12, 2011 while kiln was burning natural gas and again on April 13, 2011 while the kiln was firi ng on solid fuel. The purposes of these tests were to
determine the ratio of SAM to SO 2 

### emissions to use with Line 2 SO 2 

### continuous emissions monitors (CEM) data to demonstrate ongoing compliance with 3 0 day rolling average SAM limit and to verify
the ratio of SAM to SO 2 

### used in the permit application. The testing was c ompleted prior to
commencement of construction for modifications to L ine 1 furnace (EU040) to burn solid fuel as authorized by Air Emission Permit No. 13700113-005.

A test plan dated December 22, 2010 was submitted t o the Minnesota Pollution Control Agency (MPCA) prior to testing. Testing was initially sch eduled for January 12, 2011. The testing was delayed several times due to problems with achievin g maximum solid fuel feed to the furnace. The testing was discussed with Andy Place of the MPCA s everal times leading up to the actual testing performed. A test plan approval letter was provide d January 24, 2011 by Andrew Place. Subsequent modifications to the testing approach were discusse d with Andy Place and are documented in e-mail correspondence provided in Appendix G. Copies of t he original test plan and approval form are also provided in Appendix G.

Dan Koschak led the Barr test teams. Candice Maxwe ll and Lisa Weidemann of UTAC provided testing coordination. The tests were not witnessed by a representative of the MPCA. A list of projec t participants is provided in Appendix H.

The testing consisted of three one-hour test runs a t each stack for determination of SAM and SO 2 

### concentrations and emission rates by EPA Method 8. The tests were performed simultaneously for each fuel condition at the Line 2 (EU042) waste gas stac ks (2A SV048 and 2B SV049) as required in the permit. Test results are located in the following section. Field data along with other supporting documentation are located in the appendices.23691092 

### 2 

# Results Summary

Tables 1 and 2 present the results of the SAM and S O 2 

### tests for Line 2 waste gas stack 2A (SV048) and 2B (SV049), respectively. These tests were conduct ed on April 12 while the kiln was firing on 100 percent natural gas. The total emission rate from Emission Unit 042 of SAM is 9.3 pounds per hour (lb/hr) and the SO 2 

### emission rate is 34.5 lb/hr.

Tables 3 and 4 present the results of the SAM and S O 2 

### tests for Line 2 waste gas stack 2A (SV048) and 2B (SV049), respectively. These tests were conduct ed on April 13 while the kiln was firing on 100 percent solid fuel. The total emission rate from E mission Unit 042 of SAM is 21.3 lb/hr and the SO 2 

### emission rate is 734 lb/hr.

Table 5 presents a summary of the emission unit com bined SAM and SO 2 

### emissions and calculated
ratios. The SAM to SO 2 

### ratio while firing on natural gas is 0.300. The r atio of SAM to SO 2 

### while firing on solid fuel is 0.029. Table 5 also includ es calculated data for verification of ratios used in the permit application.

No testing difficulties or process delays were note d during the performance tests.

The tests were performed at normal production rates while the Line 2 furnace was firing natural gas an d solid fuel. The process operating data are summari zed in Tables 1-4 and the detailed process data are located in Appendix F along with MPCA required proc ess operating data forms and solid fuel analysis data. Solid fuel samples were collected during each test run on April 13, 2011 by UTAC and analyzed by Twin Ports Testing. Results of the fuel analysi s are located in Appendix F- Process Operating Data

.23691092 

### 3 

# Process Description

Line 2A and B Waste Gas Stacks (EU042, SV048, SV049 )

The Line 2 pellet induration is an Allis Chalmers r otary kiln (serial number B-41301), which is 130 fe et in length with a 21’ 6” diameter. The pellets pass through the kiln where they are heated to approximately 2400 degrees Fahrenheit. The heated gases from the kiln are mixed with recouped hot air from the pellet cooler. This air is used to dr y the green pellets prior to the kiln in the prehea t zones. The waste gases are divided into two sides which ar e served by identical Ducon venturi scrubbers (Size 825/222 Type VVO), Side A (CE050, SV048) and Side B (CE049, SV049).23691092 

### 4 

# Stack Test Procedures and Methods

Testing was performed from ports meeting EPA Method 1 criteria. The Method 1 criteria are listed in the table below. Sample port location and traverse point details are provided in Figures 1-4.

Location SV# Distance to

upstream Disturbance, (diameters) Distance to

downstream Disturbance, (diameters) Number of

ports Number of

Points

SV048 ~7.9 2.1 4 12 SV049 ~7.9 2.1 4 12



### Volumetric airflow determinations were performed in accordance with EPA Method 2 using an S type pitot tube. Airflows were determined in conjunctio n with the EPA Method 8 test.

Oxygen and carbon dioxide compositions of the Line 2 kiln 2A and 2B waste gas stacks were determined by modified EPA Method 3A. An integrate d sample of dry stack gas was collected in a Tedlar bag through the duration of each test run. The samples were analyzed using a Servomex Model 1440 oxygen and carbon dioxide analyzer calibrated with EPA Protocol gases. Copies of calibration gas certifications are located in Appendix E.

Stack gas moisture content was determined by the pe rformance of EPA Method 4, in conjunction with the EPA Method 8 sample trains.

SAM and SO 2 

### concentrations were determined with EPA Method 8. The sample train configuration, sample and sample recovery was completed per the me thod. The hydrogen peroxide reagent was prepared fresh daily on-site. Sample trains were p urged with ambient air after the test runs. Sample s were analyzed by Enthalpy Analytical using the titr ation method. A copy of the sample chain of custody and laboratory report is located in Appendi x C.

EPA Methods 1-4 and 8 can be found in 40 CFR Part 6 0, Appendix A.

# Tables

### Cliffs Natural Resources Barr Engineering Co.

United Taconite April 29, 2011 Forbes, Minnesota

TABLE 1

EPA METHOD 8 TEST RESULTS
2A Waste Gas Stack (SV048) - Gas

Parameter Run 1 Run 2 Run 3 Average Scrubber - Pressure Drop, in. H 2 

### O 11.4 10.9 10.9 11.1 Scrubber - Water Flow Rate, gal/min 2,412 2,412 2,413 2 ,412 Test Date 4/12/2011 4/12/2011 4/12/2011 --- Test Period 858 - 1004 1148 - 1253 1405 - 1509 --- Test Duration, min. 60 60 60 60 Avg. Stack Temperature, deg.F 136 137 138 137 Avg. Moisture Content, %V/V 12.1 12.7 13.1 12.6 EPA Method 8 Laboratory Results, μ g

SO 3 

### /SO 4 

### 3,600 2,870 3,270 3,247 SO 2 

### 15,800 15,400 20,000 17,067 Air Flow Rate acfm 419,000 413,000 414,000 415,000 scfm 353,000 348,000 348,000 350,000 dscfm 310,000 304,000 302,000 305,000 Sample Volume acf 32.58 33.36 33.62 33.19 dscf 31.65 31.52 31.22 31.46

Isokinetic Variation, % 98.7 100.2 99.9 99.6

Concentration, lb/dscf SO 3 

### /SO 4 

### 2.5E-07 2.0E-07 2.3E-07 2.3E-07 SO 2 

### 1.1E-06 1.1E-06 1.4E-06 1.2E-06

Emissions Rate, lb/hr SO 3 

### /SO 4 

### 4.7 3.7 4.2 4.2 SO 2 

### 20.5 19.7 25.6 21.9 Process Rates

Green Ball Feed Rate, LTPH 630 641 643 638 Fired Pellet Production Rate, LTPH 507 510 514 510

### Cliffs Natural Resources Barr Engineering Co.

United Taconite April 29, 2011 Forbes, Minnesota

TABLE 2

EPA METHOD 8 TEST RESULTS
2B Waste Gas Stack (SV049) - Gas

Parameter Run 1 Run 2 Run 3 Average Scrubber - Pressure Drop, in. H 2 

### O 10.2 9.7 9.7 9.9 Scrubber - Water Flow Rate, gal/min 2,499 2,496 2,498 2 ,498 Test Date 4/12/2011 4/12/2011 4/12/2011 --- Test Period 856 - 1006 1148 - 1255 1405 - 1511 --- Test Duration, min. 60 60 60 60 Avg. Stack Temperature, deg.F 129 135 137 134 Avg. Moisture Content, %V/V 13.5 13.2 14.0 13.6 EPA Method 8 Laboratory Results, μ g

SO 3 

### /SO 4 

### 4,310 3,530 4,450 4,097 SO 2 

### 9,280 9,570 11,400 10,083 Air Flow Rate acfm 427,000 425,000 414,000 422,000 scfm 364,000 359,000 349,000 357,000 dscfm 315,000 312,000 300,000 309,000 Sample Volume acf 34.45 34.10 33.61 34.05 dscf 33.43 32.81 31.92 32.72

Isokinetic Variation, % 101.6 100.8 101.9 101.5

Concentration, lb/dscf SO 3 

### /SO 4 

### 2.8E-07 2.4E-07 3.1E-07 2.8E-07 SO 2 

### 6.1E-07 6.4E-07 7.9E-07 6.8E-07

Emissions Rate, lb/hr SO 3 

### /SO 4 

### 5.4 4.4 5.5 5.1 SO 2 

### 11.6 12.0 14.2 12.6

Ratio of Sulfuric Acid Mist to SO 2 

### , % 46 37 39 41 Process Rates

Green Ball Feed Rate, LTPH 630 640 643 638 Fired Pellet Production Rate, LTPH 507 510 514 510

### Cliffs Natural Resources Barr Engineering Co.

United Taconite April 29, 2011 Forbes, Minnesota

TABLE 3

EPA METHOD 8 TEST RESULTS
2A Waste Gas Stack (SV048) - Solid Fuel

Parameter Run 1 Run 2 Run 3 Average Scrubber - Pressure Drop, in. H 2 

### O 11.5 11.5 11.3 11.4 Scrubber - Water Flow Rate, gal/min 2,412 2,411 2,412 2 ,412 Test Date 4/13/2011 4/13/2011 4/13/2011 --- Test Period 836 - 941 1034 - 1141 1240 - 1344 --- Test Duration, min. 60 60 60 60 Avg. Stack Temperature, deg.F 135 135 135 135 Avg. Moisture Content, %V/V 12.3 12.2 12.5 12.3 EPA Method 8 Laboratory Results, μ g

SO 3 

### /SO 4 

### 7,390 7,260 6,310 6,987 SO 2 

### 303,000 312,000 287,000 300,667 Air Flow Rate acfm 419,000 421,000 419,000 420,000 scfm 355,000 357,000 355,000 356,000 dscfm 311,000 313,000 311,000 312,000 Sample Volume acf 33.88 34.37 33.36 33.87 dscf 31.75 32.10 31.10 31.65

Isokinetic Variation, % 98.8 99.2 96.9 98.3

Concentration, lb/dscf SO 3 

### /SO 4 

### 5.1E-07 5.0E-07 4.5E-07 4.9E-07 SO 2 

### 2.1E-05 2.1E-05 2.0E-05 2.1E-05

Emissions Rate, lb/hr SO 3 

### /SO 4 

### 9.6 9.4 8.3 9.1 SO 2 

### 393 403 379 391

Ratio of Sulfuric Acid Mist to SO 2 

### , % 2.4 2.3 2.2 2.3 Process Rates

Green Ball Feed Rate, LTPH 646 646 643 645 Fired Pellet Production Rate, LTPH 520 520 512 517

### Cliffs Natural Resources Barr Engineering Co.

United Taconite April 29, 2011 Forbes, Minnesota

TABLE 4

EPA METHOD 8 TEST RESULTS
2B Waste Gas Stack (SV049) - Solid Fuel

Parameter Run 1 Run 2 Run 3 Average Scrubber - Pressure Drop, in. H 2 

### O 10.3 10.3 10.0 10.2 Scrubber - Water Flow Rate, gal/min 2,497 2,496 2,499 2 ,497 Test Date 4/13/2011 4/13/2011 4/13/2011 --- Test Period 836 - 943 1034 - 1141 1240 - 1346 --- Test Duration, min. 60 60 60 60 Avg. Stack Temperature, deg.F 126 124 125 125 Avg. Moisture Content, %V/V 11.8 13.1 12.0 12.3 EPA Method 8 Laboratory Results, μ g

SO 3 

### /SO 4 

### 9,630 10,400 8,940 9,657 SO 2 

### 272,000 283,000 256,000 270,333 Air Flow Rate acfm 420,000 415,000 422,000 419,000 scfm 362,000 358,000 364,000 361,000 dscfm 319,000 311,000 320,000 317,000 Sample Volume acf 33.67 33.87 33.90 33.81 dscf 33.05 33.09 33.10 33.08

Isokinetic Variation, % 99.2 101.8 99.0 100.0

Concentration, lb/dscf SO 3 

### /SO 4 

### 6.4E-07 6.9E-07 6.0E-07 6.4E-07 SO 2 

### 1.8E-05 1.9E-05 1.7E-05 1.8E-05

Emissions Rate, lb/hr SO 3 

### /SO 4 

### 12.3 12.9 11.4 12.2 SO 2 

### 347 352 328 342

Ratio of Sulfuric Acid Mist to SO 2 

### , % 3.5 3.7 3.5 3.6 Process Rates

Green Ball Feed Rate, LTPH 646 646 643 645 Fired Pellet Production Rate, LTPH 520 520 512 517

### Cliffs Natural Resources Barr Engineering Co.

United Taconite April 29, 2011 Forbes, Minnesota

Parameter firing solid fuel firing natural gas Fired Pellet Production Rate, LT pellets/hr 517 510 SAM Emission Rate, lb SAM/hr 21.3 9.3 SO 2 

### Emission Rate 734 34.5 Ratio of SAM:SO 2 

### Emission Rates 0.029 0.300 S in SAM, lb S/hr 6.96 3.03 S in SO 2 

### , lb S/hr 367 17.3 Total S from ore and solid fuel, lb S/hr 374

S in SAM in ore per unit production, lb S/LT pellet s 0.0059 S in SO 2 

### in ore per unit production, lb S/LT pellets 0.034

S in SAM from ore, lb S/hr 3.07 S in SO 2 

### from ore, lb S/hr 17.5 S in SAM from solid fuel, lb S/hr 3.89 S in SO 2 

### from solid fuel, lb S/hr 349 S from solid fuel, lb S/hr 353 % of S in solid fuel that converts to SAM 1.1% % of S in solid fuel that converts to SO 2 

### 98.9% Ratio of S in solid fuel that converts to SO 2 

### vs SAM 98.9 : 1.1 TABLE 5

Assume all S produced while firing 100 % natural ga s comes from the ore. This should relate to the pellet production rate:

Multiply the lb S/LT pellets from natural gas (i.e. , a measure of S from the ore) by the LT pellets/hr when firing solid fuel: Line 2 (SV048 and SV049) DERIVATION OF SAM TO SO 2 

### RATIOS

# Figures

# Appendices

# Appendix A

Report Calculations and NomenclatureCliffs Natural Resources Barr Engineering Co. United Taconite April 27, 2011 Forbes, Minnesota

Determination of Volumetric Airflow Rate, Gas Compo sition, Moisture Content, and sulfuric acid mist EPA Methods 2, 3, 4, 8 TEST 1 2A WGS (SV048) Input Data Symbol Units Run 1 Run 2 Run 3
Test Date - - 4/12/2011 4/12/2011 4/12/2011 Test Period - - 858 - 1004 1148 - 1253 1405 - 1509 Number of Sample Ports - - 4 4 4 Number of Traverse Points - - 12 12 12 Duct Dimensions (diameter or Length x Width) D, L X W inches 147.00 147.00 147.00 Barometric Pressure Pbar in. Hg 28.52 28.52 28.52 Stack Static Pressure Pg in. H2O -0.38 -0.38 -0.38 Average Stack Temperature, dry bulb Tsf degrees F 136 137 138 Actual Dry Gas Meter Volume Vm cubic feet 32.58 33.36 33.62 Dry Gas Meter Calibration Factor Y - 1.0046 1.0046 1.0046 Average Orifice Meter Pressure Drop DH in H2O 0.94 0.94 0.95 Average Meter Temperature Tmf degrees F 62 76 86 Pitot Tube Coefficient Cp - 0.840 0.840 0.840 Average Square Root of Velocity Head (DP)^0.5 - 0.946 0.933 0.932 Volume of Water Vapor Condensed in Impingers Vwc ml 88 92 91 Mass of Water Vapor Collected in Desiccant Vwsg g 5 6 10 Orsat Results, Dry Basis Carbon Dioxide %CO2 %v/v 1.0 1.0 1.0 Oxygen %O2 %v/v 18.7 18.6 18.6 Carbon Monoxide + Nitrogen - %v/v 80.3 80.4 80.4 Nozzle Diameter Dn in 0.193 0.193 0.193 Run Time theta min 60 60 60 Method 8 Lab Results SO3/SO4 M-SO3/SO4 ug 3,600 2,870 3,270 SO2 M-SO2 ug 15,800 15,400 20,000

Calculated Data Symbol Units Run 1 Run 2 Run 3 Average Absolute Stack Temperature (R) Tsr degrees R 596 597 598 Tsr = Tsf + 460 Stack Pressure Ps in Hg 28.49 28.49 28.49 Ps = Pbar + Pg / 13.6 Duct Area A Sq. ft 117.859 117.859 117.859 A = L x W/144 Meter Volume at Standard Conditions Vmstd cubic feet 31.65 31.52 31.22 Vmstd = 17.64 x Vm x Y x ((Pbar +(DH/13.6))/Tmr) Average Moisture Content of Stack Gas MC % Vol 12.10 12.65 13.10 MC = ((.04707 x Vwc+.04715*Vwsg)/((.04707 x Vwc+.04 715*Vwsg) + (Vmstd)) x 100 Molecular Weight of Stack Gas, dry Md lb/lbmol 28.91 28.90 28.90 Md = (0.44x(%CO2))+(0.32x(%O2))+(0.28x(%N2+%CO)) Molecular Weight of Stack Gas, wet Ms lb/lbmol 27.59 27.52 27.48 Ms = Md x (1-(MC/100))+18 x (MC/100) Average Stack Gas Velocity Vs ft/sec 59.19 58.47 58.50 Vs = 85.49 x Cp x (dP)^0.5 x ((Tsr/(Ps x Ms))^0.5) Actual Volumetric Flowrate Qa acfm 418,547 413,451 413,658 Qa = 60 x Vs x A Volumetric Flowrate at Standard Conditions Qs scfm 352,850 348,311 348,048 Qs = Qa x (528/(Ts+460)) x (Ps/29.92) Dry Volumetric Flowrate at Standard Conditions Qd dscfm 310,172 304,237 302,442 Qd = Qa x (1-(MC/100)) x (528/Tsr) x (Ps/29.92) Nozzle Cross-Sectional Area An sq. ft 0.000203 0.000203 0.000203 An =( 3.14 x Dn^2) /(4 x 144) Isokinetic Variation I % 98.7 100.2 99.9 I = (0.0945xTsrxVm)/(PsxVsxAn x theta x(1-(MC/100)) ) Method 8 Concentrations SO3/SO4 lb/dscf = M-SO3/SO4 x 2.20462^-9/Vmstd Cs(SO 3/SO4) lb/dscf 2.5E-07 2.0E-07 2.3E-07 SO2 lb/dscf = M-SO2 x 2.20462^-9/Vmstd Cs(SO2) lb/dscf 1.1E-06 1.1E-06 1.4E-06 SO3/SO4 emission Rate SO3/SO4 Edry = Cs(SO3/SO4) x Qd x 60 SO3/SO4 Edry lb/hr 4.7 3.7 4.2 SO2 Emission Rate Dry Catch+Organic Wet Catch SO2 Edry = Cs(SO2) x Qd x 60 SO2 Edry lb/hr 20.5 19.7 25.6 Sulfuric Acid Mist percent of Total SO2 emissions

Fraction sulfuric acid mist= (SO3/SO4 Edry)/(SO2 Ed ry) x 100 Fraction H2SO4 % 22.8 18.6 16.4Cliffs Natural Resources Barr Engineering Co. United Taconite LLC April 27, 2011 Forbes, MN

Determination of Volumetric Airflow Rate, Gas Compo sition, Moisture Content, and sulfuric acid mist EPA Methods 2, 3, 4, 8 TEST 2 2B WGS (SV049) Input Data Symbol Units Run 1 Run 2 Run 3
Test Date - - 4/12/2011 4/12/2011 4/12/2011 Test Period - - 856 - 1006 1148 - 1255 1405 - 1511 Number of Sample Ports - - 4 4 4 Number of Traverse Points - - 12 12 12 Duct Dimensions (diameter or Length x Width) D, L X W inches 146.25 146.25 146.25 Barometric Pressure Pbar in. Hg 28.52 28.52 28.52 Stack Static Pressure Pg in. H2O -0.56 -0.56 -0.56 Average Stack Temperature, dry bulb Tsf degrees F 129 135 137 Actual Dry Gas Meter Volume Vm cubic feet 34.45 34.10 33.61 Dry Gas Meter Calibration Factor Y - 1.0052 1.0052 1.0052 Average Orifice Meter Pressure Drop DH in H2O 1.11 1.07 1.02 Average Meter Temperature Tmf degrees F 63 67 74 Pitot Tube Coefficient Cp - 0.840 0.840 0.840 Average Square Root of Velocity Head (DP)^0.5 - 0.978 0.970 0.941 Volume of Water Vapor Condensed in Impingers Vwc ml 105 99 103 Mass of Water Vapor Collected in Desiccant Vwsg g 6 7 7 Orsat Results, Dry Basis Carbon Dioxide %CO2 %v/v 1.00 1.00 0.90 Oxygen %O2 %v/v 18.7 18.7 18.7 Carbon Monoxide + Nitrogen - %v/v 80.3 80.3 80.4 Nozzle Diameter Dn in 0.193 0.193 0.193 Run Time theta min 60 60 60 Method 8 Lab Results SO3/SO4 M-SO3/SO4 ug 4,310 3,530 4,450 SO2 M-SO2 ug 9,280 9,570 11,400

Calculated Data Symbol Units Run 1 Run 2 Run 3 Average Absolute Stack Temperature (R) Tsr degrees R 589 595 597 Tsr = Tsf + 460 Stack Pressure Ps in Hg 28.48 28.48 28.48 Ps = Pbar + Pg / 13.6 Duct Area A Sq. ft 116.659 116.659 116.659 A = L x W/144 Meter Volume at Standard Conditions Vmstd cubic feet 33.43 32.81 31.92 Vmstd = 17.64 x Vm x Y x ((Pbar +(DH/13.6))/Tmr) Average Moisture Content of Stack Gas MC % Vol 13.52 13.20 13.96 MC = ((.04707 x Vwc+.04715*Vwsg)/((.04707 x Vwc+.04 715*Vwsg) + (Vmstd)) x 100 Molecular Weight of Stack Gas, dry Md lb/lbmol 28.91 28.91 28.89 Md = (0.44x(%CO2))+(0.32x(%O2))+(0.28x(%N2+%CO)) Molecular Weight of Stack Gas, wet Ms lb/lbmol 27.43 27.47 27.37 Ms = Md x (1-(MC/100))+18 x (MC/100) Average Stack Gas Velocity Vs ft/sec 60.95 60.79 59.17 Vs = 85.49 x Cp x (dP)^0.5 x ((Tsr/(Ps x Ms))^0.5) Actual Volumetric Flowrate Qa acfm 426,657 425,498 414,177 Qa = 60 x Vs x A Volumetric Flowrate at Standard Conditions Qs scfm 364,305 359,146 348,517 Qs = Qa x (528/(Ts+460)) x (Ps/29.92) Dry Volumetric Flowrate at Standard Conditions Qd dscfm 315,057 311,735 299,865 Qd = Qa x (1-(MC/100)) x (528/Tsr) x (Ps/29.92) Nozzle Cross-Sectional Area An sq. ft 0.000203 0.000203 0.000203 An =( 3.14 x Dn^2) /(4 x 144) Isokinetic Variation I % 101.6 100.8 101.9 I = (0.0945xTsrxVm)/(PsxVsxAn x theta x(1-(MC/100)) ) Method 8 Concentrations SO3/SO4 lb/dscf = M-SO3/SO4 x 2.20462^-9/Vmstd Cs(SO 3/SO4) lb/dscf 2.8E-07 2.4E-07 3.1E-07 SO2 lb/dscf = M-SO2 x 2.20462^-9/Vmstd Cs(SO2) lb/dscf 6.1E-07 6.4E-07 7.9E-07 SO3/SO4 emission Rate SO3/SO4 Edry = Cs(SO3/SO4) x Qd x 60 SO3/SO4 Edry lb/hr 5.4 4.4 5.5 SO2 Emission Rate Dry Catch+Organic Wet Catch SO2 Edry = Cs(SO2) x Qd x 60 SO2 Edry lb/hr 11.6 12.0 14.2 Sulfuric Acid Mist percent of Total SO2 emissions

Fraction sulfuric acid mist= (SO3/SO4 Edry)/(SO2 Ed ry) x 100 Fraction H2SO4 % 46.4 36.9 39.0Cliffs Natural Resources Barr Engineering Co. United Taconite April 27, 2011 Forbes, Minnesota

Determination of Volumetric Airflow Rate, Gas Compo sition, Moisture Content, and sulfuric acid mist EPA Methods 2, 3, 4, 8 TEST 3 2A WGS (SV048) Input Data Symbol Units Run 1 Run 2 Run 3
Test Date - - 4/13/2011 4/13/2011 4/13/2011 Test Period - - 836 - 941 1034 - 1141 1240 - 1344 Number of Sample Ports - - 4 4 4 Number of Traverse Points - - 12 12 12 Duct Dimensions (diameter or Length x Width) D, L X W inches 147.00 147.00 147.00 Barometric Pressure Pbar in. Hg 28.60 28.60 28.60 Stack Static Pressure Pg in. H2O -0.38 -0.38 -0.38 Average Stack Temperature, dry bulb Tsf degrees F 135 135 135 Actual Dry Gas Meter Volume Vm cubic feet 33.88 34.37 33.36 Dry Gas Meter Calibration Factor Y - 1.0046 1.0046 1.0046 Average Orifice Meter Pressure Drop DH in H2O 0.99 1.00 0.99 Average Meter Temperature Tmf degrees F 82 84 85 Pitot Tube Coefficient Cp - 0.840 0.840 0.840 Average Square Root of Velocity Head (DP)^0.5 - 0.950 0.956 0.950 Volume of Water Vapor Condensed in Impingers Vwc ml 90 86 86 Mass of Water Vapor Collected in Desiccant Vwsg g 5 9 8 Orsat Results, Dry Basis Carbon Dioxide %CO2 %v/v 1.7 1.8 1.7 Oxygen %O2 %v/v 18.5 18.4 18.6 Carbon Monoxide + Nitrogen - %v/v 79.8 79.8 79.7 Nozzle Diameter Dn in 0.193 0.193 0.193 Run Time theta min 60 60 60 Method 8 Lab Results SO3/SO4 M-SO3/SO4 ug 7,390 7,260 6,310 SO2 M-SO2 ug 303,000 312,000 287,000

Calculated Data Symbol Units Run 1 Run 2 Run 3 Average Absolute Stack Temperature (R) Tsr degrees R 595 595 595 Tsr = Tsf + 460 Stack Pressure Ps in Hg 28.57 28.57 28.57 Ps = Pbar + Pg / 13.6 Duct Area A Sq. ft 117.859 117.859 117.859 A = L x W/144 Meter Volume at Standard Conditions Vmstd cubic feet 31.75 32.10 31.10 Vmstd = 17.64 x Vm x Y x ((Pbar +(DH/13.6))/Tmr) Average Moisture Content of Stack Gas MC % Vol 12.35 12.23 12.46 MC = ((.04707 x Vwc+.04715*Vwsg)/((.04707 x Vwc+.04 715*Vwsg) + (Vmstd)) x 100 Molecular Weight of Stack Gas, dry Md lb/lbmol 29.01 29.02 29.02 Md = (0.44x(%CO2))+(0.32x(%O2))+(0.28x(%N2+%CO)) Molecular Weight of Stack Gas, wet Ms lb/lbmol 27.65 27.68 27.64 Ms = Md x (1-(MC/100))+18 x (MC/100) Average Stack Gas Velocity Vs ft/sec 59.22 59.57 59.22 Vs = 85.49 x Cp x (dP)^0.5 x ((Tsr/(Ps x Ms))^0.5) Actual Volumetric Flowrate Qa acfm 418,809 421,229 418,794 Qa = 60 x Vs x A Volumetric Flowrate at Standard Conditions Qs scfm 354,856 356,856 354,744 Qs = Qa x (528/(Ts+460)) x (Ps/29.92) Dry Volumetric Flowrate at Standard Conditions Qd dscfm 311,042 313,216 310,555 Qd = Qa x (1-(MC/100)) x (528/Tsr) x (Ps/29.92) Nozzle Cross-Sectional Area An sq. ft 0.000203 0.000203 0.000203 An =( 3.14 x Dn^2) /(4 x 144) Isokinetic Variation I % 98.8 99.2 96.9 I = (0.0945xTsrxVm)/(PsxVsxAn x theta x(1-(MC/100)) ) Method 8 Concentrations SO3/SO4 lb/dscf = M-SO3/SO4 x 2.20462^-9/Vmstd Cs(SO 3/SO4) lb/dscf 5.1E-07 5.0E-07 4.5E-07 SO2 lb/dscf = M-SO2 x 2.20462^-9/Vmstd Cs(SO2) lb/dscf 2.1E-05 2.1E-05 2.0E-05 SO3/SO4 emission Rate SO3/SO4 Edry = Cs(SO3/SO4) x Qd x 60 SO3/SO4 Edry lb/hr 9.6 9.4 8.3 SO2 Emission Rate Dry Catch+Organic Wet Catch SO2 Edry = Cs(SO2) x Qd x 60 SO2 Edry lb/hr 392.7 402.7 379.1 Sulfuric Acid Mist percent of Total SO2 emissions

Fraction sulfuric acid mist= (SO3/SO4 Edry)/(SO2 Ed ry) x 100 Fraction H2SO4 % 2.4 2.3 2.2Cliffs Natural Resources Barr Engineering Co. United Taconite LLC April 27, 2011 Forbes, MN

Determination of Volumetric Airflow Rate, Gas Compo sition, Moisture Content, and sulfuric acid mist EPA Methods 2, 3, 4, 8 TEST 4 2B WGS (SV049) Input Data Symbol Units Run 1 Run 2 Run 3
Test Date - - 4/13/2011 4/13/2011 4/13/2011 Test Period - - 836 - 943 1034 - 1141 1240 - 1346 Number of Sample Ports - - 4 4 4 Number of Traverse Points - - 12 12 12 Duct Dimensions (diameter or Length x Width) D, L X W inches 146.25 146.25 146.25 Barometric Pressure Pbar in. Hg 28.60 28.60 28.60 Stack Static Pressure Pg in. H2O -0.55 -0.55 -0.55 Average Stack Temperature, dry bulb Tsf degrees F 126 124 125 Actual Dry Gas Meter Volume Vm cubic feet 33.67 33.87 33.90 Dry Gas Meter Calibration Factor Y - 1.0052 1.0052 1.0052 Average Orifice Meter Pressure Drop DH in H2O 1.07 1.08 1.10 Average Meter Temperature Tmf degrees F 58 61 61 Pitot Tube Coefficient Cp - 0.840 0.840 0.840 Average Square Root of Velocity Head (DP)^0.5 - 0.972 0.959 0.977 Volume of Water Vapor Condensed in Impingers Vwc ml 92 91 90 Mass of Water Vapor Collected in Desiccant Vwsg g 2 15 6 Orsat Results, Dry Basis Carbon Dioxide %CO2 %v/v 1.60 1.50 1.60 Oxygen %O2 %v/v 18.6 18.6 18.6 Carbon Monoxide + Nitrogen - %v/v 79.8 79.9 79.8 Nozzle Diameter Dn in 0.193 0.193 0.193 Run Time theta min 60 60 60 Method 8 Lab Results SO3/SO4 M-SO3/SO4 ug 9,630 10,400 8,940 SO2 M-SO2 ug 272,000 283,000 256,000

Calculated Data Symbol Units Run 1 Run 2 Run 3 Average Absolute Stack Temperature (R) Tsr degrees R 586 584 585 Tsr = Tsf + 460 Stack Pressure Ps in Hg 28.56 28.56 28.56 Ps = Pbar + Pg / 13.6 Duct Area A Sq. ft 116.659 116.659 116.659 A = L x W/144 Meter Volume at Standard Conditions Vmstd cubic feet 33.05 33.09 33.10 Vmstd = 17.64 x Vm x Y x ((Pbar +(DH/13.6))/Tmr) Average Moisture Content of Stack Gas MC % Vol 11.81 13.11 12.01 MC = ((.04707 x Vwc+.04715*Vwsg)/((.04707 x Vwc+.04 715*Vwsg) + (Vmstd)) x 100 Molecular Weight of Stack Gas, dry Md lb/lbmol 29.00 28.98 29.00 Md = (0.44x(%CO2))+(0.32x(%O2))+(0.28x(%N2+%CO)) Molecular Weight of Stack Gas, wet Ms lb/lbmol 27.70 27.54 27.68 Ms = Md x (1-(MC/100))+18 x (MC/100) Average Stack Gas Velocity Vs ft/sec 60.06 59.33 60.36 Vs = 85.49 x Cp x (dP)^0.5 x ((Tsr/(Ps x Ms))^0.5) Actual Volumetric Flowrate Qa acfm 420,413 415,301 422,479 Qa = 60 x Vs x A Volumetric Flowrate at Standard Conditions Qs scfm 361,835 358,149 364,132 Qs = Qa x (528/(Ts+460)) x (Ps/29.92) Dry Volumetric Flowrate at Standard Conditions Qd dscfm 319,117 311,211 320,390 Qd = Qa x (1-(MC/100)) x (528/Tsr) x (Ps/29.92) Nozzle Cross-Sectional Area An sq. ft 0.000203 0.000203 0.000203 An =( 3.14 x Dn^2) /(4 x 144) Isokinetic Variation I % 99.2 101.8 99.0 I = (0.0945xTsrxVm)/(PsxVsxAn x theta x(1-(MC/100)) ) Method 8 Concentrations SO3/SO4 lb/dscf = M-SO3/SO4 x 2.20462^-9/Vmstd Cs(SO 3/SO4) lb/dscf 6.4E-07 6.9E-07 6.0E-07 SO2 lb/dscf = M-SO2 x 2.20462^-9/Vmstd Cs(SO2) lb/dscf 1.8E-05 1.9E-05 1.7E-05 SO3/SO4 emission Rate SO3/SO4 Edry = Cs(SO3/SO4) x Qd x 60 SO3/SO4 Edry lb/hr 12.3 12.9 11.4 SO2 Emission Rate Dry Catch+Organic Wet Catch SO2 Edry = Cs(SO2) x Qd x 60 SO2 Edry lb/hr 347.4 352.1 327.8 Sulfuric Acid Mist percent of Total SO2 emissions

Fraction sulfuric acid mist= (SO3/SO4 Edry)/(SO2 Ed ry) x 100 Fraction H2SO4 % 3.5 3.7 3.5

# Appendix B

Field Data SheetsBarrEPA METHOD 8 - FIELD DATA SHEET - RUN 1Engineering CompanyProject Cliffs Natural Resources Train C-1, , P-6 Pitot TubeNo. 5-2Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV048 2A Waste Gas Stack Meter Y 1.0046Bar.Press. 28.52 in. Hg Pretest 0.000 at 15 in. HgDate 04/12/11 Test 1 Run # 1 Orifice H@1.794 Stat Press. -0.38 in. H2O Posttest 0.000 at 10 in.HgOperators DJK/RMP Probe Length 5 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °°F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 0858 636.941 5.0 639.73 0.980 1.01 2.85 639.79 * 136 * * * 58 58 18.52 10.0 642.62 1.000 1.05 2.92 642.72 * 136 * * * 58 573 15.0 645.25 0.810 0.85 2.63 645.35 * 136 * * * 59 584 20.0 648.02 0.920 0.97 2.81 648.16 * 135 * * * 59 585 25.0 650.73 0.880 0.92 2.74 650.90 * 137 * * * 61 586 30.0 653.19 0.690 0.72 2.43 653.33 * 137 * * * 62 597 35.0 655.88 0.950 1.00 2.86 656.19 * 136 * * * 63 608 40.0 658.53 0.950 1.00 2.86 659.06 * 138 * * * 65 619 45.0 661.19 0.820 0.87 2.67 661.73 * 135 * * * 66 6210 50.0 663.94 0.970 1.03 2.91 664.64 * 137 * * * 67 6311 55.0 666.80 0.940 1.00 2.87 667.51 * 137 * * * 68 6412 60.0 669.52 0.860 0.91 2.75 670.26 * 137 * * * 69 65End Time 1004Run Time 60 Avg DH= 0.94Avg Ts= 136.42Avg Tm= 61.58Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. - Final wt., g 124 140 114 1057 1067.5Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1047 1063Difference 24 40 14 10 4.5 92.5BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 2Engineering CompanyProject Cliffs Natural Resources Train C-1, 0, P-6 Pitot Tube No. 5-2Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV048 2A Waste Gas Stack Meter Y 1.0046Bar.Press. 28.52 in. Hg Pretest 0.000 at 15 in. HgDate 04/12/11 Test 1 Run # 2 Orifice H@1.794 Stat Press. -0.38 in. H2O Posttest 0.000 at 10 in.HgOperators DJK/RMP Probe Length 5 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1148 678.191 5.0 681.02 0.970 1.04 2.95 681.14 * 137 * * * 73 73 18.32 10.0 684.00 0.940 1.01 2.91 684.05 * 137 * * * 74 733 15.0 686.84 0.870 0.94 2.80 686.86 * 137 * * * 75 734 20.0 689.65 0.910 0.98 2.87 689.73 * 137 * * * 75 735 25.0 692.33 0.880 0.95 2.82 692.55 * 137 * * * 77 746 30.0 694.94 0.770 0.83 2.65 695.20 * 137 * * * 78 757 35.0 697.72 0.870 0.94 2.82 698.02 * 137 * * * 78 758 40.0 700.51 0.850 0.92 2.79 700.80 * 137 * * * 79 759 45.0 703.04 0.720 0.78 2.57 703.37 * 137 * * * 79 7610 50.0 705.88 0.920 1.00 2.91 706.28 * 136 * * * 80 7711 55.0 708.80 0.950 1.03 2.96 709.24 * 137 * * * 81 7712 60.0 711.55 0.820 0.89 2.75 711.99 * 136 * * * 81 78End Time 1253Run Time 60 Avg DH= 0.94Avg Ts= 136.83Avg Tm= 76.21Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. - Final wt., g 124 140 118 1067 1073Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1057 1067.5Difference 24 40 18 10 5.5 97.5BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 3Engineering CompanyProject Cliffs Natural Resources Train C-1, 0, P-6 Pitot Tube No. 5-2Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV048 2A Waste Gas Stack Meter Y 1.0046Bar.Press. 28.52 in. Hg Pretest 0.000 at 15 in. HgDate 04/12/11 Test 1 Run # 3 Orifice H@1.794 Stat Press. -0.38 in. H2O Posttest 0.000 at 10 in.HgOperators DJK/RMP Probe Length 5 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1405 720.171 5.0 723.07 0.960 1.03 2.96 723.13 * 138 * * * 81 81 18.32 10.0 725.80 0.960 1.03 2.97 726.10 * 138 * * * 83 823 15.0 728.48 0.840 0.91 2.79 728.88 * 137 * * * 84 824 20.0 731.31 0.880 0.95 2.85 731.74 * 137 * * * 85 835 25.0 734.15 0.840 0.91 2.79 734.53 * 138 * * * 86 836 30.0 736.75 0.730 0.79 2.60 737.13 * 138 * * * 87 847 35.0 739.61 0.910 0.99 2.92 740.05 * 136 * * * 88 858 40.0 742.50 0.880 0.96 2.87 742.92 * 138 * * * 89 869 45.0 745.18 0.770 0.84 2.69 745.61 * 138 * * * 89 8610 50.0 748.10 0.910 0.99 2.93 748.53 * 137 * * * 89 8611 55.0 751.02 0.970 1.06 3.02 751.55 * 138 * * * 90 8712 60.0 753.79 0.800 0.87 2.75 754.30 * 138 * * * 91 87End Time 1509Run Time 60 Avg DH= 0.94Avg Ts= 137.58Avg Tm= 85.58Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. - Final wt., g 126 138 120 1073 1017.5Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1067 1008Difference 26 38 20 6 9.5 99.5BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 1Engineering CompanyProject Cliffs Natural Resources Train C-5, S-2, P-4 Pitot Tube No. 4063-6 Cp 0.840 Sample Train Leak Rate,cfm:Sample Location SV049 2B Waste Gas Stack Meter Y 1.0052Bar.Press. 28.52 in. Hg Pretest 0.000 at 15 in. HgDate 04/12/11 Test 2 Run # 1 Orifice H@1.9533 Stat Press. -0.56 in. H2O Posttest 0.000 at 6 in.HgOperators TAK, MJN Probe Length 4 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °°F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 0856 729.801 5.0 732.82 1.100 1.25 3.06 732.86 * 126 * * * 60 58 18.72 10.0 735.82 1.050 1.21 3.02 735.88 * 125 * * * 61 593 15.0 738.56 0.870 1.00 2.75 738.62 * 126 * * * 62 594 20.0 741.82 1.250 1.44 3.30 741.92 * 126 * * * 63 605 25.0 745.16 1.250 1.43 3.29 745.21 * 130 * * * 64 616 30.0 747.97 1.000 1.15 2.95 748.16 * 129 * * * 65 617 35.0 750.88 0.970 1.12 2.91 751.07 * 130 * * * 65 628 40.0 753.69 0.990 1.14 2.94 754.01 * 130 * * * 66 639 45.0 756.40 0.850 0.97 2.72 756.73 * 136 * * * 66 6310 50.0 759.16 0.750 0.87 2.57 759.30 * 126 * * * 65 6311 55.0 761.75 0.800 0.92 2.64 761.94 * 132 * * * 66 6312 60.0 764.25 0.690 0.80 2.47 764.41 * 127 * * * 66 63End Time 1006Run Time 60 Avg DH= 1.11Avg Ts= 128.58Avg Tm= 62.67Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF 3" Impinger1 2 3 4 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 132 143 118 1433 1067Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1421 1061Difference 32 43 18 12 6 111BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 2Engineering CompanyProject Cliffs Natural Resources Train C-5, S-2, P-4 Pitot Tube No. 4063-6 Cp 0.840 Sample Train Leak Rate,cfm:Sample Location SV049 2B Waste Gas Stack Meter Y 1.0052Bar.Press. 28.52 in. Hg Pretest 0.000 at 15 in. HgDate 04/12/11 Test 2 Run # 2 Orifice H@1.9533 Stat Press. -0.56 in. H2O Posttest 0.000 at 5 in.HgOperators TAK, MJN Probe Length 4 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1148 775.401 5.0 778.30 0.990 1.13 2.93 778.33 * 126 * * * 65 66 18.92 10.0 781.30 1.100 1.24 3.07 781.40 * 135 * * * 65 653 15.0 784.20 0.900 1.01 2.78 784.17 * 135 * * * 65 654 20.0 787.40 1.250 1.41 3.27 787.44 * 135 * * * 66 655 25.0 790.58 1.200 1.34 3.20 790.64 * 139 * * * 67 656 30.0 793.48 0.970 1.09 2.88 793.52 * 138 * * * 68 667 35.0 796.30 0.940 1.08 2.87 796.39 * 126 * * * 68 668 40.0 799.10 0.990 1.11 2.91 799.30 * 139 * * * 69 679 45.0 801.80 0.820 0.92 2.66 801.96 * 139 * * * 70 6710 50.0 804.50 0.820 0.93 2.66 804.62 * 136 * * * 70 6711 55.0 807.20 0.780 0.88 2.59 807.21 * 139 * * * 70 6812 60.0 809.50 0.630 0.71 2.33 809.55 * 138 * * * 71 68End Time 1255Run Time 60 Avg DH= 1.07Avg Ts= 135.42Avg Tm= 67.04Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 130 141 118 1443 1074Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1433 1067Difference 30 41 18 10 7 106BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 3Engineering CompanyProject Cliffs Natural Resources Train C-5, S-2, P-4 Pitot Tube No. 4063-6 Cp 0.840 Sample Train Leak Rate,cfm:Sample Location SV049 2B Waste Gas Stack Meter Y 1.0052Bar.Press. 28.52 in. Hg Pretest 0.000 at 15 in. HgDate 04/12/11 Test 2 Run # 3 Orifice H@1.9533 Stat Press. -0.56 in. H2O Posttest 0.000 at 5 in.HgOperators TAK, MJN Probe Length 4 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1405 818.601 5.0 821.50 0.960 1.09 2.90 821.50 * 138 * * * 71 71 18.92 10.0 824.45 0.980 1.12 2.93 824.43 * 138 * * * 72 713 15.0 827.12 0.850 0.97 2.74 827.17 * 136 * * * 73 714 20.0 830.30 1.100 1.27 3.13 830.29 * 132 * * * 74 725 25.0 833.20 1.100 1.26 3.11 833.41 * 139 * * * 75 726 30.0 836.10 0.950 1.08 2.90 836.30 * 139 * * * 75 727 35.0 839.05 0.880 1.01 2.79 839.10 * 137 * * * 76 738 40.0 841.90 0.900 1.03 2.82 841.92 * 140 * * * 76 739 45.0 844.66 0.850 0.97 2.74 844.66 * 140 * * * 77 7410 50.0 847.29 0.734 0.85 2.56 847.22 * 136 * * * 77 7411 55.0 849.80 0.730 0.84 2.55 849.77 * 139 * * * 78 7512 60.0 852.21 0.660 0.77 2.44 852.21 * 133 * * * 78 75End Time 1511Run Time 60 Avg DH= 1.02Avg Ts= 137.25Avg Tm= 73.96Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 129 148 118 1451 1081Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1443 1074Difference 29 48 18 8 7 110BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 1Engineering CompanyProject Cliffs Natural Resources Train C-1, , P-6 Pitot TubeNo. 5-2Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV048 2A Waste Gas Stack Meter Y 1.0046Bar.Press. 28.60 in. Hg Pretest 0.000 at 10 in. HgDate 04/13/11 Test 3 Run # 1 Orifice H@1.794 Stat Press. -0.38 in. H2O Posttest 0.000 at 15 in.HgOperators DJK/RMP Probe Length 5 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °°F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 0836 765.001 5.0 767.90 0.970 1.05 2.97 767.97 * 135 * * * 80 78 18.52 10.0 770.76 1.000 1.09 3.04 771.01 * 136 * * * 80 783 15.0 773.46 0.790 0.86 2.70 773.71 * 134 * * * 82 794 20.0 776.28 0.920 1.01 2.92 776.64 * 135 * * * 82 795 25.0 779.05 0.930 1.02 2.94 779.58 * 135 * * * 83 806 30.0 781.65 0.820 0.90 2.77 782.35 * 132 * * * 84 817 35.0 784.35 0.920 1.01 2.93 785.28 * 136 * * * 84 818 40.0 787.15 0.910 1.00 2.92 788.20 * 136 * * * 85 829 45.0 789.80 0.740 0.81 2.64 790.84 * 135 * * * 86 8310 50.0 792.57 1.000 1.10 3.07 793.91 * 136 * * * 81 8311 55.0 796.03 1.000 1.10 3.05 796.96 * 136 * * * 87 8412 60.0 798.88 0.860 0.95 2.85 799.81 * 135 * * * 88 84End Time 0941Run Time 60 Avg DH= 0.99Avg Ts= 135.08Avg Tm= 82.25Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 122 134 122 1024 1011Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1012 1006Difference 22 34 22 12 5 95BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 2Engineering CompanyProject Cliffs Natural Resources Train C-1, 0, P-6 Pitot Tube No. 5-2Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV048 2A Waste Gas Stack Meter Y 1.0046Bar.Press. 28.60 in. Hg Pretest 0.000 at 10 in. HgDate 04/13/11 Test 3 Run # 2 Orifice H@1.794 Stat Press. -0.38 in. H2O Posttest 0.000 at 12 in.HgOperators DJK/RMP Probe Length 5 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1034 805.841 5.0 808.85 0.970 1.06 3.01 808.85 * 133 * * * 83 83 18.32 10.0 811.82 1.000 1.09 3.05 811.91 * 135 * * * 83 823 15.0 814.64 0.840 0.92 2.80 814.70 * 134 * * * 83 834 20.0 817.47 0.910 0.99 2.91 817.61 * 136 * * * 84 835 25.0 820.25 0.890 0.97 2.88 820.49 * 136 * * * 84 836 30.0 822.88 0.720 0.79 2.59 823.09 * 135 * * * 85 837 35.0 825.77 0.970 1.06 3.01 826.10 * 136 * * * 86 838 40.0 828.61 1.000 1.09 3.06 829.16 * 136 * * * 86 839 45.0 831.33 0.820 0.90 2.77 831.93 * 135 * * * 86 8410 50.0 834.39 1.050 1.15 3.14 835.07 * 135 * * * 86 8411 55.0 837.31 1.000 1.09 3.06 838.13 * 136 * * * 86 8412 60.0 840.21 0.830 0.91 2.79 840.92 * 135 * * * 87 84End Time 1141Run Time 60 Avg DH= 1.00Avg Ts= 135.17Avg Tm= 84.08Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 122 139 116 1033 1073Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1024 1064Difference 22 39 16 9 9 95BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 3Engineering CompanyProject Cliffs Natural Resources Train C-1, 0, P-6 Pitot Tube No. 5-2Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV048 2A Waste Gas Stack Meter Y 1.0046Bar.Press. 28.60 in. Hg Pretest 0.000 at 10 in. HgDate 04/13/11 Test 3 Run # 3 Orifice H@1.794 Stat Press. -0.38 in. H2O Posttest 0.000 at 9 in. HgOperators DJK/RMP Probe Length 5 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1240 848.861 5.0 851.82 0.970 1.07 3.04 851.90 * 134 * * * 82 82 18.32 10.0 854.79 1.000 1.09 3.05 854.95 * 136 * * * 83 833 15.0 857.60 0.870 0.96 2.86 857.81 * 132 * * * 83 824 20.0 860.48 0.960 1.05 2.99 860.80 * 135 * * * 84 835 25.0 863.38 0.910 1.00 2.92 863.71 * 136 * * * 85 836 30.0 866.01 0.770 0.84 2.69 866.40 * 135 * * * 86 837 35.0 868.85 0.940 1.03 2.97 869.37 * 136 * * * 86 848 40.0 871.37 0.870 0.95 2.86 872.23 * 136 * * * 81 849 45.0 873.73 0.780 0.85 2.69 874.92 * 136 * * * 88 8510 50.0 876.57 0.970 1.07 3.03 877.95 * 135 * * * 90 8711 55.0 879.43 0.990 1.09 3.07 881.02 * 136 * * * 90 8712 60.0 882.22 0.820 0.91 2.79 883.82 * 136 * * * 92 88End Time 1344Run Time 60 Avg DH= 0.99Avg Ts= 135.25Avg Tm= 85.04Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 122 140 118 1039 1081Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1033 1073Difference 22 40 18 6 8 94BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 1Engineering CompanyProject Cliffs Natural Resources Train C-5, S-2, P-4 Pitot Tube No. 4-3Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV049 2B Waste Gas Stack Meter Y 1.0052Bar.Press. 28.60 in. Hg Pretest 0.000 at 15 in. HgDate 04/13/11 Test 4 Run # 1 Orifice H@1.9533 Stat Press. -0.55 in. H2O Posttest 0.000 at 6 in.HgOperators TAK, MJN Probe Length 4 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °°F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 0836 861.801 5.0 864.80 1.050 1.19 2.97 864.77 * 124 * * * 56 55 18.72 10.0 867.70 1.100 1.24 3.04 867.81 * 124 * * * 56 563 15.0 870.40 0.920 1.04 2.79 870.60 * 124 * * * 57 564 20.0 873.35 1.200 1.36 3.18 873.78 * 124 * * * 58 565 25.0 876.20 1.100 1.25 3.05 876.84 * 124 * * * 59 566 30.0 879.40 1.000 1.13 2.91 879.75 * 125 * * * 60 567 35.0 882.10 0.880 1.00 2.73 882.48 * 125 * * * 60 578 40.0 881.90 0.950 1.07 2.83 885.31 * 129 * * * 61 579 45.0 887.60 0.870 0.98 2.71 888.02 * 132 * * * 61 5810 50.0 890.44 0.780 0.88 2.58 890.60 * 127 * * * 61 5811 55.0 892.90 0.800 0.91 2.62 893.21 * 124 * * * 61 5812 60.0 895.47 0.750 0.85 2.53 895.74 * 125 * * * 61 58End Time 0943Run Time 60 Avg DH= 1.07Avg Ts= 125.58Avg Tm= 58.00Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF 3" Impinger1 2 3 4 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 132 135 115 1398 1031Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1388 1029Difference 32 35 15 10 2 94BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 2Engineering CompanyProject Cliffs Natural Resources Train C-5, S-2, P-4 Pitot Tube No. 4-3Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV049 2B Waste Gas Stack Meter Y 1.0052Bar.Press. 28.60 in. Hg Pretest 0.000 at 15 in. HgDate 04/13/11 Test 4 Run # 2 Orifice H@1.9533 Stat Press. -0.55 in. H2O Posttest 0.000 at 7 in.HgOperators TAK, MJN Probe Length 4 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1034 905.131 5.0 908.10 1.050 1.23 3.04 908.17 * 124 * * * 60 59 18.92 10.0 911.05 1.000 1.17 2.97 911.14 * 124 * * * 60 593 15.0 913.77 0.870 1.02 2.77 913.90 * 124 * * * 61 604 20.0 916.70 1.100 1.29 3.12 917.02 * 124 * * * 61 595 25.0 919.60 1.050 1.23 3.04 920.06 * 124 * * * 61 606 30.0 922.50 0.950 1.11 2.90 922.96 * 124 * * * 62 607 35.0 925.31 0.850 1.00 2.74 925.70 * 124 * * * 62 608 40.0 928.30 1.000 1.17 2.97 928.67 * 124 * * * 62 609 45.0 931.10 0.900 1.05 2.82 931.49 * 126 * * * 62 6010 50.0 933.80 0.760 0.89 2.59 934.08 * 125 * * * 61 6011 55.0 936.40 0.780 0.91 2.62 936.70 * 125 * * * 62 6012 60.0 939.00 0.760 0.89 2.59 939.29 * 125 * * * 62 60End Time 1141Run Time 60 Avg DH= 1.08Avg Ts= 124.42Avg Tm= 60.54Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 136 127 118 1408 1046Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1398 1031Difference 36 27 18 10 15 106BarrEPA METHOD 8 - FIELD DATA SHEET - RUN 3Engineering CompanyProject Cliffs Natural Resources Train C-5, S-2, P-4 Pitot Tube No. 4-3Cp 0.840 Sample Train Leak Rate, cfm:Sample Location SV049 2B Waste Gas Stack Meter Y 1.0052Bar.Press. 28.60 in. Hg Pretest 0.000 at 15 in. HgDate 04/13/11 Test 4 Run # 3 Orifice H@1.9533 Stat Press. -0.55 in. H2O Posttest 0.000 at 6 in.HgOperators TAK, MJN Probe Length 4 ft.Probe Liner Type: Glass OtherSampleIdeal SampleOxygenSample Time Actual Velocity Orifice Point Ideal Train Stack Sample Train Temperatures, °F Content,Point DT Meter Vol Head DP, DH Volume Meter Vol Vacuum Temp Filter Probe Impinger Meter Meter %Vm, ft3in. H2O in. H2OVm, ft3Vm, ft3 in. Hg Ts,°FOutlet Inlet OutletStart Time 1240 950.401 5.0 953.50 1.150 1.32 3.14 953.54 * 124 * * * 59 59 18.92 10.0 956.70 1.100 1.25 3.07 956.61 * 125 * * * 60 593 15.0 959.35 0.870 0.99 2.73 959.34 * 124 * * * 61 594 20.0 962.58 1.200 1.37 3.21 962.56 * 124 * * * 61 595 25.0 965.70 1.200 1.37 3.21 965.77 * 124 * * * 61 606 30.0 968.30 0.950 1.09 2.86 968.63 * 124 * * * 62 607 35.0 971.10 0.930 1.07 2.83 971.46 * 124 * * * 62 608 40.0 973.80 0.970 1.10 2.88 974.34 * 129 * * * 62 609 45.0 976.56 0.880 1.01 2.75 977.09 * 126 * * * 63 6110 50.0 979.20 0.750 0.86 2.55 979.64 * 124 * * * 63 6111 55.0 981.83 0.820 0.94 2.67 982.31 * 124 * * * 63 6112 60.0 984.30 0.720 0.83 2.50 984.80 * 125 * * * 63 61End Time 1346Run Time 60 Avg DH= 1.10Avg Ts= 124.75Avg Tm= 60.83Integrated Gas Sampling Data :MOISTURE RECOVERY DATA :Box No. NA Leak Rate NA cc/min Filter No. GFF Impinger 1 2 34 Desiccant TotalBag No. NAO2ReadingNA % Nozzle No. Glass Final wt., g 134 144 108 1412 1052Bag Vol. NAO2Analyzer No.NA Nozzle Dn. 0.193 Initial wt., g 100 100 100 1408 1046Difference 34 44 8 4 6 96

# Appendix C

Laboratory Reports and Sample Chain of Custody

# Barr Engineering Company

7390 Ohms Lane Edina, MN 55439-2330



# Client # 23/69-1092

Analytical Report (0411-91)

EPA Method 8 (Titrations)

Sulfuric acid mist/Sulfur trioxide Sulfur dioxide



# Enthalpy Analytical, Inc.
Phone: (919) 850 - 4392 / Fax: (919) 850 - 9012 / www.enthalpy.com 2202 Ellis Road Durham, NC 27703 - 551

## Compound Sample ID / Catch Weight (mg)

2A WGS SV048 on 4/12/11 **T1 R1 T1 R2**  **T1 R3** Sulfuric acid mist/Sulfur Trioxide 3.60 2.87 3.27 Sulfur Dioxide 15.8 15.4 20.0

2B WGS SV049 on 4/12/11 **T2 R1 T2 R2**  **T2 R3** Sulfuric acid mist/Sulfur Trioxide 4.31 3.53 4.45 Sulfur Dioxide 9.28 9.57 11.4

2A WGS SV048 on 4/13/11 **T3 R1 T3 R2**  **T3 R3** Sulfuric acid mist/Sulfur Trioxide 7.39 7.26 6.31 Sulfur Dioxide 303 312 287

2B WGS SV049 on 4/13/11 **T4 R1 T4 R2**  **T4 R3** Sulfuric acid mist/Sulfur Trioxide 9.63 10.4 8.94 Sulfur Dioxide 272 283 256

**T2 R0 Blank IPA**  **H2O2** Sulfuric acid mist/Sulfur Trioxide 0.0307 ND Sulfur Dioxide 0.0951 Company

Analyst Parameters Barr Engineering Co. EO EPA Method 8 Client # Job # # Samples 23/69-1092 0411-91 12 Runs, 1 Blank

0411-91 res 4/20/2011

# Summary of Results

# Results

# Narrative Summary

# Enthalpy Analytical Narrative Summary

Company Barr Engineering Company Client # 23/69-1092 Analyst EO Job # 0411-91 Parameters EPA Method 8 # Samples 12 Runs, 1 Blank

Custody Bryan Tyler received the samples on 4/15/11 after being relinquished by Barr Engineering Company. The samples were received at 18.9 C in good condition. Prior to, during, and after analysis, the samples were kept under lock with access only to authorized personnel by Enthalpy Analytical, Inc.
Analysis The samples were analyzed for sulfuric acid mist (including sulfur trioxide) and sulfur dioxide using the analytical procedures in EPA Method 8, Determination of Sulfuric Acid and Sulfur Dioxide Emissions from Stationary Sources (40 CFR Part 60, Appendix A).
The samples were titrated using a barium chloride solution prepared in the lab. The normality was determined according to the procedures described in the method. The samples were titrated to a pink endpoint using a thorin indicator.
QC Notes Replicate titrations were performed with the titrant volumes meeting the QC criteria of within 1% or 0.02 mL, whichever is greater.
Reagent blanks were received and analyzed with these samples.

Calculations Sulfuric acid mist (H 2 

## SO 4 

## ) calculations

C H2SO4 

## = (N)(V t 

## -V b 

## )(V sol 

## /V a 

## )(49.04)

Where:

C H2SO4 

### Catch weight as sulfuric acid (mg) N Normality of the barium chloride titrant
V t 

### Volume of the titrant used to achieve pink endpoint
V b 

### Titrant volume to achieve pink endpoint w/Lab IPA
V sol 

### Volume of the entire sample solution
V a 

### Volume of the aliquot taken for the titration 49.04 Equivalent weight for sulfuric acid

# Enthalpy Analytical Narrative Summary (continued)

Calculations (continued) Sulfur dioxide (SO 2 

## ) calculations

C SO2 

## = (N)(V t 

## -V b 

## )(V sol 

## /V a 

## )(32.03)
Where:

C SO2 

### Catch weight as sulfur dioxide (mg) N Normality of the barium chloride titrant
V t 

### Volume of the titrant used to achieve pink endpoint
V b 

### Titrant volume to achieve pink endpoint w/Lab IPA
V sol 

### Volume of the entire sample solution
V a 

### Volume of the aliquot taken for the titration 32.03 Equivalent weight for sulfur dioxide. 

## Reporting Notes Samples are analyzed using a micro-burette to conserve sample and reduce waste. The burette is 1/10 the volume of that specified in EPA Method 6. Results are reported in milligrams (mg) catch.
These analyses met the requirements of the NELAC Standard. Any deviations from the requirements of the reference method or NELAC Standard have been previously noted in the report narrative. The results presented in this report are representative of the samples as provided to the laboratory.
Enthalpy Analytical, Inc. is nationally accredited to perform EPA Method 8 for compliance purposes by the Louisiana Department of Environmental Quality’s Louisiana Environmental Laboratory Accreditation Program (LELAP), certificate number 04010.

# General Reporting Notes

The following are general reporting notes that are applicable to all Enthalpy Analytical, Inc. data reports, unless specifically noted otherwise.

The acronym MDL represents the Minimum Detection Limit. Below this value the laboratory cannot determine the presence of the analyte of interest reliably. The acronym LOQ represents the Limit of Quantification. Below this value the laboratory cannot quantitate the analyte of interest within the criteria of the method. The acronym ND following a value indicates a non-detect or analytical result below the MDL.
The letter J following a value indicates an analytical result between the MDL and the LOQ. A J flag indicates that the laboratory can positively identify the analyte of interest as present, but the value should be considered an estimate.
The letter E following a value indicates an analytical result exceeding 100% of the highest calibration point. The associated value should be considered as an estimate. The acronym DF represents Dilution Factor. This number represents dilution of the sample during the preparation and/or analysis process. The analytical result taken from a laboratory instrument is multiplied by the DF to determine the final undiluted sample results.
The addition of MS to the Sample ID represents a Matrix Spike. An aliquot of an actual sample is spiked with a known amount of analyte so that a percent recovery value can be determined. This shows what effect the sample matrix may have on the target analyte, i.e. whether or not anything in the sample matrix interferes with the analysis of the analyte(s).
The addition of MSD to the Sample ID represents a Matrix Spike Duplicate. Prepared in the same manner as an MS, the use of duplicate matrix spikes allows further confirmation of laboratory quality by showing the consistency of results gained by performing the same steps multiple times.
The addition of LD to the Sample ID represents a Laboratory Duplicate. The analyst prepares an additional aliquot of sample for testing and the results of the duplicate analysis are compared to the initial result. The result should have a difference value of within 10% of the initial result (if the results of the original analysis are greater than the LOQ).
The addition of AD to the Sample ID represents an Alternate Dilution. The analyst prepares an additional aliquot at a different dilution factor (usually double the initial factor). This analysis helps confirm that no additional compound is present and coeluting or sharing absorbance with the analyte of interest, as they would have a different response/absorbance than the analyte of interest. The Sample ID LCS represents a Laboratory Control Sample. Clean matrix, similar to the client sample matrix, prepared and analyzed by the laboratory using the same reagents, spiking standards and procedures used for the client samples. The LCS is used to assess the control of the laboratory’s analytical system. Whenever spikes are prepared for our client projects, two extra spikes are prepared. The extras (randomly chosen) are labeled with the associated project number and kept in-house at the appropriate temperature conditions. When the project samples are received for analysis, the LCSs are analyzed to confirm that the analyte could be recovered from the media, separate from the samples which were used on the project and which may have been affected by source matrix, sample collection and/or sample transport.

# General Reporting Notes
(continued)

Significant Figures : Where the reported value is much greater than unity (1.00) in the units expressed, the number is rounded to a whole number of units, rather than to 3 significant figures. For example, a value of 10,456.45 ug catch is rounded to 10,456 ug. There are five significant digits displayed, but no confidence should be placed on more than two significant digits. Manual Integration : The data systems used for processing will flag manually integrated peaks with an “M”. There are several reasons a peak may be manually integrated. These reasons will be identified by the following two letter designations. The peak was not integrated by the software “NI” , the peak

was integrated incorrectlyby the software “II” or the wrong peak was integrated by the software “WP” . These codes will accompany the analyst’s manual integration stamp placed next to the compound name.

# Sample Custody

# This Is The Last Page Of This Report.

# Appendix D

Calibration Data

### Routine Dry Gas Meter Calibration Control Module: C-1 Leak checks Barometric Press. -- 29 .21 Date: 04/08/11 Negative -- ok >15 W.C. Previous Y -- 1.0 020 Technician: MDM3 Positive -- ok >5 in.Hg Previous Delta H -- 1.8072
Orifice Wet Test Wet Test Dry Gas Meter Orifice Diff Volume, Meter Volume Coefficient Coefficient Pressure H Ft 3 

### Inlet Outlet Temp, °F Ft 3 

### Y dH@ Nominal Initial Initial Initial Initial Initial 0.500 5191.00 68.0 68.0 71.0 605.925 Actual Final

5197.00 68.0 68.0 71.0 611.845 14 33.91 0.50 Total Average Average Average Total Minutes

6.00 68.0 68.0 71.0 5.920 14.57 1.0065 1.7076 68.0 Nominal Initial Initial Initial Initial Initial 1.000 5198.00 68.0 68.0 71.0 612.830 Actual Final

5203.00 69.0 68.0 71.0 617.755 8.0 44.47 1.00 Total Average Average Average Total

5.00 68.5 68.0 71.0 4.925 8.74 1.0074 1.7713 68.3 Tm Nominal Initial Initial Initial Initial Initial 2.000 5185.00 68.0 68.0 71.0 600.015 Actual Final Final Final Final Final Minutes SEC

5190.00 68.0 68.0 71.0 604.940 6 13.63 2.00 Total Average Average Average Total

5.00 68.0 68.0 71.0 4.925 6.23 1.0044 1.7979 68.0 Tm Nominal Initial Initial Initial Initial 3.000 5205.00 69.0 68.0 71.0 619.725 Cal. Point Dry Gas Meter Temp, °F Elapsed Time of

Control Module 1 3.000 5205.00 69.0 68.0 71.0 619.725 Actual Final Final Final Final Final Minutes SEC

5210.00 69.0 68.0 71.0 624.655 5.0 7.6 3.00 Total Average Average Total

5.00 69.0 68.0 71.0 4.930 5.13 1.0019 1.8278 68.5 Tm Nominal Initial Initial Initial Initial Initial 4.000 5212.00 69.0 68.0 71.0 626.620 Actual Final Final Final Final Final Minutes SEC

5222.00 70.0 69.0 71.0 636.455 8.0 58.47

. 4.00 Total Average Average Average Total

10.00 69.5 68.5 71.0 9.835 8.97 1.0028 1.8653

69.0 Tm Average 1.0046 1.7940

Control Module 1Cliffs Natural Resources Barr Engineering Co. United Taconite April 29, 2011 Forbes, Minnesota

Emission Measurement Center (EMC) Approved Alternate M ethod (ALT-009) Alternative Method 5 Post-Test Calibration

TEST 1 Control Module C-1 2A Waste Gas Stack (SV048) Input Data Symbol Units Run 1 Run 2 Run 3
Test date - - 4/12/2011 4/12/2011 4/12/2011 Test period - - 858 - 1004 1148 - 1253 1405 - 1509 Total run time t min 60 60 60 Total sample volume measured by dry gas meter V m acf 32.6 33.4 33.6 Absolute average dry gas meter temp T m °F 61.6 76.2 85.6 Absolute average dry gas meter temp T m °R 521.3 535.9 545.3 Barometric pressure P b inches Hg 28.5 28.5 28.5 Conversion factor (29.92/528)(0.75) 2

--- (in Hg/°R) cfm 2 0.0319 0.0319 0.0319 Average orifice meter differential ∆ h avg in. H 2 O 0.94 0.94 0.94 Orifice meter calibration coefficient ∆ H @ in. H 2 O 1.79 1.79 1.79 Dry molecular weight of stack gas M d lb/lb-mole 28.91 28.90 28.90 Dry molecular weight of air --- lb/lb-mole 29.00 29.00 29.00 Specific gravity of mercury --- Dimensionless 13.60 13.60 13.6 0 Dry gas meter calibration check value Y qa Dimensionless 1.0202 1.0094 1.0115 Dry gas meter calibration factor Y Dimensionless 1.0046 1.004 6 1.0046

Average of Y qa 's from test run series 1.0137 Dry gas meter calibration factor 1.0046 % difference between average Y qa 's and Y -0.90% (must be within ± 5%) 

## ) ( 29

6. 13 ( 0319 .0 t

@ avg d avg b m

m qa 

## h M h P H T V Y ∆ • ∆ + ∆ ⋅
=Cliffs Natural Resources Barr Engineering Co. United Taconite April 29, 2011 Forbes, Minnesota

Emission Measurement Center (EMC) Approved Alternate M ethod (ALT-009) Alternative Method 5 Post-Test Calibration

TEST 3 Control Module C-1 2A Waste Gas Stack (SV048) Input Data Symbol Units Run 1 Run 2 Run 3
Test date - - 4/13/2011 4/13/2011 4/13/2011 Test period - - 836 - 941 1034 - 1141 1240 - 1344 Total run time t min 60 60 60 Total sample volume measured by dry gas meter V m acf 33.9 34.4 33.4 Absolute average dry gas meter temp T m °F 82.3 84.1 85.0 Absolute average dry gas meter temp T m °R 541.9 543.8 544.7 Barometric pressure P b inches Hg 28.6 28.6 28.6 Conversion factor (29.92/528)(0.75) 2

--- (in Hg/°R) cfm 2 0.0319 0.0319 0.0319 Average orifice meter differential ∆ h avg in. H 2 O 0.99 1.00 0.99 Orifice meter calibration coefficient ∆ H @ in. H 2 O 1.79 1.79 1.79 Dry molecular weight of stack gas M d lb/lb-mole 29.01 29.02 29.02 Dry molecular weight of air --- lb/lb-mole 29.00 29.00 29.00 Specific gravity of mercury --- Dimensionless 13.60 13.60 13.6 0 Dry gas meter calibration check value Y qa Dimensionless 1.0224 1.0148 1.0416 Dry gas meter calibration factor Y Dimensionless 1.0046 1.004 6 1.0046

Average of Y qa 's from test run series 1.0263 Dry gas meter calibration factor 1.0046 % difference between average Y qa 's and Y -2.16% (must be within ± 5%) 

## ) ( 29

6. 13 ( 0319 .0 t

@ avg d avg b m

m qa 

## h M h P H T V Y ∆ • ∆ + ∆ ⋅
=

### THERMOCOUPLE ID C-1-I
Cal Date: 1/14/2011 

### CALIBRATION TECHNICIAN: AGA

REFERENCE STANDARDS DATE
Hart Scientific 9103-A s/n A1B289 Report No. T10-010 5-2 1/5/2010 Hart Scientific 9140 s/n A1B086 Report No. T10-0105- 1 1/5/2010 

### Temperature Calibration Points 20 70 150 Reference Deg F (To) 20 70 150 Probe Temp (deg F) 20 69 150 Reference Temp (deg R) deg F + 460 480 530 610 Probe Temp (deg R), deg F + 460 480 529 610 Difference (degrees) 0 1 0 % Diff Abs. T 0.0% 0.2% 0.0% 

# THERMOCOUPLE CALIBRATION

Meter In

TRACEABILITY LABORATORY

Hart Scientific Hart Scientific

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-1-I Regression R Squared = 0.999997

-20 1200

Technician signature
QA signature FAHRENHEIT CALIBRATION RANGE 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-1-I Regression R Squared = 0.999997

### THERMOCOUPLE ID C-1-O
Cal Date: 1/14/2011 

### CALIBRATION TECHNICIAN: AGA

REFERENCE STANDARDS DATE
Hart Scientific 9103-A s/n A1B289 Report No. T10-010 5-2 1/5/2010 Hart Scientific 9140 s/n A1B086 Report No. T10-0105- 1 1/5/2010 

### Temperature Calibration Points 20 70 150 Reference Deg F (To) 20 70 150 Probe Temp (deg F) 22 69 148 Reference Temp (deg R) deg F + 460 480 530 610 Probe Temp (deg R), deg F + 460 482 529 608 Difference (degrees) -2 1 2 % Diff Abs. T 0.4% 0.2% 0.3% 

# THERMOCOUPLE CALIBRATION

Meter Out

TRACEABILITY LABORATORY

Hart Scientific Hart Scientific

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-1-O Regression R Squared = 0.999964

-20 1200

Technician signature
QA signature FAHRENHEIT CALIBRATION RANGE 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-1-O Regression R Squared = 0.999964

### PYROMETER CALIBRATION

Pyrometer Number: C-1 

### Date: 1/14/11 Pyrometer Reference: CL-300-1000F 

### Technician: TJW2

Pyrometer o F
Pass/Fail

1000 538 Pass
950 510 Pass
900 482 Pass
850 454 Pass
800 427 Pass
750 399 Pass
700 371 Pass
650 343 Pass
600 316 Pass
550 288 Pass
500 260 Pass
450 232 Pass 601

551

499

449 752

701

652 1001

951

901

851 Reference (°F) Reference (°C) Reading

801

400 204 Pass
350 177 Pass
300 149 Pass
250 121 Pass
200 93 Pass
150 67 Pass
100 38 Pass
50 10 Pass
0 -18 Pass
-50 -46 Fail

Pass/Fail based on +/- 0.75% of Renkin value Unit not to be used at range in which failure occur red

Technician signature: QA signature: 0
-45 200

150

98

49 399

350

301

251

### Routine Dry Gas Meter Calibration Control Module: C-5 Leak checks Barometric Press. -- 29.05 Date: 04/07/11 Positive -- ok >5 W.C. Previous Y -- 1.0009 Technician: MDM3 Negative ok > 15 in.Hg Previous Delta H -- 1.9498
Orifice Wet Test Wet Test Dry Gas Meter Orifice Diff Volume, Meter Volume Coefficient Coefficient Pressure H Ft 3 

### Inlet Outlet Temp, °F Ft 3 

### Y dH@ Nominal Initial Initial Initial Initial Initial 0.500 5141.00 71.0 70.0 71.0 696.425 Actual Final Final Final Final Final Minutes SEC

5146.00 72.0 71.0 71.0 701.345 12 51.06 0.50 Total Average Average Average Total Minutes

5.00 71.5 70.5 71.0 4.920 12.85 1.0150 1.9157

71.0 Nominal Initial Initial Initial Initial Initial 1.000 5147.00 72.0 71.0 70.5 702.340 Actual Final Final Final Final Final Minutes SEC

5154.00 73.0 72.0 70.5 709.295 12.0 48.72 1.00 Total Average Average Average Total

7.00 72.5 71.5 70.5 6.955 12.81 1.0068 1.9356

72.0 Tm Nominal Initial Initial Initial Initial Initial 2.000 5135.00 70.0 69.0 71.0 690.480 Actual Final Final Final Final Final Minutes SEC

5140.00 71.0 70.0 71.0 695.435 6 33.34 2.00 Total Average Average Average Total

5.00 70.5 69.5 71.0 4.955 6.56 1.0021 1.9978

70.0 Tm Nominal Initial Initial Initial Initial Initial Dry Gas Meter Temp, °F Cal. Point Elapsed Time of

Nominal Initial Initial Initial Initial Initial 3.000 5155.00 73.0 72.0 70.5 710.290 Actual Final Final Final Final Final Minutes SEC

5162.00 74.0 72.0 70.5 717.240 7.0 23.69 3.00 Total Average Average Average Total

7.00 73.5 72.0 70.5 6.950 7.39 1.0038 1.9327

72.8 Tm Nominal Initial Initial Initial Initial Initial 4.000 5164.00 74.0 72.0 70.5 719.225 Actual Final Final Final Final Final Minutes SEC

5174.00 75.0 73.0 70.5 729.200 9.0 16.53 4.00 Total Average Average Average Total

10.00 74.5 72.5 70.5 9.975 9.28 0.9981 1.9847

73.5 Tm Average 1.0052 1.9533Cliffs Natural Resources Barr Engineering Co.

United Taconite April 29, 2011 Forbes, Minnesota

Emission Measurement Center (EMC) Approved Alternate M ethod (ALT-009) Alternative Method 5 Post-Test Calibration

TEST 2 Control Module C-5 2B Waste Gas Stack (SV049) Input Data Symbol Units Run 1 Run 2 Run 3
Test date - - 4/12/2011 4/12/2011 4/12/2011 Test period - - 856 - 1006 1148 - 1255 1405 - 1511 Total run time t min 60 60 60 Total sample volume measured by dry gas meter V m acf 34.5 34.1 33.6 Absolute average dry gas meter temp T m °F 62.7 67.0 74.0 Absolute average dry gas meter temp T m °R 522.3 526.7 533.6 Barometric pressure P b inches Hg 28.5 28.5 28.5 Conversion factor (29.92/528)(0.75) 2

--- (in Hg/°R) cfm 2 0.0319 0.0319 0.0319 Average orifice meter differential ∆ h avg in. H 2 O 1.11 1.07 1.02 Orifice meter calibration coefficient ∆ H @ in. H 2 O 1.95 1.95 1.95 Dry molecular weight of stack gas M d lb/lb-mole 28.91 28.91 28.89 Dry molecular weight of air --- lb/lb-mole 29.00 29.00 29.00 Specific gravity of mercury --- Dimensionless 13.60 13.60 13.6 0 Dry gas meter calibration check value Y qa Dimensionless 1.0029 0.9996 0.9973 Dry gas meter calibration factor Y Dimensionless 1.0052 1.005 2 1.0052

Average of Y qa 's from test run series 1.0000 Dry gas meter calibration factor 1.0052 % difference between average Y qa 's and Y 0.52% (must be within ± 5%) 

## ) ( 29

6. 13 ( 0319 .0 t

@ avg d avg b m

m qa 

## h M h P H T V Y ∆ • ∆ + ∆ ⋅
=Cliffs Natural Resources Barr Engineering Co.

United Taconite April 29, 2011 Forbes, Minnesota

Emission Measurement Center (EMC) Approved Alternate M ethod (ALT-009) Alternative Method 5 Post-Test Calibration

TEST 4 Control Module C-5 2B Waste Gas Stack (SV049) Input Data Symbol Units Run 1 Run 2 Run 3
Test date - - 4/13/2011 4/13/2011 4/13/2011 Test period - - 836 - 943 1034 - 1141 1240 - 1346 Total run time t min 60 60 60 Total sample volume measured by dry gas meter V m acf 33.7 33.9 33.9 Absolute average dry gas meter temp T m °F 58.0 60.5 60.8 Absolute average dry gas meter temp T m °R 517.7 520.2 520.5 Barometric pressure P b inches Hg 28.6 28.6 28.6 Conversion factor (29.92/528)(0.75) 2

--- (in Hg/°R) cfm 2 0.0319 0.0319 0.0319 Average orifice meter differential ∆ h avg in. H 2 O 1.07 1.08 1.10 Orifice meter calibration coefficient ∆ H @ in. H 2 O 1.95 1.95 1.95 Dry molecular weight of stack gas M d lb/lb-mole 29.00 28.98 29.00 Dry molecular weight of air --- lb/lb-mole 29.00 29.00 29.00 Specific gravity of mercury --- Dimensionless 13.60 13.60 13.6 0 Dry gas meter calibration check value Y qa Dimensionless 1.0030 1.0030 1.0105 Dry gas meter calibration factor Y Dimensionless 1.0052 1.005 2 1.0052

Average of Y qa 's from test run series 1.0055 Dry gas meter calibration factor 1.0052 % difference between average Y qa 's and Y -0.03% (must be within ± 5%) 

## ) ( 29

6. 13 ( 0319 .0 t

@ avg d avg b m

m qa 

## h M h P H T V Y ∆ • ∆ + ∆ ⋅
=

## THERMOCOUPLE ID C-5-I
Cal Date: 1/13/2011 

### CALIBRATION TECHNICIAN: MMK2

REFERENCE STANDARDS DATE
Hart Scientific 9103-A s/n A1B289 Report No. T10-010 5-2 1/5/2010 Hart Scientific 9140 s/n A1B086 Report No. T10-0105- 1 1/5/2010 

### Temperature Calibration Points 20 70 150 Reference Deg F (To) 20 70 150 Probe Temp (deg F) 21 69 149 Reference Temp (deg R) deg F + 460 480 530 610 Probe Temp (deg R), deg F + 460 481 529 609 Difference (degrees) -1 1 1 % Diff Abs. T 0.2% 0.2% 0.2% 

# THERMOCOUPLE CALIBRATION

Meter In

TRACEABILITY LABORATORY

Hart Scientific Hart Scientific

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R



### REFERENCE TEMPERATURE, deg.R THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-5-I Regression R Squared = 0.999989

-20 1200

Technician signature
QA signature FAHRENHEIT CALIBRATION RANGE 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R



### REFERENCE TEMPERATURE, deg.R THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-5-I Regression R Squared = 0.999989

### THERMOCOUPLE ID C-5-O
Cal Date: 1/13/2011 

### CALIBRATION TECHNICIAN: MMK2

REFERENCE STANDARDS DATE
Hart Scientific 9103-A s/n A1B289 Report No. T10-010 5-2 1/5/2010 Hart Scientific 9140 s/n A1B086 Report No. T10-0105- 1 1/5/2010 

### Temperature Calibration Points 20 70 150 Reference Deg F (To) 20 70 150 Probe Temp (deg F) 21 69 149 Reference Temp (deg R) deg F + 460 480 530 610 Probe Temp (deg R), deg F + 460 481 529 609 Difference (degrees) -1 1 1 % Diff Abs. T 0.2% 0.2% 0.2% 

# THERMOCOUPLE CALIBRATION

Meter Out

TRACEABILITY LABORATORY

Hart Scientific Hart Scientific

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R



### REFERENCE TEMPERATURE, deg.R THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-5-O Regression R Squared = 0.999989

-20 1200

Technician signature

QA signature FAHRENHEIT CALIBRATION RANGE 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R



### REFERENCE TEMPERATURE, deg.R THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID C-5-O Regression R Squared = 0.999989

### PYROMETER CALIBRATION

Pyrometer Number: C-5 

### Date: 1/13/11 Pyrometer Reference: CL-300-1000F 

### Technician: TJW2

Pyrometer o F
Pass/Fail

1000 538 Pass
950 510 Pass
900 482 Pass
850 454 Pass
800 427 Pass
750 399 Pass
700 371 Pass
650 343 Pass
600 316 Pass
550 288 Pass
500 260 Pass
450 232 Pass 599

548

497

447 751

700

650 1000

950

899

850 Reference (°F) Reference (°C) Reading

799

400 204 Pass
350 177 Pass
300 149 Pass
250 121 Pass
200 93 Pass
150 67 Pass
100 38 Pass
50 10 Pass
0 -18 Pass
-50 -46 Pass

Pass/Fail based on +/- 0.75% of Renkin value

Technician signature: QA signature: 1
-49 200

151

98

49 398

348

300

251

### THERMOCOUPLE ID TC4-3
Cal Date: 1/8/2011 

### CALIBRATION TECHNICIAN: MMK2

REFERENCE STANDARDS DATE
Hart Scientific 9103-A s/n A1B289 Report No. T10-010 5-2 1/5/2010 Hart Scientific 9140 s/n A1B086 Report No. T10-0105- 1 1/5/2010 

### Temperature Calibration Points 32 212 400 650 Ambient Reference Deg F (To) 32 212 400 650 70 Probe Temp (deg F) 34 212 398 650 70 Reference Temp (deg R) deg F + 460 492 672 860 1110 530 Probe Temp (deg R), deg F + 460 494 672 858 1110 530 Difference (degrees) -2 0 2 0 0 % Diff Abs. T 0.4% 0.0% 0.2% 0.0% 0.0% Is difference less than 1.5% at all measured points? YES 

# THERMOCOUPLE CALIBRATION

M-5 Probe

TRACEABILITY LABORATORY

Hart Scientific Hart Scientific

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve THERMOCOUPLE ID TC4-3 Regression R Squared = 0.999974

Are extrapolated limits less than 1.5%? YES -20 1200

Technician signature
QA signature FAHRENHEIT CALIBRATION RANGE

If not acceptable, describe corrective action: 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve THERMOCOUPLE ID TC4-3 Regression R Squared = 0.999974

### THERMOCOUPLE ID TC5-2
Cal Date: 1/7/2011



### CALIBRATION TECHNICIAN: MMK2

REFERENCE STANDARDS DATE
Hart Scientific 9103-A s/n A1B289 Report No. T10-010 5-2 1/5/2010 Hart Scientific 9140 s/n A1B086 Report No. T10-0105- 1 1/5/2010 

### Temperature Calibration Points 32 212 400 650 Ambient Reference Deg F (To) 32 212 400 650 70 Probe Temp (deg F) 33 209 398 648 70 Reference Temp (deg R) deg F + 460 492 672 860 1110 530 Probe Temp (deg R), deg F + 460 493 669 858 1108 530 Difference (degrees) -1 3 2 2 0 % Diff Abs. T 0.2% 0.4% 0.2% 0.2% 0.0% Is difference less than 1.5% at all measured points? YES 

# THERMOCOUPLE CALIBRATION

M-5 Probe

TRACEABILITY LABORATORY

Hart Scientific Hart Scientific

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID TC5-2 Regression R Squared = 0.99997

Are extrapolated limits less than 1.5%? YES -20 1200

Technician signature
QA signature FAHRENHEIT CALIBRATION RANGE

If not acceptable, describe corrective action: 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700

400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700THERMOCOUPLE TEMPERATURE, deg.R

REFERENCE TEMPERATURE, deg.R



# THERMOCOUPLE CALIBRATION

Calibration Curve - Unit Under Test Upper Limit of Calibration
Lower Limit of Calibration Extrapolated Calibration Curve 

### THERMOCOUPLE ID TC5-2 Regression R Squared = 0.99997

### Field Barometer Calibration Calibration to National Weather Service at Chisholm -Hibbing Airport

Station elevation at Barr Hibbing Office 3128 14th Avenue East, Hibbing, MN 1460 ft.

Barometer: DJK Field Barometer Barr Office

Date Technician Time Altimeter ID Time Barometric Pressure Station

Pressure Condition Remarks NWS Observation

3/16/11 RMP 16:05 29.76 DJK 16:11 28.35 28.35 In Calibration As Found 4/18/11 DJK 5:53 29.94 DJK 6:12 28.50 28.48 In Calibration As Found

# Appendix E

Cylinder Gas Certifications

# Appendix F

Process Operating Data

### Form ST-05



# Operating Data Summary For Process Sources

Minnesota Pollution Control Agency 520 Lafayette Rd. N. Saint Paul, MN 55155-4194 ( 651)-296-6300
6/9/06

Equipment & Operating Data 1. 2. X NO: If no, explain:

3.

4.

5. ratios as appropriate



### Run 1 Average 630 638 507 510

3512 3465 211 208

6 Date(s) and procedure(s) of last maintenance/cleaning within 6 months: Remains unchanged from info. provided in test plan 

### Test Date(s): 4/12/2011 Process Equipment Number/Identification: WGS 2A (SV048) Company Name: United Taconite, LLC

See attached Process rate (amount of raw material or finished product pe r hour, wet or dry basis) while combusting (list fuel type(s) and



### Process Parameter: list type and units Run 2 Run 3 Process Equipment Description: 

### Line 2 Induration Furnace Were the process and control equipment operated consistent w ith normal procedures? YES:



### Include copy of production records or instrumentati on which indicates rate of production or operation of the equipment, i.e. units per hour, pounds per hour, pressure, air flow, etc.

Greenball Feed Rate, LTPH 641 643 Fired Pellets, LTPH 510 514

Fuel Input (list units) Natural Gas (cfm) 3371 3513 Heat Input (10 6 

### British thermal units/hour) 202 211

Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as 

### 6

• Baghouse, Cyclone, and Multi-clone: ∆ P (in. w.c.)

• ESP: Number and identity of operating field(s) 

### Run 1 Average 11.41 11.1 2412.12 2412.4

Run 1 Average

aq-f6-ST05 Form ST-05
, Page 1 of 1 Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as approved in the test plan. (See test plan and approval letter)



### Examples of APC equipment and parameters generally monitored. Monitor as in test plan and/or approval letter.

• Scrubber (list type of scrubber): ∆ P (in. w.c.) and feed rate (gpm and psig)

• Catalytic Incinerator :( ° F in , ° F out ) and Thermal Incinerator: ( ° F temperature ) 

### APC and parameter monitored Run 2 Run 3 Scrubber Pressure Drop, (in. w.c.) 10.91 10.86 Scrubber Flow (gpm) 2412.11 2412.82

List pollutant & averaging basis.--should reflect p ermit Run 2 Run 3

Monitor (list averaging basis):

Note: This form provides only a summary of the operating cond itions during the performance test. Additional and more detailed records are required to meet the requirements of Minn. R. 7017.2035, subp. 3. This form is to be submitted as part of the performance test report. 

### Continuous Opacity Monitor(list hourly average) Monitor (list averaging basis):

Abbreviations: APC-air pollution control gpm.-gallons per minute in. w.c .-inches of water column

lbs.-pounds psig-pressure per square inch gauge ∆ P- pressure drop

### Form ST-05



# Operating Data Summary For Process Sources

Minnesota Pollution Control Agency 520 Lafayette Rd. N. Saint Paul, MN 55155-4194 ( 651)-296-6300
6/9/06

Equipment & Operating Data 1. 2. X NO: If no, explain:

3.

4.

5. ratios as appropriate



### Run 1 Average 630 638 507 510

3512 3465 211 208

6 Date(s) and procedure(s) of last maintenance/cleaning within 6 months: Remains unchanged from info. provided in test plan 

### Test Date(s): 4/12/2011 Process Equipment Number/Identification: WGS 2A (SV049) Company Name: United Taconite, LLC

See attached Process rate (amount of raw material or finished product pe r hour, wet or dry basis) while combusting (list fuel type(s) and



### Process Parameter: list type and units Run 2 Run 3 Process Equipment Description: 

### Line 2 Induration Furnace Were the process and control equipment operated consistent w ith normal procedures? YES:



### Include copy of production records or instrumentati on which indicates rate of production or operation of the equipment, i.e. units per hour, pounds per hour, pressure, air flow, etc.

Greenball Feed Rate, LTPH 641 643 Fired Pellets, LTPH 510 514

Fuel Input (list units) Natural Gas (cfm) 3371 3513 Heat Input (10 6 

### British thermal units/hour) 202 211

Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as 

### 6

• Baghouse, Cyclone, and Multi-clone: ∆ P (in. w.c.)

• ESP: Number and identity of operating field(s) 

### Run 1 Average 10.23 9.9 2498.68 2497.8

Run 1 Average

aq-f6-ST05 Form ST-05
, Page 1 of 1 Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as approved in the test plan. (See test plan and approval letter)



### Examples of APC equipment and parameters generally monitored. Monitor as in test plan and/or approval letter.

• Scrubber (list type of scrubber): ∆ P (in. w.c.) and feed rate (gpm and psig)

• Catalytic Incinerator :( ° F in , ° F out ) and Thermal Incinerator: ( ° F temperature ) 

### APC and parameter monitored Run 2 Run 3 Scrubber Pressure Drop, (H2O) 9.74 9.73 Scrubber Flow (GPM) 2496.34 2498.24

List pollutant & averaging basis.--should reflect p ermit Run 2 Run 3

Monitor (list averaging basis):

Note: This form provides only a summary of the operating cond itions during the performance test. Additional and more detailed records are required to meet the requirements of Minn. R. 7017.2035, subp. 3. This form is to be submitted as part of the performance test report. 

### Continuous Opacity Monitor(list hourly average) Monitor (list averaging basis):

Abbreviations: APC-air pollution control gpm.-gallons per minute in. w.c .-inches of water column

lbs.-pounds psig-pressure per square inch gauge ∆ P- pressure drop

### Form ST-05



# Operating Data Summary For Process Sources

Minnesota Pollution Control Agency 520 Lafayette Rd. N. Saint Paul, MN 55155-4194 ( 651)-296-6300
6/9/06

Equipment & Operating Data 1. 2. X NO: If no, explain:

3.

4.

5. ratios as appropriate



### Run 1 Average 646 645 517 517

9.25 9.12 253 248

6 Include copy of production records or instrumentati on which indicates rate of production or operation of the equipment, i.e. units per hour, pounds per hour, pressure, air flow, etc.

Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as 

### Run 2 646 521

9.14 247 Heat Input (10 6 

### British thermal units/hour) Company Name:

Process Equipment Description: Were the process and control equipment operated consistent w ith normal procedures? YES:

Date(s) and procedure(s) of last maintenance/cleaning within 6 months: Remains unchanged from info. provided in test plan

Process rate (amount of raw material or finished product pe r hour, wet or dry basis) while combusting (list fuel type(s) and See attached



### Fuel Input (list units) Coal (TPH)

4/13/2011

Run 3 643 Line 2 Induration Furnace

Greenball Feed Rate, LTPH

United Taconite, LLC Process Equipment Number/Identification: Test Date(s):

512

8.97 243 WGS 2A (SV048)

Fired Pellets, LTPH Process Parameter: list type and units

6

• Baghouse, Cyclone, and Multi-clone: ∆ P (in. w.c.)

• ESP: Number and identity of operating field(s) 

### Run 1 Average 11.49 11.4 2411.59 2411.6

Run 1 Average

aq-f6-ST05 Form ST-05
, Page 1 of 1 Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as approved in the test plan. (See test plan and approval letter)

Note: This form provides only a summary of the operating cond itions during the performance test. Additional and more detailed records are required to meet the requirements of Minn. R. 7017.2035, subp. 3. This form is to be submitted as part of the performance test report. 

### Run 2 Run 2 11.45 2411.43 Examples of APC equipment and parameters generally monitored. Monitor as in test plan and/or approval letter.

• Scrubber (list type of scrubber): ∆ P (in. w.c.) and feed rate (gpm and psig)

• Catalytic Incinerator :( ° F in , ° F out ) and Thermal Incinerator: ( ° F temperature )



### Scrubber Flow (gpm) 11.28 2411.7 APC and parameter monitored Run 3

Run 3 List pollutant & averaging basis.--should reflect p ermit Continuous Opacity Monitor(list hourly average) Monitor (list averaging basis): Monitor (list averaging basis): Scrubber Pressure Drop, (in. w.c.)

Abbreviations: APC-air pollution control gpm.-gallons per minute in. w.c .-inches of water column

lbs.-pounds psig-pressure per square inch gauge ∆ P- pressure drop

### Form ST-05



# Operating Data Summary For Process Sources

Minnesota Pollution Control Agency 520 Lafayette Rd. N. Saint Paul, MN 55155-4194 ( 651)-296-6300
6/9/06

Equipment & Operating Data 1. 2. X NO: If no, explain:

3.

4.

5. ratios as appropriate



### Run 1 Average 646 645 517 517

9.25 9.12 253 248

6 Date(s) and procedure(s) of last maintenance/cleaning within 6 months: Remains unchanged from info. provided in test plan 

### Test Date(s): 4/13/2011 Process Equipment Number/Identification: WGS 2A (SV049) Company Name: United Taconite, LLC

See attached Process rate (amount of raw material or finished product pe r hour, wet or dry basis) while combusting (list fuel type(s) and



### Process Parameter: list type and units Run 2 Run 3 Process Equipment Description: 

### Line 2 Induration Furnace Were the process and control equipment operated consistent w ith normal procedures? YES:



### Include copy of production records or instrumentati on which indicates rate of production or operation of the equipment, i.e. units per hour, pounds per hour, pressure, air flow, etc.

Greenball Feed Rate, LTPH 646 643 Fired Pellets, LTPH 521 512

Fuel Input (list units) Coal (TPH) 9.14 8.97 Heat Input (10 6 

### British thermal units/hour) 247 243

Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as 

### 6

• Baghouse, Cyclone, and Multi-clone: ∆ P (in. w.c.)

• ESP: Number and identity of operating field(s) 

### Run 1 Average 10.26 10.2 2496.96 2497.3

Run 1 Average

aq-f6-ST05 Form ST-05
, Page 1 of 1 Summarize control equipment operating data documented during testing. Values reported should reflect maximum, minimum, ave rages, or as approved in the test plan. (See test plan and approval letter)



### Examples of APC equipment and parameters generally monitored. Monitor as in test plan and/or approval letter.

• Scrubber (list type of scrubber): ∆ P (in. w.c.) and feed rate (gpm and psig)

• Catalytic Incinerator :( ° F in , ° F out ) and Thermal Incinerator: ( ° F temperature ) 

### APC and parameter monitored Run 2 Run 3 Scrubber Pressure Drop, (H2O) 10.26 10.05 Scrubber Flow (GPM) 2495.87 2499.15

List pollutant & averaging basis.--should reflect p ermit Run 2 Run 3

Monitor (list averaging basis):

Note: This form provides only a summary of the operating cond itions during the performance test. Additional and more detailed records are required to meet the requirements of Minn. R. 7017.2035, subp. 3. This form is to be submitted as part of the performance test report. 

### Continuous Opacity Monitor(list hourly average) Monitor (list averaging basis):

Abbreviations: APC-air pollution control gpm.-gallons per minute in. w.c .-inches of water column

lbs.-pounds psig-pressure per square inch gauge ∆ P- pressure dropGAS TESTGreenball Fired Pellets Fuel Fuelasking Coal Gas Line 2A L2A WG Line 2B L2B WGstart end LTPH LTPH TPH cfm dP Flow GPM dP Flow GPM4/12/11 8:58 4/12/11 9:13628.72506.190.003511.8511.432414.8610.242507.574/12/11 9:13 4/12/11 9:28633.67509.820.003513.9411.412408.8810.232494.024/12/11 9:28 4/12/11 9:43631.05507.600.003512.5311.432409.8910.232496.264/12/11 9:43 4/12/11 9:58627.96505.590.003509.4011.392414.8510.202496.87AVERAGE630.35507.300.003511.9311.412412.1210.232498.684/12/11 11:48 4/12/11 12:03639.70510.380.003506.3610.832414.829.692498.064/12/11 12:03 4/12/11 12:18637.58506.150.003507.5010.932407.919.772498.004/12/11 12:18 4/12/11 12:33642.83510.140.003395.2810.892411.579.722494.664/12/11 12:33 4/12/11 12:48643.45512.050.003074.0810.972414.159.802494.64AVERAGE640.89509.680.003370.8110.912412.119.742496.344/12/11 14:05 4/12/11 14:20644.05513.780.003510.1011.022409.559.852495.384/12/11 14:20 4/12/11 14:35644.23514.540.003516.7310.872411.969.742499.474/12/11 14:35 4/12/11 14:50641.27512.740.003511.5610.822418.479.652496.824/12/11 14:50 4/12/11 15:05643.08514.180.003512.3210.722411.309.682501.28AVERAGE643.16513.810.003512.6810.862412.829.732498.24SV 48 SV 49Run 1Run 2Run 3Coal TestGreenball Fired Pellets Fuel Fuelasking Coal Gas Line 2A L2A WG Line 2B L2B WGstart end LTPH LTPH TPH cfm dP Flow GPM dP Flow GPM4/13/11 8:39 4/13/11 8:54644.37514.809.220.0011.472412.3810.262497.594/13/11 8:54 4/13/11 9:09645.22515.359.160.0011.502415.7510.282504.764/13/11 9:09 4/13/11 9:24647.71518.639.300.0011.462413.1310.242492.594/13/11 9:24 4/13/11 9:39647.14519.899.310.0011.502405.1010.272492.91AVERAGE646.11517.179.250.0011.492411.5910.262496.964/13/11 10:35 4/13/11 10:50645.02521.439.110.0011.432415.6010.192489.724/13/11 10:50 4/13/11 11:05647.51522.559.190.0011.422410.9910.282504.864/13/11 11:05 4/13/11 11:20647.32521.069.070.0011.472407.9710.312491.844/13/11 11:20 4/13/11 11:35645.67520.319.210.0011.482411.1410.272497.06AVERAGE646.38521.339.140.0011.452411.4310.262495.874/13/11 12:40 4/13/11 12:55647.11515.168.440.0011.272413.2110.092496.054/13/11 12:55 4/13/11 13:10643.17511.798.890.0011.252410.3710.012505.834/13/11 13:10 4/13/11 13:25646.02514.609.190.0011.302413.0010.062497.304/13/11 13:25 4/13/11 13:40635.95504.939.350.0011.292410.2110.042497.40AVERAGE643.06511.628.970.0011.282411.7010.052499.15SV 48 SV 49Run 1Run 2Run 3

### During maintenance downtime from 3/13/2011 to 3/27/2011, the following was completed:

Maintenance on Line 2 scrubbers, including inspections, draining, and pressure washing, replacement of hoses and piping as necessary General maintenance in the Line 2 kiln Repair of Line 2 baffle walls

# Appendix G

Stack Test PlanFrom: Maxwell, Candice A. [Candice.Maxwell@CliffsNR.com] Sent: Thursday, April 07, 2011 3:59 PM To: 'Place, Andrew (MPCA)' Cc: Tom Kuchinski; Dan Koschak Subject: UTAC SAM Testing

Good Afternoon Andy,

United Taconite is planning to conduct the sulfuric acid mist (SAM) testing on Line 2 next week (4/11). As we discussed on March 8, 2011, we plan on using Method 8 for the analysis.

Please let me know if you would like to discuss anything else prior to next week’s testing.

Thanks!

Candice

Candice Maxwell Section Manager ‐ Environmental Affairs P 218.744.7849 F 218.744.7635 candice.maxwell@cliffsnr.com CLIFFS NATURAL RESOURCES United Taconite LLC PO Box 180, Eveleth, MN 55734



### _ _____________________________________________________________________________________________________ This electronic message and any at tachments included with this me ssage are for the exclusive use of the individual or entity to which it is intended to be addressed. This message may contai n information that is privileged or confidential and thereby exempt and protected from unauthor ized disclosure under applicable law. If the reader of this message is not the intended recipient, or an employee or agent responsible for delivering the message to the intended recipient, be aware that any disclosure, dissemination, distribut ion or copying of this communication, or the use of its contents, is not authorized and is strictly prohibited. If you have received this communication and are not the intended recipient, please notify the sender immediately and permanently delete the original messag e from your e-mail system.

______________________________________________________________________________________________________ 

## Pa g e 1 of 1

4/26/2011 file://P:\M p ls\23 MN\69\23691092 United Taconite 2010 Stack Testin g \WorkFiles\A p ril 2

...From: Place, Andrew (MPCA) [Andrew.Place@state.mn.us] Sent: Tuesday, March 08, 2011 2:30 PM To: Maxwell, Candice A. Cc: Tom Kuchinski; Dan Koschak Subject: RE: Test Plan Approval

Candice,

I am fine with this changes to the previous approval. Thank you for the update.

A ndy Place Performance Test Coordinator Minnesota Pollution Control Agency 520 Lafayette Road St. Paul, MN 55155

‐ 4194 651

‐ 757

‐ 2652 Andrew.Place@state.mn.us

From: Maxwell, Candice A. [mailto:Candice.Maxwell@CliffsNR.com] Sent: Tuesday, March 08, 2011 11:48 AM To: Place, Andrew (MPCA) Cc: 'Tom Kuchinski'; Dan Koschak Subject: RE: Test Plan Approval

Good Morning Andy,

As we discussed this morning, we are tentatively planning to test Line 2A and 2B waste gas stacks the week of April 4 th for sulfuric acid mist (SAM). We are planning to conduct the SAM testing using Method 8 to verify the ratios used in the permit calculations (the same method the ratio was based on).

Please let me know if you have any questions.

Thanks again for your time this morning.

Candice



### Candice Maxwell Section Manager - En vironmental Affairs P 218.744.7849 F 218.744.7635 candice.maxwell@cliffsnr.com CLIFFS NATURAL RESOURCES United Taconite LLC PO Box 180, Eveleth, MN 55734

From: Place, Andrew (MPCA) [mailto:Andrew.Place@state.mn.us] Sent: Monday, January 24, 2011 1:58 PM To: Maxwell, Candice A. Cc: Tom Kuchinski; Dan Koschak; Palzkill, Steven (MPCA) Subject: Test Plan Approval

Candice,
The forms for the upcoming performance test on EU042 are attached with this email. Please read the approval over prior to the t est to ensure you are in agreement with the conditions surrounding the test.
Print a copy of this email as verification of the appr oval date. Additional forms and guidance may be found at http://www.pca.state.mn.us /air/performancetest.html . If you have any questions or comments, feel free to call.

Thanks,

A ndy Place 

## Pa g e 1 of 2

4/26/2011 file://P:\M p ls\23 MN\69\23691092 United Taconite 2010 Stack Testin g \WorkFiles\A p ril 2

...Performance Test Coordinator Minnesota Pollution Control Agency 520 Lafayette Road St. Paul, MN 55155

‐ 4194 651

‐ 757

‐ 2652 Andrew.Place@state.mn.us



### _ _____________________________________________________________________________________________________ This electronic message and any at tachments included with this me ssage are for the exclusive use of the individual or entity to which it is intended to be addressed. This message may contai n information that is privileged or confidential and thereby exempt and protected from unauthor ized disclosure under applicable law. If the reader of this message is not the intended recipient, or an employee or agent responsible for delivering the message to the intended recipient, be aware that any disclosure, dissemination, distribut ion or copying of this communication, or the use of its contents, is not authorized and is strictly prohibited. If you have received this communication and are not the intended recipient, please notify the sender immediately and permanently delete the original messag e from your e-mail system.

______________________________________________________________________________________________________ 

## Pa g e 2 of 2

4/26/2011 file://P:\M p ls\23 MN\69\23691092 United Taconite 2010 Stack Testin g \WorkFiles\A p ril 2

...aq-f6-08

5/1/07 Page 1 of 2 

# Air Performance Test Form

Performance Test Plan Approval



## Facility Information (please print)
Facility name: United Taconite, LLC AQ#: 869A Facility contact: Candice Maxwell Address: 1200 West Highway 16, Forbes, MN 55738 Phone: (218) 744-7849 Unit(s) to be tested: Lines 2A & 2B (SV048 & SV049) Title V Sulfur Acid Mist Scheduled for: January 12, 2011 at your facility lo cated in: Forbes, Minnesota.


## Test Plan
Submitted on (date): December 22, 2010 Discussed on (date): January 21, 2011 via email


### Your test plan has been approved by the Minnesota P ollution Control Agency (MPCA) as follows:

Shortened test notification approved Test plan approved without modification Test plan approved with the following provisions:

1. The test will be completed using a NCASI Method 8A sample train for three 1 hour runs. The samples wi ll be analyzed by Ion Chromatography which is alternative to the listed method but is allowed by CTM13B.

2. The two stacks will be tested simultaneously as req uired by the permit under two fuel firing scenarios (solid fuel and natural gas)

3. The unit shall be operating at ≥ 630 long tons greenball/hour to avoid a throughput limit being set.

4. Please be reminded all periods indicating noncompli ance with emission limits must be reported to the M PCA. This includes any periods of engineering tests. Ope rating at a rate other than that required by the cu rrent air permit must also be reported. Deviations ultimately need to be reported on the facility’s semiannual d eviation and annual compliance certification forms.



### 5. Label on CD copy should include: Facility Name, AQ File No., Emission Unit Designator, and Test Date.


## Attached Forms

Operating Data Summary – Combustion Sources Operating Data Summary – Waste Combustors Operating Data Summary – Process Sources Operating Data Summary – Asphalt Plants Certifications Form Microfiche/CD-ROM Submittal Form Performance Test Report Completeness Criteria
Note: Forms are also available at www.pca.state.mn.us/air/performancetest.html 

## Approved by:

Date: January 24, 2010 Andrew Place, Pollution Control Specialist Compliance and Enforcement Unit Minnesota Pollution Control Agency

Please contact me at 651-757-2652 if you have any q uestions regarding this approval.
Please be aware that enforcement action will be tak en for performance test failures indicating emissio ns above applicable limits (excess actual emissions to the environment). Failu res commonly result in assessment of a monetary pen alty. Upon the first testaq-f6-08

5/1/07 Page 2 of 2 failure, the Company should take immediate measures to minimize emissions. The measures taken should b e documented, as they will become part of the record of corrective action s. Hard Copy Performance Test Reports and Microfiche o r CD Copy submittals will be addressed to: Air Quality Compliance Tracking Coordinator Minnesota Pollution Control Agency 520 Lafayette Road North St. Paul, Minnesota 55155-4194

cc: Dan Koschak, Barr Engineering (email) Steve Palzkill, MPCA (email) AQ Correspondence File No. 869A

# Test Plan F or A Taconite Production Facility United Taconite, LLC

Forbes, Minnesota

D ate Test P lan created/revised: December 22 , 2010 S che duled Test Dates: Week of January 10 or 24 , 2010 (weather dependent)

PART I: General Information

Emissions facility location Facility contact Testing company contact

United Taconite, LLC 1200 West Hwy 16 Forbes , Minnesota 55738 Candice Maxwell Section Manager

- Environmental Affairs United Taconite, LLC P.O. Box 180 Eveleth, Minnesota 55738 (218)744

- 7849 (218) 744

- 7635 (fax) Dan Koschak S r. Air Quality Technician Barr Engineering Company 3128 14 th Avenue East Hibbing , MN 55746 (218)225

- 8635



### Minnesota Air Emissions Permit Number : 13700113

- 00 5 AQD File Number: 869A

Reason e missions units are to be tested:

Performance Test: Due before the start of actual construction on EU 040 for the project authorized by Air E mission Permit No. 13700113

- 005 while firing only solid fuel and another test while firing only natural gas to verify the ratio of sulfuric acid mist to sulfur dioxide used in the application for Air Emission Permit No. 13700113

- 005. The 2A and 2B stacks (SV048 and SV049) shall be tested simultaneously.
Two testing weeks have been listed as potential testing perio ds. This is due to concerns with possible cold weather affecting safety and method performance as well.

The table below provides the emissions units’ plant nomenclature and permit identification

. Stack drawing s showing stack dimensions and test port orientation and locations relative to airflow disturbances are attached

.

Process unit nomenclature Emissions unit number Stack vent number Group No.

East Line 2 Induration Stack 2A EU042 SV048

-- West Line 2 Induration Stack 2B EU042 SV049

--

## 2 PART II: Testing Requirements

The following table identifies pollutants to be determined; applicable emissions limit and units, and associated regulation for each emissions unit and stack vent



### .

Process unit nomenclature Limitation Basis of Pollutant Tested Pollutant Tested /Permit Limit Specific Methods/Procedures Required Citation

Line 2 Waste

Gas Stack 2A (SV048 )

(EU042) Title I Condition: Testing associated

with a limit taken to avoid classification as a major modification under 40

CFR Section 52.21 and Minn. R. 7007.3000; Minn. R. 7017.2020, subp. 1 EU042 Sulfuric Acid Mist: less than or equal to 15.4 tons using 30

- day Rolling Sum rolled daily.

EU042 Sulfur Dioxide: less than or equal to 197 tons using 30

- day Rolling Sum rolled daily Sulfuric Acid M ist /Sulfur Dioxide
Testing will be performed

on EU042 Waste Gas S tacks SV048 and SV049 simultaneously during two fuel firing conditions ( solid f uel and natural gas only)

EPA Method 1

- 4 40 CFR Part 60 Appendix A

NCASI Method 8A or EPA

Method 8 (see Part IV) Line 2 Waste Gas S tack 2B (SV04 9) (EU042)



### Part III: Operating Conditions

. Process equipment description for units to be tested

Emission Unit #(s) Stack Vent # Description EU042 SV048, SV049 Line 2 induration process waste gases



### Process Parameters to be Monitored : all units to be tested at 90 percent or greater of maximum production
Emission Unit #(s) Process Parameter Units Frequency Range

EU042 (Line 2) Greenball feed rate Long Tons per hour 15 minutes > 630

Finished pellet production rate, Long Tons per hour 15 minutes ~550

Solid fuel input Tons/hour 15 minutes ~7.0

- 9.0

Natural Gas usage CFM 15 minutes ~4000 CFM

## 3 Control equipment ID Control equipment description Monitored parameters Control device parameters recorded at minimum of 15 minute intervals during the test CE049, SV048 CE050, SV049 Wet scrubber high efficiency w/out lime Scrubber water flow rate, gpm Pressure drop across each scrubber, inches
w.c.



### Part IV: Test Methods All tests will be performed using the following USEPA reference test methods.

Test methods Method 1 Sample and Velocity Traverses for Stationary Sources. Once per location
Method 2 EPA Method 2 for stack gas velocity and volumetric flow rate. One determination per sulfuric acid mist test run. Method 3 / 3 A EPA Method 3 or modified 3A to determine stack gas molecular weight at the Line 2 Waste Gas stacks . Integrated stack gas samples will be collected in Tedlar bag and analyzed with instrument calibrated per EPA Method 3A. Method 4 EPA Method 4 for determination of moisture content in stack gas will be performed in conjunction with sulfuric acid mist

. Sulfuric Acid Mist/SO 2 

### NCASI Method 8A or EPA Method 8 NCASI Method 8A or EPA Method 8 for the determination of sulfuric acid mist and sulfur dioxide. Three tests run each to determine sulfuric acid mist and sulfur dioxide concentrations. The test method to be used is currently being researched and will be discussed in the pretest meeting.



### Part V: Continuous Emissions Monitors SO 2 

### and NOx CEMS systems are installed on both stacks. To date neither CEMS has been certified. A RATA was completed on SV049 in November 2010

.


### Part VI: Other Sulfuric acid mist (SAM) emissions will be reported in concentration and lb/hour

. A ratio of SAM to sulfur dioxide will be provided. The test r eport will be submitted to the MPCA on or before February 28, 2010.



### Test Dates : tests scheduled for January 11

- 14 with January 24

- 28 , 2010 as a backup dates depending on weather conditions

. The proposed test schedule follows 1 

### :

Monday January 10 , 20 10 Tuesday January 11, 20 10 Wednesday January 12 , 20 10 Thursday January 13 , 20 10 Friday January 14 , 20 10

Setup

1200

- 1600 Test 2A and 2B Waste Gas Stacks on

solid fuel (SV048 and SV049)

3

- runs for sulfuric

acid mist /SO 2



### 0700

- 15 00 Test 2A and 2B Waste Gas Stacks

on natural gas (SV048 and SV049)

3

- runs for sulfuric

acid mist /SO 2



### 0700

- 15 00

## 4 1 The test schedule may be modified prior to the test dates



### United Taconite and Barr Engineering contacts will make themselves available for a prete st meeting prior 7 days in advance of the testing. At the preference of t he MPCA, United Taconite suggest s the pretest meeting be conducted by telephone.



### Maintenance: A description of any necessary work done within 30 days prior to the test and the normal maintenance schedule followed will be included i n the test report.


### Test Reports: One hard copy and one electronic copy in .pdf format on CD of the test repor t will be submitted to the MPCA on or before February 28, 2010.


### Test plans and report submittals will be addressed to:

Andrew Place Performance Test Coordinator Minnesota Pollution Control Agency 520 Lafayette Road St. Paul, MN 55155

- 4194



### Closing Remarks If there are questions or comments about the information provided, please contact me by telephone or e

- mail.

Candice Maxwell Section Manager

- Environmental Affairs United Taconite , LLC

Attachments : Figure 1

— Test port location drawing s ( SV048, EU042 ) Figure 2

— Test port location drawings ( SV049, EU042 )

c: Dan Koschak

— Barr Engineering Company

# Appendix H

Project Participants and Contact Information#23691092.06 007 

# Project Participants and Contact Information

Minnesota Pollution Control Agency
Andrew Place – Performance Test Coordinator

United Taconite, LLC Candice Maxwell – Section Manager - Environmental Affairs Jennifer Kruse– Process Engineer and Lab Supervisor
Lisa Weidemann – Environmental Coordinator

Barr Engineering Company Tim Russell – Vice President/Chemical Engineer Tom Kuchinski – Stack Testing Supervisor Dan Koschak – Senior Air Quality Technician/Project Manager Ryan Pantzke – Air Quality Technician Michael Norstrem – Air Quality Technician T.J. Webb – Air Quality Technician

CONTACT INFORMATION MPCA Andrew Place Performance Test Coordinator Compliance and Enforcement Section—Industrial Division Minnesota Pollution Control Agency 520 Lafayette Rd. N. Saint Paul, Minnesota 55155 (651) 296-7169 

### andrew.place@state.mn.us United Taconite, LLC Candice Maxwell Section Manager - Environmental Affairs 1200 West Hwy 16 Forbes, MN 55738 (218) 744-7849 Candice.Maxwell@CliffsNR.com Barr Engineering Co. Dan Koschak Sr. Air Quality Technician Barr Engineering Company 3128 14 th 

### Ave East Hibbing, MN 55746 (218) 262-8635 dkoschak@barr.com