# Results of the October 24-November 3,2007 Voluntary Nitrogen Oxides Variability Testing on Line 2Pellet Indurating Furnace (EU021) Stacks SV025, SV026, SV027 and SV028 at Hibbing Taconite Company's Taconite Facility Located in Hibbing, Minnesota

MPCAAQDFileNo.541 Air Emission Permit

# No. 13700061-002 Barr Project No. 23/69-B82-001
Prepared for Hibbing Taconite Company 

# Hibbing, Minnesota
December 2007

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# Results of the October 24-November 3,2007 Voluntary Nitrogen Oxides Variability Testing on Line 2Pellet Indurating Furnace (EU021) Stacks SV025, SV026, SV027 and SV028 at Hibbing Taconite Company's Taconite Facility Located in Hibbing, Minnesota

4700 Wesl 771" Street Minneapolis, MN 55435 Phone: (952) 832·2600 Fax: (952) 832.2601 

# MPCA AQD File No. 541 Air Emission Permit No. 13700061-002 Barr Project No. 23/69-B82-001
Prepared/or Hibbing Taconite Company Hibbing, Minnesota December 2007



# BARR

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# Results of the October 24-November 3, 2007 Voluntary Nitrogen Oxides Variability Testing on Line 2 Pellet Indurating Furnace (EU021) Stacks SV025, SV026, SV027 and SV028 at Hibbing Taconite Company's Taconite Facility Located in Hibbing, Minnesota

Table of Contents Introduction """ " " I Results Summary " 2 Sampling and Analysis Procedure " " 4

Figure 1 Figure 2

Appendix A Appendix B Appendix C Appendix D Appendix E Appendix F Appendix G AppendixH Appendix I List 

## of Figures Test Port Locations - Pellet Indurating Furnace Line 2 (SV025, 026, 027, 028), (EU021) Traverse Point Locations - Pellet Indurating Furnace Line 2 (SV025, 026, 027, 028), (EU021) List of Appendices Report Calculations and Nomenclature Field Data Sheets Instrument Output Ambient Temperature Records Calibration Data Cylinder Gas Certifications Process Operating Data Stack Test Plan Project Participants

# Introduction
Barr Engineering conducted nitrogen oxides (NOx) emissions concentration testing at Hibbing Taconite Company located in Hibbing, Minnesota. The test was conducted as a voluntary effort to evaluate the variability of NO x emissions as it relates to the normal operation of taconite production to establish a predictive equation for NOx emissions. The test simultaneously measured the NOx emissions from the four Line 2 Furnace Waste Gas Stacks for 168 hours.
A test plan was submitted to the Minnesota Pollution Control Agency (MPCA) dated August 29, 2007/0ctober 12, 2007. A copy ofthe test plan is provided in Appendix H. No pretest meeting was held or MPCA approval letter granted due to the voluntary nature of the test.
Pete Rossmiller and Tom Leier of Barr Engineering performed the NOx testing. Andrea Hayden of Hibbing Taconite Company coordinated the test team and facility operations. A representative of the MPCA was not present to witness the tests. A list of project participants is provided in Appendix I. The testing was performed from October 24- November 3,2007.

During the test, the Furnace Line 2 was operated using multiple operating conditions, which were within standard operations. Process data was provided for each condition including fired pellet production rate (long tons per hour), and firing temperatures. The process operating data is located in Appendix G.
The report provides results of the testing and does not address development of the NOx predictive equations. Hibbing taconite will provide predictive equation information under separate cover.
Calculations and other' supporting documentation are located in the appendices.

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# ! Results Summary

On October 24,2007, testing started at Hibbing Taconite's Pellet Indurating Furnace Line 2 Stacks and continued until November 3, 2007. The data that was collected was considered valid when all four analyzers/systems were operating correctly and simultaneously. From October 24 - 31, unheated lines transported the dry sample gas to the analyzer trailer for analysis, with moisture removal occurring at the stack. Difficulties with moisture removal systems occurred due to cold temperatures. Significant down time was experienced. The problem was corrected by using heat traced sample lines and moisture removed in the analyzer trailer for the remainder of the testing. The delays are documented in the Microsoft Excel file.
Hard copies of the data were not printed out due to the large volume of data. Instead, an electronic CD copy is provided with this report that contains all of the test data and emission rate calculations. The data that is provided is calculated by minute. The emission rate of NO x (IblIong ton) was calculated using the average tonnage of the condition obtained with hourly averages. The firing temperatures provided are the average of the condition based on hourly averages.
Hourly average ambient temperatures collected from the on-site meteorological station are provided in AppendixD.

2

# Process Description

Hibbing Taconite Company (HTC) mines iron are (magnetite) and produces taconite pellets that are shipped to steel producers for processing in blast furnaces. The emission sources tested capture the waste gases from the pellet indurating process. Pelletizing Plant Concentrate slurry flows to the thickener after which limestone is added for compression strength. The moisture of the concentrate is reduced by disk filters and then mixed with bentonite and conveyed to balling drums. After leaving the balling drum the green balls are discharged to a roll screen to control the pellet size. The green balls are transferred to an oscillating conveyor and then to a roll conveyor for additional removal of less than !4 inch material. The green balls are distributed evenly across the pallet cars, prior to their entry to the pellet furnace. The pallet cars have a layer of fired pellets already on the bottom and sides of the car called a hearth layer. The hearth layer allows for even airflow through the pellet bed and acts as a buffer between the pallet cal' and the heat generated through the exothermic conversion of magnetite to hematite. There are three natural gas fired furnaces at HTC, Lines 1 and 2 (Phase I), and Line 3 (Phase II). The straight grate furnaces at HTe have several distinct zones. The first two stages are updraft and downdraft drying zones. The next zones are the preheat zone and firing zone. The temperature climbs as the pellets pass through each zone reaching a peak in the firing zone, after which the pellets enter the after-firing zone where the conversion of magnetite to hematite is completed. The last two zones are cooling zones that allow the pellets to be discharged at a temperature of around 120 degrees Fahrenheit, Heated ail' discharged from the two cooling zones is recirculated to the first zones of the furnace for drying and preheating the green balls. Off gases from the furnaces are vented primarily through two ducts, the hood exhaust that handles the drying and recirculated cooling gases, and the wind box exhaust that handles the preheat, firing, and after-firing gases. The windbox exhaust flows through a multiclone, which protects a downstream fan, and then is combined with the hood exhaust steam in a common header. The exhaust gases are subsequently divided into four streams which lead to four venturi rod scrubbers and exhaust from individual stacks.

3

# Sampling and Analysis Procedure 

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! I I The testing was performed from ports meeting EPA Method 1 criteria (40 CFR Part 60, Appendix A). An initial airflow using an S-type pitot was performed using EPA Method 2 criteria (40 CFR Part 60, Appendix A). An S-type pitot tube was fixed at the point in the stack most representative of the average velocity pressure. Differential pressure was read with a Dwyer Magnesense gauge at the stack and the output signal was recorded in l-minute averages with a data logger. Calibrated type "K" thermocouples were positioned in the stack with appropriate signal wire connected to the data logger for stack temperature. Static pressure of the stacks was taken at the beginning of the test and that value was used throughout. Barometric pressure was recorded at the stack test trailer every minute.
Calculations of volumetric airflow were made with l-minute data values for velocity pressure, temperature, barometric pressure, oxygen, and carbon dioxide (for density). Stack gas moisture was measured using approximation method (wet bulb-dry bulb technique) from EPA Method 4 criteria (40 CFR Part 60, Appendix A) for each condition and applied to all calculations for that period. A single static pressure for each stack was used for all calculations.
Nitrogen oxides, oxygen, and carbon dioxide concentrations were determined with modified EPA Method 7E and 3A (40 CFR Part 60, Appendix A). Protocol I gas standards are used for daily instrument calibration, system bias, and calibration drift checks. At least one system bias was performed each day. Copies of the gas certification analysis can be found in Appendix F. A data logger was used to collect the instrument output and calibration log. The data logger averages 60 l-second readings for these I-minute averages. l-minute I-hour averages are provided in the electronic document. Detailed calibration information is displayed in Appendix E and data logger output is displayed in Appendix C.
The system bias calibrations were performed at least once each day and these calibration results are used to bias correct the raw NOx, 02, and C02 averages between the calibration times. A file can be found in the CD jacket on the back of the front page which contains the Microsoft Excel file "60 minute file 11- 19-07(Values)."

4

## NOT TO SCALE 104.5" 

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2 TEST PORTS @ 

### 90' 

# o ",185"



# t TESTING PLATFORM ELEVATION

FROM SCRUBBER



# TEST PORT LOCATIONS HIBBING TACONITE COMPANY HIBBING, MINNESOTA PELLET INDURATING FURNACE LINE 2: VENTURI SCRUBBER (SV025,026,027,028), (EU021) FIGURE 1

## 2 10.50" NO. OF TEST PORTS PORT LENGTH PORT DIAMETER NO. OF TRAVERSE POINTS DUCT DIAMETER 6" 12 104.50" 

# •

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POINT INSERTION DEPTH IN " 1 4.55 2 15.30 3 30.92 4 73.58 5 89.20 6 99.95

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# I , TRAVERSE POINT LOCATIONS HIBBING TACONITE COMPANY HIBBING. MINNESOTA PELLET INDURATING FURNACE LINE 2: VENTURI SCRUBBER 

# (SV025.026.027.02S). (EU021) NOT TO SCALE 

# FIGURE 2

### Calculation Equations - EPA 

### Methods 3A, 6C, 7E, 

### 10, Modified 16A/16B

System bias adjustment on source concentration indicated by the analyzer.

where: is the adjusted source concentration, ppm(dry) is the average concentration indicated by the analyzer, ppm (dry) is the average of the initial and final system calibration responses of the zero gas, ppm is the average of the initial and final system calibration responses of the upscale gas, ppm is the certified concentration of the upscale calibration gas, ppm
Convert source concentration into emission rate (lblhr).

where: 

## C(..!!1E....) dscm 

### MW



### 24.04 E(lbIIlr) 

### 6.242xlO·8 

## Qd 60 

## C _MWxCppm (...!!!L) - 24.04

dscm

E(lblhr) 

# = (6.242 X

## 10-8

# )x C(..!!!K..)X

## 60X

## Qd dscm


### amount of compound, by weight(mg), per dry standard cubic meter of air is the molecular weight of the gaseous compound whereMW= 64 S02 46 N02 

### 28 CO 34 TRS (Assume H2

### S Molecular Weight) is the molar volume of gas at 68 "F and 29.92 in Hg, L'g-mole emission rate of gaseous compound in pounds per hour is the conversion factor from mg/nr' to Ib/ft3 

### flow rate of dry gas at standard conditions in cubic feet per minute, dscfm is the conversion factor from minutes to hours

W:\Business Units\EM\Subunit Admin\Tcchnical &Support Services\AJR SAMPLING\Tcmplate~\Reports\Equations\analyzereq.doc

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# III BARR Project Hibbing Taconite Nox CEMS Sample Location -"L;;.;.in""e-"2';r;--::=r--:---::::--__ Date 

# J(Jidy Operators TYL Duct Dimensions inches Port Length inches Pilot Tube No. Manometer 

### 10 Digital Therm 

### 10 _ Cp Bar. 

### 10



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### OF Averaae

### ..,fAf> Gas

### vei- FUSee ACFM SCFM DSCFM

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### TYL Duct Dimensions Inches Port length Inches Pitot Tube No. Manometer 

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## IOb,!l~i 

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Bar Press (In Hol Stat. Press (In H2O) Temo -DIY Bulb OF 

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## vV).. 1.J' Temo - Wel BulbOF 

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PitotLeakCheck Positive: Negative: _
Traverse Point Information Cyclonic Velocity Head -Inches H2O Slack Temperature -OF Point Inches From: Flow Run 1 Run2 Run3 Run 4 Run 1 Run2 Run 3 Run 4 Number Wall Port 

### ~ LIP LIP LIP LIP Temo. Temo. Temp. Temp.

Schematic of Ducl Cross-Section Run3 Run4 Run2 Slack Pres. - In Ho Duct Area - SQ Ft. Mole Weicht - Md Mole Welch! - Ms Ava. Temo. - OF Averaoe~ Gas Vel - FUSee ACFM SCFM OSCFM

# -- BARR Project Hibbing Taconite Nox CEMS Sample Location -=L:::.in==e:...:2::-:-~.....,"7","""_ Date 

## IfJ(?$/Or Operators TYL Duct Dimensions Inches Port Length Inches Pilot Tube No. Manometer 10 Digital Therm 10 _ Cp Bar. 

### 10



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Bar Press (In Hg) Slat. Press (In H2O) Temo - Drv Bulb of 1)1) 

## U? tb3 

## 1~ Temp- Wet Bulb of 

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Traverse Point Information Cyclonic Velocity Head -Inches H2O Stack Temperature. OF Point Inches From: Flow Run 1 Run 2 Run3 Run 4 Run1 Run 2 Run 3 Run 4 Number Wall Port L" AP AP liP liP Temp. Temp. Temp. Temp.

Schematic of Duct crcss-seenon Run 4 Stack Pres. - In Hg Run2 Run3

Duct Area - Sq Ft. Mola Waigh! - Md Mole Welghl - Ms Ava. Temp. - OF Average 

## ..,r;;;p Gas Vel - FUSee ACFM SCFM DSCFM

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### Taconite Nox CEMS Sample

### Location ..:l::.:.ln:::e-=2:....,-....,...,~r..,...-

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### Length Inches Pitot Tube 

### No. Manometer 

### ID Digital Therm ID _ 

### Cp BaLID



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Traverse Point Information Cyclonic VelocTtV Head • Inches H2O Stack Temperature. of Point Inches From: Flow Run 1 Run 2 Run3 Run 4 Run 1 Run 2 Run3 Run4 Number Wall Port 

### LD AP AP ;l.P ;l.P Temo. Temo, Temo. Temp,

Schematic of Duct Cross-Section Run 4
Duct Area- SQ Ft. Run2 Run 3 Stack Pres, • In Ho
Mole Welaht • Md Mole Weight· Ms Ava, Temo •• OF AveraoeV6P Gas vel- FUSec ACFM SCFM DSCFM

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### ...-:-+

_ Date 

# to(

# 70t0r Operators 

### TYL Duct Dimensions lnches Port Length Inches Pitot Tube No. Manometer 

### 10 Digital Therm 

### 10 _ Cp 

### Bar.ID _ T.C.ID _ 

## EPA METHOD 2 FIELD DATA SHEET

~~ SV025 SV026 SV027 SV028

Ba r Press (in Hal Stat. Press (In H2O) Temo - Drv Bulbof 

### ~ 

## ?to lID

### 4 t!JSTemo - Wet Bulbof 

## rif).. t» 7' JD)J 

### It(,f

Moist Content - % 

### °2% Time of Meas.
Pitot Leak Check Positive: Negative:

_ Traverse Point Information Cyclonic Velocity Head -Inches H!O Stack Temperature - OF Point Inches From: Flow Run 1 Run2 Run 3 Run4 Run 1 Run2 Run 3 Run4 Number Wall Port L." liP tiP liP tiP Temo. Temo. Temp. Temo.

Schematic of Duct Cross-SecUon Run 4 Run2 Run3 Slack Pres. - In Ha Duct Area - Sa Ft. Mole Welahl - Md Mole Weicht - Ms Avo. Temo. - OF Averacev'6P Gas Vel - FtlSec ACFM SCFM DSCFM

# •• BARR Project Hibbing Taconite Nox CEMS Sample Location ,.:;L.:.:,;lnc:.e,.:;2'--:----.--r- _ Date 

# to/¥f"a= Operators TYL Ducl Dimensions Inches Port Length Inches Pitot Tube No. Cp Manometer ID Bar. JD Digital Therm ID T.C.ID _ 

### EPA METHOD 2 FIELD DATA SHEET

~~~~ SV025 SV026 SV027 SV028 •..__ ,.:_~.;'~"'O'_~ Bar Press IInHa\ Slat. Press (InHzO) Temp -Drv Bulbof 

### n9LI 

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Pitot Leak Check Positive: Negative: _
Traverse Polntlnformatlon Cyclonic Velocity Head-Inches H2O Stack Temperature. OF Point Inches From: Flow Run 1 Run2 Run3 Run4 Run1 Run2 Run 3 Run4 Number Wail Port L!' AP •••..P •••..P AP Temo. Temo. Temp. Temo.

Schemalic of Duct Cross-Seelion Run3 Run4 Run2 Stack Pres.· InHo DuctArea •Sa Ft. Mole Weiahl - Md Mole Weloh! • Ms Ava. Temo.• oF Averaa

## e...;:;;;p Gas Vel· FtlSee ACFM SCFM DSCFM

# •• BARR Project Hibbing Taconite Nox CEMS Sample Location .=L:::.in:.:::e.!::2'---r::"....,....,._-=,--__ Date 

# 107'71] 111- Operators 

### r TYL Duct Dimensions inches Port Length Inches Pito! Tube No. Cp Manometer ID Bar.ID Digital Therm ID T.C.ID _ 

## EPA METHOD 2 FIELD DATA SHEET 

# ~~_s,~ SV025 SV026 SV027 SV028

Bar Press (In Ho) Stat. Press (InH2O) Temo - Drv Bulbof 

## /IYG'. I-OCj l/)\., 

# 'I). Temn -Wet BulbOF 

### VV).. lt9fg fOi) 

## If/

MoIst Content - % O2

### % Time of Meas.
Pitot Leak Check Positive: Negative: _ Traverse PoInt Information Cyclonic Velocity Head· Inches H2O Stack Temperature -OF Point Inches From: Flow Run 1 Run 2 Run3 Run 4 Run 1 Run2 Run 3 Run 4 Number Wal! Port L" t.P t.P t.P t.P Temp. Temn, Temn. Temo.

Schematic of Duct crcss-secnon Run4 Run 2 RUn3 Stack Pres. - In Ha Ducl Area - So Ft. Mole Welnhl - Md Mole Weloht - Ms Ava.Temn. - OF AVerageVM> Gas Vel -FUSee ACFM SCFM DSCFM

# III BARR Project Hibbing Taconite Nox CEMS Sample Location ~L~ln,e-r2'-1-'•• ...,...,.:;-:::o

_ Date {//

# IIIvr Operators ' lYL Duct Dimensions Inches Port Length Inches Pilot Tube No. Manometer ID Digital Therm 

### 10 _ Cp Bar.ID _ T.C.ID _ 

### EPA METHOD 2 FIELD DATA SHEET

~~~~ SV025 SV026 SV027 SV028

Bar Press (In Ha) Stat. Press (In H2O) Temo - Drv Bulb of (.)P, 

### tts 

## Iv<,- f.(~ Temo - Wet Bulb of 

## V7I / I 

## 'f IIY) 

### 't"1

Moist Content - % O2% Time of Meas.
Pitot Leak Check Positive: Negative: _
Traverse Point Information Cyclonic Velocity Head -Incbes H2O Stack Temperature. of Point Inches From: Flow Run 1 Run2 Run 3 Run4 Run 1 Run 2 Run3 Run4 Number Wall Port L" ••••.P hP hP AP Temo. Temo. Temo. Temp.

Schematic of Ducl Cross-Secllon Run3 Run 4 Run 2 Stack Pres. - In Ho DuctArea -So Ft. Mole Weloht - Md Mole Weioht - Ms Avo. Temo. - OF Averaae v""AP Gas Vel - FUSec ACFM SCFM DSCFM

# -- BARR Project Hibbing Taconite Nox CEMS Sample Location ..:L:::.lno::e,..:27t---r--=-~ _ Date 

# 7// 2 

# l<rr Operators I TYL Duct Dimensions Inches Port Length inches PitotTube No. Manometer ID Digital Therm ID _ Cp Bar.ID



# --- T.C.ID _ 

### EPA METHOD 2 FIELD DATA SHEET 

## ~Ji~ SV025 SV026 SV027 SV028

Bar Press (In Hg) Stat. Press (In H2O) Temo - Drv Bulbof IH). 

### ~ 

## t6i../ q;, Temo - We! Bulbof 

## 1'J/t J

## l.:rtI J1?~ 

## .jy

Moist Conlent -% O2% Time of Meas.
Pltot Leak Check Positive: Negative: _ Traverse Point Information Cyclonic Velocity Head - Inches H2O Stack Temperature .oF Point Inches From: Flow Run 1 Run2 Run3 Run 4 Run 1 Run2 Run 3 Run4 Number Wall Port L" AP AP AP AP Temo. Temp. Temo. Temo.

Schematic of Ductcross-secnon Run4 Run 2 Run3 Stack Pres .• in Ho DuetArea -So FI. Mole Weicht - Md Mole Weicht· Ms Ava.Temo. -of AveracevTP Gas Vel· FUSee ACFM SCFM DSCFM

# •• BARR Project Hibbing Taconite Nox CEMS Sample Location .!:L:::.in:.:;:e:..;2'-ri?-----c•...

_ Date ~ Operators TYL Duct Dimensions Inches Port Length Inches Pitot Tube No. Manometer ID Digital Therm ID _ 

### Cp Bar.ID _ T.C.ID _ 

### EPA METHOD 2 FIELD DATA SHEET 

# ~~~~~«~~ SV025 SV026 SV027 SV028 Bar Press lin Hal Slat. Press (In H2O) Temo - Drv Bulbof 

# .,n.e J!frJ,

~. 

# 4'1 Temo - Wei Bulbof 

# hn. Iv-c.. 

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Moisl Content -% 

### , 

### O2

### % TIme of Meas.
Pitot Leak Check Positive: ___ Negative: _
Traverse Point Information Cyclonic Veloclty Head- Inches H2O Slack Temperature -of Point Inches From: Flow Run 1 Run2 Run 3 Run 4 Run 1 Run2 Run3 Run 4 Number Wall Port L" liP 

### ..••P .•••P liP Temo. Temo. Temo. Temo •

Schematic of Duct Cross-Section Run4 Run 2 Run3 Stack Pres. - In Ha Duel Area - Sa Ft. Mole Wel!!ht - Md Mole Welahl- Ms Avg. Temp. - OF Averaae../iW Gas Vel - FUSee ACFM SCFM DSCFM

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## Due to the magnitude of the data, the data has been copied to a cd located on the back of the title page. The data is in a Microsoft Excel format.1 

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### Date Date Date Air Mth 

### Day Year Time Temp 

## C.S.T. (degF) 

## 10 24 2007 0 38 10 24 2007 100 37 10 24 2007 200 36 10 24 2007 300 35 10 24 2007 400 34 10 24 2007 500 33 10 24 2007 600 33 10 24 2007 700 32 10 24 2007 800 31 10 24 2007 900 31 10 24 2007 1000 33 10 24 2007 1100 36 10 24 2007 1200 40 10 24 2007 1300 41 10 24 2007 1400 44 10 24 2007 1500 46 10 24 2007 1600 48 10 24 2007 1700 50 10 24 2007 1800 47 10 24 2007 1900 42 10 24 2007 2000 39 10 24 2007 2100 38 10 24 2007 2200 38 10 24 2007 2300 37 10 25 2007 0 37 10 25 2007 100 38 10 25 2007 200 39 10 25 2007 300 38 10 25 2007 400 37 10 25 2007 500 36 10 25 2007 600 36 10 25 2007 700 36 10 25 2007 800 36 10 25 2007 900 37 10 25 2007 1000 41 10 25 2007 1100 47 10 25 2007 1200 52 10 25 2007 1300 56 10 25 2007 1400 59 10 25 2007 1500 60 10 25 2007 1600 61 10 25 2007 1700 60 10 25 2007 1800 56 10 25 2007 1900 52 10 25 2007 2000 49 10 25 2007 2100 46 10 25 2007 2200 45 10 25 2007 2300 43

# I Date Date Date Air Mth Day Year Time Temp 

# I C.S.T. (degF) 

## 10 26 2007 0 42 10 26 2007 100 42 

# I 10 26 2007 200 41 10 26 2007 300 39 10 26 2007 400 38 10 26 2007 500 37 

# I ' 10 26 2007 600 36 10 26 2007 700 35 10 26 2007 800 34 

# I ' 10 26 2007 900 35 10 26 2007 1000 41 10 26 2007 1100 46 

# I ; 10 26 2007 1200 51 10 26 2007 1300 53 10 26 2007 1400 57 

# I 10 26 2007 1500 59 10 26 2007 1600 56 10 26 2007 1700 48 10 26 2007 1800 46 

# I ' 10 26 2007 1900 45 10 26 2007 2000 44 10 26 2007 2100 44 

# I 10 26 2007 2200 42 10 26 2007 2300 41 10 27 2007 0 40 

# I 10 27 2007 100 39 10 27 2007 200 38 10 27 2007 300 37 10 27 2007 400 35 

# I 10 27 2007 500 32 10 27 2007 600 32 10 27 2007 700 30 

# I , 10 27 2007 800 30 10 27 2007 900 32 10 27 2007 1000 35 

# I 10 27 2007 1100 39 10 27 2007 1200 43 10 27 2007 1300 45 

# I 10 27 2007 1400 46 10 27 2007 1500 44 10 27 2007 1600 44 10 27 2007 1700 44 

# I 10 27 2007 1800 41 10 27 2007 1900 37 10 27 2007 2000 34 10 27 2007 2100 32 10 27 2007 2200 31 10 27 2007 2300 30

### Date Date Date Air Mth Day Year Time Temp C.S.T. (degF) 

## 10 28 2007 0 29 10 28 2007 100 28 10 28 2007 200 28 10 28 2007 300 29 10 28 2007 400 27 10 28 2007 500 26 10 28 2007 600 26 10 28 2007 700 25 10 28 2007 800 25 10 28 2007 900 27 10 28 2007 1000 31 10 28 2007 1100 35 10 28 2007 1200 39 10 28 2007 1300 43 10 28 2007 1400 44 10 28 2007 1500 45 10 28 2007 1600 45 10 28 2007 1700 45 10 28 2007 1800 44 10 28 2007 1900 42 10 28 2007 2000 42 10 28 2007 2100 41 10 28 2007 2200 40 10 28 2007 2300 43 10 29 2007 0 44 10 29 2007 100 44 10 29 2007 200 43 10 29 2007 300 43 10 29 2007 400 44 10 29 2007 500 43 10 29 2007 600 41 10 29 2007 700 42 10 29 2007 800 41 10 29 2007 900 41 10 29 2007 1000 46 10 29 2007 1100 50 10 29 2007 1200 53 10 29 2007 1300 57 10 29 2007 1400 60 10 29 2007 1500 62 10 29 2007 1600 64 10 29 2007 1700 63 10 29 2007 1800 59 10 29 2007 1900 52 10 29 2007 2000 50 10 29 2007 2100 48 10 29 2007 2200 47 10 29 2007 2300 46

# I

Dale Date Date Air 

# I
Mth Day Year Time Temp C.S.T. (degF) 

# I 10 30 2007 0 45 I 

## 10 30 2007 100 43 10 30 2007 200 42 [ 10 30 2007 300 42 10 30 2007 400 41 10 30 2007 500 40 

# I ' 10 30 2007 600 40 10 30 2007 700 39 10 30 2007 800 38 j 10 30 2007 900 39 10 30 2007 1000 44 10 30 2007 1100 49 10 30 2007 1200 54 j 10 30 2007 1300 60 10 30 2007 1400 62 10 30 2007 1500 64 

# I 10 30 2007 1600 65 10 30 2007 1700 63 10 30 2007 1800 59 

# I 10 30 2007 1900 55 10 30 2007 2000 54 10 30 2007 2100 53 

# ! 10 30 2007 2200 52 10 30 2007 2300 51 10 31 2007 0 51 10 31 2007 100 52 

# I 10 31 2007 200 51 10 31 2007 300 46 10 31 2007 400 42 

# I 10 31 2007 500 40 10 31 2007 600 39 10 31 2007 700 40 

# I ' 10 31 2007 800 39 10 31 2007 900 38 10 31 2007 1000 38 10 31 2007 1100 37 

# I 10 31 2007 1200 37 10 31 2007 1300 36 10 31 2007 1400 37 

# I 10 31 2007 1500 37 10 31 2007 1600 38 10 31 2007 1700 38 10 31 2007 1800 37 10 31 2007 1900 36 10 31 2007 2000 35 10 31 2007 2100 34 10 31 2007 2200 33 10 31 2007 2300 32

### Date Date Date Air Mth Day Year 

### Time Temp C.S.T. (degF) 

## 11 1 2007 0 31 11 1 2007 100 30 11 1 2007 200 29 11 1 2007 300 28 11 1 2007 400 28 11 1 2007 500 28 11 1 

## 2007 600 29 11 1 2007 700 29 11 1 2007 800 28 11 1 2007 900 28 11 1 2007 1000 32 11 1 2007 1100 37 11 1 2007 1200 41 11 1 2007 1300 45 11 1 2007 1400 48 11 1 2007 1500 50 11 1 2007 1600 49 11 1 2007 1700 49 11 1 2007 1800 47 11 1 2007 1900 45 11 1 2007 2000 45 11 1 

## 2007 2100 44 11 1 2007 2200 43 11 1 2007 2300 43 11 2 2007 0 43 11 2 2007 100 43 11 2 2007 200 44 11 2 2007 300 44 11 2 2007 400 44 11 2 2007 500 43 11 2 

## 2007 600 41 11 2 2007 700 41 11 2 2007 800 41 11 2 2007 900 41 11 2 2007 1000 41 11 2 

## 2007 1100 41 11 2 2007 1200 43 11 2 

## 2007 1300 45 11 2 

## 2007 1400 46 11 2 

## 2007 1500 47 11 2 2007 1600 46 11 2 2007 1700 44 11 2 2007 1800 43 11 2 

## 2007 1900 41 11 2 

## 2007 2000 39 11 2 

## 2007 2100 39 11 2 2007 2200 39 11 2 2007 2300 39I 

# ! 

# I Date Date Date 

### Air Mth Day Year Time Temp 

# I C,S,T. (degF) 

## 11 3 2007 0 38 11 3 2007 100 38 

# I 11 3 2007 200 38 11 3 2007 300 38 11 3 2007 400 37 11 3 2007 500 36 

# I ' 11 3 2007 600 34 11 3 2007 700 33 11 3 2007 800 32 

# I 11 3 2007 900 32 11 3 

## 2007 1000 34 11 3 2007 1100 39 

# I 11 3 2007 1200 42 11 3 2007 1300 43 11 3 2007 1400 46 

# I 11 3 

## 2007 1500 47 11 3 2007 1600 46 11 3 

## 2007 1700 44 11 3 

## 2007 1800 43 

# I 11 3 

## 2007 1900 40 11 3 

## 2007 2000 39 11 3 

## 2007 2100 39 

# I 11 3 2007 2200 38 11 3 

## 2007 2300 36 

# I
I 

# I ! 

# I

)

# BARR EPA METHOD 3A ANALYZER CALIBRATION (Oxygen) 

### Engineering Company Project Sample loco Date Operators Hibbing Taconite line 2 (SV025) __ .....:1~0/~24~.;;.11/212007 

### TYUPJR CYlinder Serial No. Certified Value Cal. Anal. Model 200 

### 1 Zero Gas CC125306 0.0 21.5 % J Mld·ranae CA06683 9.0 20 cmlhr 

### I Hlqh-ranae CC12009 21.5 Analyzer Modell SN Analyzer Range (span) Stripchart Speed (units): ANAlYZERCAlI8RATION DATA Note: Difference must be less than +1·2 percent of span Cylinder Analyzer Absolute Difference, Test Runs: _1_

# - ..1Q Value Calibration Difference % of Span Response Zero Gas 0.0 0.0 0.0 0.00% Mld·raae 9.0 9.0 0.0 0.00% Hiah-ranne: 21.5 21.4 0.1 0.65%

PRETEST RESPONSE TIME Note: Time to register 95% stepchange with high level gas. 

# I ~~f(::;) 

# I~i:>'i::':.'513"c~;;.:1 ~'iS'.:;5s..,,":;..1 h~+'~ -'\";'C If---'A;..:.v,---"~""r;i"g",,,e:'---1

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal blas cannot exceed +/. 5 percent of span. Drift eannot exceed +/- 3 percent of span
IniUal Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift,

Response, Response, Cal. Bras Response, Cal. Bias Percent of 10/25/2007 PPM PPM % of Span PPM % of Span span Zero Gas 0.0 ~:~j:' '0:0' -.,'::c::.. .. 0.00% ',0 0.93% 0.93% ..,', Unseale Gas 21.4 

## ~;ct:21.6~~'~c,= -1.86% <""21.3.-."; -0.46% 1.39% 10/26/2007 Zero Gas 0.0 0.2 0.93% ··>{:O.2 

## "".-/1 0.93% 0.00% uoscate Gas 21.4 21.3 -0.46% <Cf;'21-.-4. ',~! 0.00% 0.46% 10/27/2007 Zero Gas 0.0 0.2 0.93% ;:6.2 .: ,~ 0.93% 0.00% Upscale Gas 

# I 0.00% ,,+021.2 

## ·.:.:1 -0.93% 21.4 21.4 -0.93% 10/28/2007 Zero Gas 0.0 0.2 0.93% 

### ~F<O:O,; 0.00% -0.93% Uoscale Gas 21.4 21.2 -0.93% 

## I.:I'',--21To~: ~,.i ·1.86% ·0.93% 10/29/2007 Zero Gas 0.0 0.0 0.00% rtF~'bX,>··N:n 0.46% 0.46% uescate Gas 21.4 21.0 -1.86% 1':-';· 'L hV..• c -, '" ·1.86% 0.00% 10/30/2007 Zero Gas 0.0 0.1 0.46% 

### '.,,-"--'1 0.46% 0.00% Upscale Gas 21.4 21.0 -1.86% -1.86% 0.00% 10/31/2007 Zero Gas 0.0 0.1 0.46% ,,-"~'".I 1.39% 0.93% Uoscale Gas 21.4 21.0 -1.86% i'::;2tO:=-h -1.86% 0.00% 10/31/07 PM Zero Gas 0.0 0.3 1.39% 

## 1<.Yi'i~~·"d 1.39% 0.00% Upscale Gas 21.4 21.0 -1.86% 

## :h:'2i4" . '::-1 0.00% 1.86% 11/1/2007 Zero Gas 0.0 0.3 1.39% ;-- ~- 

### 0.2."' 

# I 0.93% -0.46% Uoscale Gas 21.4 

## I 21.4 0.00% 

# > 2(0 ' 

### '--;'1 ·1.86% -1.86% 11/2/2007 Zero Gas 0.0 0.2 0.93% 0.1 0,46% -0,46% Upscale Gas 21.4 21.0 -1.86% 21.2 -0.93% 0.93% System Calibration Bias 

### = [(System Cal. Response - Analyzer Cal. Response) ISpan) x 100 Drift

# = [(Final System Cal. Response - Initial System Cal Response) / Span] x 100 02

# BARR EPA METHOD 3A ANALYZER CALIBRATION (Carbon Dioxide) Engineering Company Project Sample Loc. Date Operators Hibbing Taconite Line 2 (SV025) ___ 1=.=0.:.:;/2:=47.--11/212007 

### TYU Analyzer Modell SN Analyzer Range (span) Siripchart Speed (units): PJR CVllnder Serial No. Certified Value Cal. Anal. Model 200 Zero Gas CC126306 0.0 9.0 % Mld·ranaB CC12009 5.0 N1A Hlah-ranae CA06683 9.0
ANALYZER CALIBRATION DATA Note: Difference must be less than +1-2 percent of span Cylinder Analyzer Absolute Difference, Test Runs: _1_ 

# - ..J!L Value Calibration Difference % of Span Resoonse Zero Gas 0.0 0.0 0.0 0.00% Mid·raoe 5.0 5.0 0.0 0.44% Hloh·ranoe: 9.0 9.0 0.0 0.00%

PRETEST RESPONSE TIME Note: Time 10register 95% stepchange with high level gas. 

# I Res~onse 

# I···,·· 1 

# l 2 

# ,I 3 

# ;,,1 Average:

Time {sec~ 53, ",,'55:·:,', '.", ···~51 53

. -

...

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +/- 5 percent of span. Drift cannot exceed +1-3 percent of span
Inllial Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift,

Response, Response, Cal. Bias Response, Cal. Bias Percent of 10/25/2007 PPM PPM % of Span PPM % of Soan soan Zero Gas 0.0 0.00% .f'!'c":CO.O"c,,,-,,;, 0.00% 0.00% Upscale Gas 5.0 

# m 0.00% I,·,',',',; -1.11% -1.11% 10126/2007 Zero Gas 0.0 0.0 0.00% 

## ,\1 -2.22% 

## I -2.22% Upscale Gas 5.0 4.9 -1.11% 1_"· :::'.,-4;\1,",:,,-, -1.11% 0.00% 10/27/2007 Zero Gas 0.0 -0.2 -2.22% .~'C·U;",:,,··-.-I -2.22% 0.00% Upscale Gas 5.0 4.9 -1.11% 1>:;::<',,';,5' "",":"\~

## I 0.00% 1.11% 10/26/2007 Zero Gas 0.0 -0.2 -2.22% '.';'.;';:'0.2 

## ':,'1 -2.22% 0.00% Uoscale Gas 5.0 5.0 0.00% ":'4.9\1 -1.11% -1.11% 10/29/2007 Zero Gas 0.0 -0.2 -2.22% '<·"~0;2 

## " ~:I -2.22% 0.00% Upscale Gas 5.0 4.9 -1.11% l~t~;4;9 I -1.11% 0.00% 10/30/2007 Zero Gas 0.0 -0.2 -2.22% ',':' :'"0.2 

## '1 -2.22% 0.00% Upscale Gas 5.0 4.9 -1.11% '~";:,·A.6 -2.22% -1.11% 10/31/2007 Zero Gas -2.22% I"L:JJ~O,' ,..:,.~~c -1.11% 1.11% 0.0 -0.2 Uoscale Gas 5.0 4.6 -2.22% ·.c

### 4JI;cel -2.22% 0.00% 10/31/07 PM Zero Gas 0.0 -0.1 -1.11% 1",0"', 

## -,.r,\t.,1 -2.22% -1.11% Upscale Gas 5.0 4.8 -2.22% Ic,~,c.:''';!1' -1.11% 1.11% 1111/2007 Zero Gas 0.0 -0.2 -2.22% 

## Icx+-;"il'i~"T:1 -2.22% 0.00% Upscale Gas 5.0 4.9 -1.11% l'r'~'::"""';;;"C ''''''''1 -2.22% -1.11% 111212007 Zero Gas 0.0 . -0.2 -2.22% ·0.2 -2.22% 0.00% Upscale Gas 5.0 4.8 -2.22% 4.9 -1.11% 1.11% System Calibration BIas

### = (System Cal. Response - Analyzer Cal. Response) ISpan) x 100 Drift '" {(Final Syslem Cal. Response - Initial System Cal Response) ISpan) x 100 800 815

C02

# BARR EPA METHOD 7E ANALYZER CALIBRATION Engineering Company Project Sample Loc. Date Operators Hibbing Taconite Une 2 (SV025) 10/24-111212007 PJR Cvllnder Serial No. Certified Value Cal. Anal. 300CLD CA-NOx-2 Zero Gas CC126306 0 513 ppm Mld-rance SA15839 47.5 Hlah-ranue SA10103 124.9 Upper-range CC7380 513 

### TYU Anatyzer Modell SN Analyzer Range (span) Stripchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +/- 2 percent of span Cylinder Analyzer Absolute Difference, Test Runs: _1_-.....1Q... Value Calibration Difference % of Span Response Zero Gas 0 0 0 0.00% Mld-raae 47.5 0 47.5 9.26% Hiah-ranne: 124.9 123.6 1.3 0.25% Upper-range: 513 514 1 0.19% PRETEST RESPONSE TIME Note: Time to register 95% stepchange with high level gas. 

# I ~~f(;:~ 1~;;:"i'513c,:;.,•.• 

# J.:. :~;>525i,:',.,I, ""'5~·"i, •..,It--A:..ov;..;e5~r;r'gc:;;e:,--

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +/- 5 percent af span, Drift cannot exceed +l- 3 percent of span
Initial Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift,

Response, Response, Cal. Bias Response, Cal. Bias Percent of 10125/2007 PPM PPM % of soan PPM % of Span soan Zero Gas 0 I"'·.:.···.·.··::···():···.·.·.·;. 0.00% >:0.9 - 0.18% 0.18% Upscale Gas 123.6 

## -!i04c,j': 74.15% ··'"501;3

.. 73.63% -0.53% 1012612007 Zero Gas 0 0.9 0.18% 

### ,:,,-'- :ll:3 '..'.::....-'~

### 1 0.06% -0.12% Upscale Gas 123.6 124.9 0.25% ;';1.120)8 

# ·.ct -0.55% -0.80% 1012712007 Zero Gas 0 0.3 0.06% 

### .. 0.08% 0.02% Upscale Gas 252.3 245.7 -1;29% ,,,,.':244:SG;;:' -1.52% -0.23% 10/2812007 Zero Gas 0 0.4 0.08% 0.00% -0.08% 800 Upscale Gas 252.3 244.5 -1.52% 

# .";,',; -1.60% -0.08% 805 10/29/2007 Zero Gas 0 0.0 0.00% L~::<'--u;' -,'-'<' -0.02% -0.02% 815 Unseale Gas 252,3 244.1 -1.60% 

## i'~>243!5 

# -I -1.72% -0.12% 820 10130/2007 Zero Gas 0 -0.1 -0.02% 

### l~Lt6':$

# ',:,'1 0.12% 0.14% Unscale Gas 252.3 243.5 -1.72% :'-;'::<:243.1>-"1 -1.79% -0.08% 1013112007 Zero Gas 0 0.6 0.12% "'C- 

# .-~n 0.12% 0.00% Upscale Gas 252.3 243.1 -1.79% ·-242:5·.q -1.91% -0.12% 10/31/07 PM Zero Gas 0 0.6 0.12% <'""cO.~o 0.08% -0.04% Upscale Gas 252.3 242.5 -1.91% '243.6 -1.70% 0.21% 11/112007 Zero Gas 0 0.4 0.08% ;'-S:';0~6> 

# I 0.12% 0.04% Unscala Gas 252.3 243.6 -1.70% " "243.3 

# 'I -1.75% -0.06% 11/212007 Zero Gas 0 0.6 0.12% , C~-'_"CI 0.14% 0.02% Upscale Gas 252.3 

## I 243.3 -1.75% 

## :S~24z':9fic; -1.83% -0.08% System Calibration Bias

## = [(System Cal. Response - Analyzer Cal. Response) 1Span] x 100 Drift

## = ((Final System Cal. Response -Inftlal System Cal Response) ISpan] x 100

# BARR EPA METHOD 3A ANALYZER CALIBRATION (Oxygen) 

### Engineering Company Project Sample Loc. Date Operators Hibbing Taconite __ .....:1..:::0/c:;:2:::-4-,;.-11/212007 

### TYU Line 2 (SV026)
PJR Cylinder Serial No. Certified Value Cal. Anal. Model 200 I Zero Gas CC126306 0.0 21.5 % I Mid-range CA066B3 9.0 20cmfhr I Hiah-renne CC12009 21.5 Analyzer Modell SN Analyzer Range (span) Stripchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +/- 2 percent or span Cylinder Analyzer Absolute Difference, Test Runs: _1_ 

# - .J! Value Calibration Difference % or Span Response Zero Gas 0.0 0.1 0.1 0.46% Mid·rage 9.0 9.0 0.0 0.00% Hloh-ranoe: 21.5 21.5 0.0 0.19%

PRETEST RESPONSE TIME Note: Time to regIster 95% stepchange with hIgh level gas.

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bIas cannot exceed +1-5 percent of span. Drift cannot exceed +/- 3 percent of span
InlUal Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift, Response, Response, Cal. 81as Response, Cal. Bias Percent of 10/25/2007 PPM PPM % of Soan PPM % or Soan soan Zero Gas 0.1 ~,~ v.\i':c,;- -0.46% 

## ':i'0:0 - 

### ~ -0.46% 0.00% Upscale Gas 21.5 ::':.<'21'.:2/.':' -1.39% :':-~'21.2 " -1.39% 0.00% 10/26/2007 Zero Gas 0.1 0.0 -0.46% ;,,:',0.0 

# I -0.46% 0.00% Upscale Gas 21.5 21.2 -1.39% 

### /;,21;3; 

## ·'1 -0.93% 0.46% 10/27/2007 Zero Gas 0.1 0.0 -0.46% 

## ';,::::-1 -0,46% 0.00%

", Upscale Gas 21.5 21.3 -0.93% ;,\",",'21;4'.·.> -0.46% 0.46% 10/28/2007 Zero Gas 0.1 

## I 0.0 -0.46% :.' •..., -0,46% 0.00% Upscale Gas 21.5 21.4 -0.46% I·~±:-:"-.~",C' 7.;1 -1.39% -0.93% 10/29/2007 Zero Gas 0.1 0.0 -0.46% 1;"~.}20:0;~=,m -0.46% 0.00% Upscale Gas 21.5 21.2 -1.39% 

## P~c,;'- '.>;.:, -2.32% -0.93% 10/30/2007 Zero Gas 0.1 0.0 -0.46% 

### :;:;,rO:O_);! -0.46% 0.00% Upscale Gas 21.5 21.0 -2.32% 

# I' ..-'.'.- .' -2.79% -0,46% -20.9 10/31/2007 Zero Gas 0.1 0.0 -0.46% I:!d: 0.0 'j -0.46% 0.00% Upscale Gas 21.5 20.9 -2.79% 

### j- .. -:21,1_ ;. -1.86% 0.93% 10/31/07 PM Zero Gas 0.1 0.0 -0,46%

-- :0.0 " -0.46% 0.00% Upscale Gas 21.5 21.1 -1.85% ''''\21:2

- -.: -1.39% 0,45% 11/1/2007 Zero Gas 0.1 0.0 -0,46% '=-c::. ;;'0.0

. ~,. -0.46% 0.00% ,-- Upscale Gas 21.5 21.2 -1.39% 

### 21'.0 

## :: -2.32% -0.93% 11/212007 Zero Gas 0.1 0.0 -0,46% 0.0 -0.46% 0.00% Upscale Gas 21.5 21.0 -2.32% 

## I 21.1 -1.86% 0.46% System Calibration Bias

### = [(System Cal. Response - Analyzer Cal. Response) / Span) x 100 Drift '"(Final System Cal. Response -ln1llal System Cal Response) / Span) x 100 02

# BARR EPA METHOD 3A ANALYZER CALIBRATION (Carbon DIoxIde) 

### Engineering Company Project Sample Loc. Date Operators Hibbing Tacon1!e __ ....;1:..=0=-=/2~4-..,;.11/2/2007 

### TYU Line 2 (SV026)
PJR Cylinder Serial No. Certified Value Cal. Anal. Model 200 

### I Zero Gas CC126306 0.0 9.0 % 

### I Mld·range CC12009 5.0 N1A I Hlah-ranae CA06683 9.0 Analyzer Modell SN Analyzer Range (span) Stripchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +/- 2 percent of span Cylinder Analyzer Absolute Difference, Test Runs: _1_ 

## - ...llL Value Calibration Difference % of Span ResDonse Zero Gas 0.0 0.0 0.0 0.00% Mld-raoe 5.0 5.1 0.1 0.67% High-range: 9.0 9.0 0.0 0.00%

PRETEST RESPONSE TIME Note: Time to register 95% stepchange with high level gas.

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +/- 5 percent of span. Drift cannot exceed +1- 3 percent of span
Inillal Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift,

Response, Response, Cal. Bias Response, Cal. Bias Percent of 10/25/2007 PPM PPM % of Soan PPM % of Soan soan Zero Gas 0.0 -3.33% \':·:-0;1···· 

### ......• -1.11% 2.22% Upscale Gas 5.1 

### .......... -3.33% ,'/,' '5.0
....." -1.11% 2.22% 10126/2007 Zero Gas 0.0 -0.1 -1.11% . , ';-0.2 -2.22% -1.11% Upscale Gas 5J 5.0 -1.11% 4.9 

## 1 -2.22% -1.11% 10/2712007 Zero Gas 0.0 -0.2 -2.22%

' . 

### :43 -3.33% -1.11% Uoscale Gas 5.1 4.9 -2.22% 

### .····"4.9 -2.22% 0.00% 10/2812007 Zero Gas 0.0 -0.3 -3.33% 

## ,r-'-·::~O:2-\.;1 -2.22% 1.11% Upscale Gas 5.1 4.9 -2.22% ,'/"4,8,":-:1 -3.33% -1.11% 10129/2007 Zero Gas 0.0 -0.2 -2.22% ~'>:I -3.33% -1.11% Upscale Gas 5.1 4.8 -3.33% ,"<:-iic:1 -3.33% 0.00% 10/30/2007 Zero Gas 0.0 -0.3 -3.33% 

### ...'.,

## .. 

## .,., -1.11% 2.22% Upscale Gas 5.1 4.8 -3.33% -2.22% 1.11% 10/31/2007 Zero Gas 0.0 -0.1 -1.11% 

## ~"'·~~b.3:.·;1 -3.33% 

## I -2.22% Upscale Gas 5.1 4.9 -2.22% 

### I'c\> 4.8 '

### ~::::"A -3.33% -1.11% 10/31/07 PM Zero Gas 0.0 -0.3 -3.33% ·\~6.2.<~:I -2.22% 1.11% Uoscale Gas 5.1 4.8 

## I -3.33% 1';-':;+4.8.";1 -3.33% 0.00% 11/1/2007 Zero Gas 0.0 -0.2 -2.22% 

### I·' ":;>-0.2 

## ·····d -2.22% 0.00% Uoscale Gas 5.1 4.8 -3.33% 

### I " 

## "4.8· 

# :1 -3.33% 0.00% -." 11/212007 Zero Gas 0.0 ·0.2 -2.22% 0.0 0.00% 2.22% Upscale Gas 5.1 4.8 -3.33% 4.9 -2.22% 1.11% System Callbrallon Bias = [(System Cal. Response - Analyzer Cal. Response) / Span) x 100 Drift

### =[(Final System Cal. Response -Initial System Cal Response) / Span) x 100 C02

# BARR EPA METHOD 7E ANALYZER CALIBRATION Engineering Company Project Sample Loc. Dale Operators Hibbing Taconite Line 2 (SV026) __ -,1~0!!;/2~4-:..!.11/212007 

### TYUPJR Cvlinder Serial No. Certified Value Cal. Anal. 300CLD CA·NOx-2 Zero Gas CC126306 0 513 ppm Mld-ranae SA15639 124.9 Hiah·ranoe SA10103 252.3 

### uoner-ranne CC7380 513 Analyzer Modell SN Analyzer Range (span) Slrlpchart Speed (unl!s): ANALYZER CALIBRATION DATA Nole: Difference must be less than +1- 2 percent of span Cylinder Analyzer Absolute Difference, Tes! Runs: _1_" 

### ...JQ... Value Calibration Difference % of Span Resoonse Zero Gas 0 0.1 0.1 0.02% Mld-raoe 124.9 123.5 1.4 0.27% Hloh-ranoe: 252.3 248.8 3.5 0.68% Upper-range: 513 513.6 0.6 0.12% PRETEST RESPONSE TIME Note: Time to register 95% stepchange with high level gas.

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias canna! exceed +/- 5 percent of span. Drift cannot exceed +1" 3 percent of span
Initial Values Final Values Analyzer Cal System Cal System Cal Sys!emCal SyslemCal Drift, Response, Response, Cal. Bias Response, Cal. Bias Percent of 10/25/2007 PPM PPM % of Span PPM % of Soan soan Zero Gas 0.1 0.14% 0.18% 0.04% Upscale Gas 123.5 -' 

# •..~1~li.6',·'.,·:, -0.57% -0.60% -0.04% ."., 10/26/2007 Zero Gas 0.1 1.0 0.16% :'··'H·,· ec"';':' 0.18% 0.00% Upscale Gas 123.5 -0.60% '-~::~--~.,-:,-,:":-- .: :..-..~:- -0.99% 120.4 -:'"'::1,18.4 >,: -0.39% 10/2712007 Zero Gas 0.1 1.0 0.18% 

## :,:',:'db.a

## ic,\_: 0.14% -0.04% Upscale Gas 123.5 118.4 -0.99% 

### :'~'i-'cf1'7-.5'c:,; -1.17% ·0.16% 10/28/2007 Zero Gas 0.1 0.8 0.14% 

## I.:y.-::;"co····d 0.16% 0.02% 820 Upscale Gas 123.5 117.5 -1.17% '115:9 -1.48% ·0.31% 828 10/29/2007 Zero Gas 0.1 0.9 0.16% ·':>-'d.2 - 

## 1 0.21% 0.06% Upscale Gas 123.5 115.9 -1.48% 

## 1""·-116.0 -1.46% 0.02% 10/30/2007 Zero Gas 0.1 1.2 0.21% I \!;';;;,1.0. 0.18% -0.04% Upscale Gas 248.8 

## f;:jiti

# 23.4;8iJ$~; -2.73% 

### '·,·' .;:····-·'·-·-·:e~;1 -2.92% -0.19% ' (""'.233,8" 'c.", 10/31/2007 Zero Gas 0.1 1.0 0.18% ::;-;.2:6:3-'" 0.04% -0.14% Upscale Gas 248.8 233.8 -2.92% 

## 31/,ici

## 233;O -3.08% -0.16% 10/31/07 PM Zero Gas 0.1 0.3 0.04% kc 0.14% 0.10% Upscale Gas 248.8 233.0 -3.08% ;",;[,'235:3-;"::: -2.63% 0.45% 111112007 Zero Gas 0.1 0.8 0.14% 

### '~ 'I 0.14% 

## I 0.00% Upscale Gas 248.8 235.3 -2.63% -')'.234:9' ~, -2.71% -0.08% 1112/2007 Zero Gas 0.1 0.8 0.14%' - 

## "'-f~4~/1 0.25% 0.12% Upscale Gas 248.8 234.9 -2.71% 

### "-,,,'i235:0c<' -2.69% 0.02% System Calibration Bias - ((System Cal. Response - Analyzer Cal. Response) ISpan) x 100 Drift

### =[(Final System Cal. Response -Initial System Cal Response) ISpan) x 100

# BARR EPA METHOD 3A ANALYZER CALIBRATION (Oxygen) 

### Engineering Company Project Sample Loc. Date Operators Hibbing Taconlle Line 2 (SV027) __ ....:1c::;0/:.:;:2=-4.~11/212007 

### TYU Analyzer Modell SN Analyzer Range (span) Stripchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +/. 2 percent of span PJR Cvlinder Serial No. Certified Value Cal. Anal. Model 200 

### I Zero Gas CC126306 0.0 21.5 % I Mld·range CA06683 9.0 20 cmlhr I Hlah-ranae CC12009 21.5

Cylinder Analyzer Absolute Difference, Test Runs: _1_· 

### ....1.Q Value Calibration Difference % of Span Resoonse Zero Gas 0.0 0.0 0.0 0.00% Mid·rage 9.0 9.0 0.0 0.00% Hloh·ranoe: 21.5 21.6 0.1 0.28%

PRETEST RESPONSE TIME Note: Time to register 95% stepchange with high level gas.

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +1-5percent of span. Drift cannot exceed +1- 3 percent of span
InfUal Values Final Values Analyzer Cal System Cal Sys!emCal System Cal System Cal Drift, Response, Response, Cal. Bias Response, Cal. Bias Percent or 10/25/2007 PPM PPM % or Soan PPM % of Span span Zero Gas 0.0 

### ,>,,",' ","0"'," 0.00% 0.00% 0.00% Upscale Gas 21.6 1i'C"'C;,", ;;"",' -1.39% I"; -1.39% 0.00% 10/26/2007 Zero Gas 0.0 0.1 0.46% I",;:CC~;'L;',?~;I 0.46% 0.00% Uoscale Gas 21.6 21.3 -1.39% ~':{2{4" 

## "A -0.93% 0.46% 10/27/2007 Zero Gas 0.0 0.1 0.46% 1:;':0.0',' ii 0.00% ·0.46% Upscale Gas 21.6 21.4 -0.93% ~'':;-:21.5 ." ~. -0.46% 0.46% 10/28/2007 Zero Gas 0.0 0.0 0.00% -':-.-'~: ,"'0:0 -I 0.00% 0.00% Uoscale Gas 21.6 21.5 -0.46% ,:',{21:3 "

" -1.39% -0.93% 10/29/2007 Zero Gas 0.0 0.0 0.00% :;,0.,1 >' 0.46% 0.46% Upscale Gas 21.6 21.3 -1.39% 

### ";::-':2t1'

-- -- -2.32% -0.93% 10/30/2007 Zero Gas 0.0 0.1 0.46% L~':;;0;1~;:~ 0.46% 

## I 0.00% Upscale Gas 21.6 21.1 -2.32% k'-:":, -2.32% 

## I 0.00% 10/3112007 Zero Gas 0.0 0.1 0.46% 

# qrc;o.o:':'1 0.00% -0.46% Upscale Gas 21.6 21.1 -2.32% ;',''--2(2 :.0,--••. -1.86% 0.46% .-." 10/31f07 PM Zero Gas 0.0 0.0 0.00% 0.00% 0.00% Upscale Gas 21.6 21.2 -1.86% -1.39% 0.46% 11/1/2007 Zero Gas 0.0 0.0 0.00% n,:,,~;o.O-:;;;d 0.00% 0.00% Upscale Gas 21.6 21.3 -1.39% ,"! -2.32% -0.93% 11/212007 Zero Gas 0.0 0.0 0.00% 0.0 0.00% 0.00% Upscale Gas 21.6 21.1 -2.32% 21.3 -1.39% 0.93% System Calibration Blaa= ({System Cal. Response - Analyzer Cal. Response) ISpan} x 100 Drift '" {(Final System Cal. Response -Initial System Cal Response) ISpan) x 100 850 856

02

# BARR EPA METHOD 3A ANALYZER CALIBRATION (Carbon Dioxide) Engineering Company Project Sample Loc. Date Operators Hibbing Taconite LIne 2 (SV027) __ ...;1:.:;;0:.:;12::;.4-..,;..11/212007 

### TYUPJR Cvlinder Serial No. Certified Value Cal. Anal. Model 200 I Zero Gas CC126306 0.0 9.0 % 

### I Mid-range CC12009 5.0 NIA I Hich-rance CA06683 9.0 Analyzer Modell SN Analyzer Range (span) Stripchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +1-2 percent of span Cylinder Analyzer Absolute Difference, Test Runs: _1_- ...1Q... Value Calibration Difference % of Span ResDonse Zero Gas 0.0 0.0 0.0 0.00% Mld·raae 5.0 5.1 0.1 0.67% Hlch·ranae: 9.0 9.1 0.1 1.11%

PRETEST RESPONSE TIME Note: TIme to register 95% stepchange with high level gas.

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +1-5percent of span. Drift cannot exceed +1-3 percent of span
Inlt1alValues Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift, Response, Response, Cal. Bias Response, Cal. Bias Percent of 10/25/2007 PPM PPM %

### otsoan PPM %

### ctsean SDan

... .~-~.-. "0.'1 }, Zero Gas 0.0 . ",:,0.0''':'''.' 0.00% 1.11% 1.11% Uoscale Gas 5.1 

### 1 

### "S5~(j·;·i -1.11% 

### c.\ "5.0 .:,: -1.11% 0.00% 10/26/2007 Zero Gas 0.0 0.0 0.00% I;iX,":lj'1' ,'6"1 1.11% 1.11% unscale Gas 5.1 5.0 -1.11% C""~,4;~ , .•, ""'I -2.22% -1.11% 10/27/2007 Zero Gas 0.0 0.1 1.11% '.',·.,u;l.c-·~':.rc-,I -2.22% -3.33% Uoscale Gas 5.1 4.9 -2.22% 1""':··:"_'4;~-·":"':',::i1 -2.22% 0.00% 10/28/2007 Zero Gas 0.0 -0.2 -2.22% 

## ,"'i'I -2.22% 0.00% Uoscale Gas 5.1 4.9 -2.22% Je: ':A 

# ~/'~11 -2.22% 0.00% 10/29/2007 Zero Gas 0.0 -0.2 -2.22% I:'ij:cc"u.",_'~"': ,'I -2.22% 0.00% Uoscale Gas 5.1 4.9 -2.22% 'r~;C:t\t'-8'

# -':"1 -3.33% -1.11% 10/3012007 Zero Gas 0.0 -0.2 -2.22% h''['co.2 '.': I -2.22% 0.00% Uoscale Gas 5.1 4.8 -3.33% 

### 1~"iC-:('4.8':,rl -3.33% 0.00% 10/31/2007 Zero Gas 0.0 -0.2 -2.22% :',;:,::,'~()01" 

### ::'1 -1.11% 1.11% Uoscale Gas ,. -- -3.33% 5.1 4.8 -3.33%
.. , ',' 4.8 0.00% 10/31107 PM Zero Gas 0.0 -0.1 -1.11% .... ·'"0:1 0 -1.11% 0.00% Uoscale Gas 5.1 4.8 -3.33% ,::L;{9 -2.22% 1.11% 11/1/2007 Zero Gas 0.0 -0.1 -1.11% 

### IY'>:';~();2;,~d -2.22% -1.11% Upscale Gas 5.1 4.9 -2.22% 

## F~~:i'4:8;:'\ -3.33% -1.11% 11/212007 Zero Gas 0.0 ' -0.2 -2.22% 0.0 0.00% 2.22% Uoscale Gas 5.1 4.8 -3.33% 4.9 -2,22% 1.11%



# - 850 856

System Calibration Bias - ({System Cal. Response - Analyzer Cal. Response) ISpan) x 100 Drift:; ((Final System Cal. Response - Initial System Cal Response) ISpan] x 100 C02

# BARR EPA METHOD 7E ANALYZER CALIBRATION Engineering Company Project Sample Lac. Date Operators Hibbing Taconite __ ....:1",,0/:.:;:2:::-4-,;.-1112/2007 TYU LIne 2 (SV027)
PJR Cvllnder Serlal No. Certified Value Cal. Anal. 300CLD CA·NOx-2 Zero Gas CC126306 0 513 ppm Mld·range SA15839 47.5 HiClh·ranCle SA10103 124.9 Upper-range CC73BO 513 Analyzer Model ISN Analyzer Range (span) Strlpchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +/. 2 percent of span Cylinder Analyzer Absolute Difference, Test Runs: _1_ 

# - .n, Value Calibration Difference % of Span Response Zero Gas 0 0 0 0.00% Mld·raCle 47.5 44.3 3.2 0.62% High-range: 124.9 118 6.9 1.35% Upper-range: 513 511.5 1.5 0.29% PRETEST RESPONSE TIME Note: Time to regIster 95% stepchange with high level gas. 

# I ~~:(;:~ 1;:,+,c"5\,,~~,I~'''''~'':6i±'c'c,I·''-<'85~'i:,;"I Average: 54

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +1-5 percent or span, Drlft cannot exceed +f- 3 percent of span
Initial Values FInal Values Analyzer Cal System Cal System Cal System Cal System Cal Drlft,

Response, Response, Cal. Bias Response, Cal. Bias Percent of 10/25/2007 PPM PPM % of Span PPM % of Soan span Zero Gas 0 .ce:,'. 0.16% J -0.25% ·0.41% Upscale Gas 118 

## ~11a.1:'o;c -0.25% -'ic

## 'J13.e .-:~ ·0.86% ·0.60% 1012612007 Zero Gas 0 2.2 0.43% <0.9 -0.16% ·0.60% Upscale Gas 118 114.7 -0.64% 

## '115.4 'c': -0.51% 0.14% 10/27/2007 Zero Gas 0 ·0.9 -0.18% 

## :>:,:1 -0.21% -0.04% Upscale Gas 118 115.4 -0.51% 

### ;;i.11"1'4:9-:,{yfi -0.60% -0.10% 10/2812007 Zero Gas 0 -1.1 ·0.21% '··c·'] -0.19% 0.02% Upscale Gas 118 114.9 ·0.60% " ."t; ·0.37% 0.23% 1012912007 Zero Gas 0 -1.0 ·0.19% -0.06% 0.14% 850 Upscale Gas 118 116.1 -0.37% 

## "~~:J21~4"i'¥J 0.66% 1.03% 854 10/30/2007 Zero Gas 0 -0.3 -0.06% ·0.14% -0.08% Upscale Gas 118 121.4 0.66% ~~<.'124.5: 1.27% 0.60% 10/31/2007 Zero Gas 0 -0.7 -0.14% 

## ;'1 -0.02% 0.12% 

## lI':;~;1"·. Upscale Gas 118 124.5 1.27% 18;6· 0.12% -1.15% 10/31/07 PM Zero Gas 0 -0.1 -0.02% 7":':·-:0.2~"" - -0.04% ·0.02% Upscale Gas 118 118.6 0.12% ;'.:.: 'J17.8 

## <'el -0.04% -0.16% 1111/2007 Zero Gas 0 -0.2 -0.04% ":T~1;1 ~'i .: 0.21% 0.25% Upscale Gas 118 117.6 -0.04% I· ...·· ..·· 0.12% 0.16% I ,~118.6 .-::, 11/212007 Zero Gas 0 1.1 0.21% •.:'''c,0.6 0.16% -0.06% Upscale Gas 118 118.6 0.12% "".,:,~114;4,:::"= -0.70% -0.82% System Calibration Bias

# = (System Cal. Response - Analyzer Cal. Response) / Span} x 100 Drlft

# = (Final System Cal. Response - Initial System Cal Response) ISpan] x 100

# BARR EPA METHOD 3A 

### ANALYZER CALIBRA liON (Oxygen) 

### Engineering Company Project Sample loco Date Operators Hibbing Taconite __ -=',-=,0/:.::;2,.:..4-.,:..11/2/2007 

### TYU line 2 (SV028)
PJR Cylinder Serial No. Certified Value Cal. Anal. Model 200 f Zero Gas CC126306 0.0 21.5 % f Mid-range CA066B3 9.0 20 cmlhr f H1Qh-ranlle CC12009 21.5 Analyzer Model/ SN Analyzer Range (span) Strlpchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +/- 2 percent of span Cylinder AnalYi:er Absolute Difference, Tesl Runs: _1_- 

### -11 Value Calibrallon Difference % of Span Response Zero Gas 0.0 0.3 0.3 1.39% Mld-raae 9.0 9.0 0.0 0.00% Hloh-ranae: 21.5 21.5 0.0 0.19%

PRETEST RESPONSE TIME Nole: Time to register 95% stepchange with high level gas.

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +/- 5 percent of span. Drift cannot exceed +/- 3 percent of span
Inillal Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift,

Response, Response, Cal. Bias Response, Cal. Bias Percent of 10/25/2007 PPM PPM % of Span PPM % of Span span Zero Gas 0.3 -1.39% T' 

### '-6;(j " -1.39% 0.00% Uoscale Gas 21.5 ' ',...:

..~_ ..'21:3-;7.'- -0.93% 21:4' .': -0.46% ::_~:"-,. . -,

### ~ 0.46% 10/26/2007 Zero Gas 0.3 0.0 -1.39% 

### . "':j):O".' -1.39% 0.00% Uoscale Gas 21.5 21.4 -0.46% 1"7 21.5 0.00% 0.46% 10/27/2007 Zero Gas 

## I 0.3 0.0 -1.39% ". :--0;0 

# ;1 -1.39% 0.00% Upscale Gas 

# I 21.5 21.5 

### I 0.00% Ic';,, .j; 

## ;;1 -0.46% 

# I -0.46% 10/28/2007 Zero Gas 0.3 0.0 -1.39% 

### I

## (flL6:0\,\·J -1.39% 0.00% Uoscale Gas 21.5 21.4 -0.46% 

# '.',;." ·····'01 -0.93% -0.46% ,.,,"·,,·.,21,3' 10/29/2007 Zero Gas 0.3 

### I 0.0 -1.39% cc",-n' .',.';-;;"1 -1.39% 0.00% Upscale Gas 21.5 21.3 

## I -0.93% I"'++,,'Z .Z.i"'.C-,·" -1.39% -0.46% 10/30/2007 Zero Gas 0.3 0.0 -1.39% :'~.';O:(j'

.. - -1.39% 0.00% Uoscale Gas 21.5 21.2 -1.39% -1.86% -0.46% 10/31/2007 Zero Gas 0.3 0.0 -1.39% 

## f-=£io;,1':"1 -0.93% 0.46% Upscale Gas 21.5 21.1 -1.86% ~..:\-::;'21~3 .•,.-. -0.93% 0.93% 10/31/2007 Zero Gas 0.3 0.1 -0.93% 

# 1-",- 0.1 -0.93% 0.00% Uoscale Gas 21.5 21.3 -0.93% ,.,,::.,". 21.2 

## :1 -1.39% -0.46% ;"

-~ ".. 11/1/2007 Zero Gas 0.3 0.1 -0.93% 

### I'e: "0.2 

# . , -0.46% 0.46% UDscale Gas 21.5 21.2 -1.39% ;,21:2
..... -1.39% 0.00% 11/212007 Zero Gas 0.3 0.2 -0.46% 0.2 -0.46% 

## I 0.00% Upscale Gas 21.5 21.2 

## I -1.39% 

## I 21.2 -1.39% 0.00% System Calibration Blas «({System Cal. Response - Analyzer Cal. Response) ISpan) x 100 Drift '" ((Final System Cal. Response - Initial System Cal Response) ISpan] x 100 

### 02

# BARR EPA METHOD 3A ANALYZER CALIBRATION (Carbon Dioxide) Engineering Company Project Sample lac. Date Operators Hibbing Taconite Une 2 (SV028) 10/24-11/2/2007 PJR Cvlinder Serial No. Certified Value Cal. Anal. Model 200 I Zero Gas CC126306 0.0 9.0 % 

### I Mid-ranue CC12009 5.0 N1A I High-range CA066B3 9.0 

### TYU Analyzer Modell SN Analyzer Range (span) Stripchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +/- 2 percent of span Cylinder Analyzer Absolute Difference, Test Runs: _1_ 

## - ...llL Value Calibration Difference % of Span Response Zero Gas 0.0 0.0 0.0 0.00% Mld-raae 5.0 5.0 0.0 0.44% High-range: 9.0 9.0 0.0 0.00%

PRETEST RESPONSE TIME Note: Time to register 95% stepchange with high level gas.
I ~~s;(~:~) k:.,Cj:5~~ .. (:.k""':f''''523." •••

# ,I,~~~...,~." _c"I-----'Ac.:.v:.:;e5,;.,;r;"'g.=.;e:'---'

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +/- 5 percent of span. Drift cannot exceed +/- 3 percent of span
Initial Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift,

Response, Response, Cal. Bias Response, Cal. Bias Percent of 1012512007 PPM PPM % of Soan PPM % of Soan soan Zero Gas 0.0 -: 0.00% _.:, I 

## <"".> 0.00% 0.00% Uoscale Gas 5.0 -"'U.~'. c' 0.00% 1';''-'''' 0.00% 0.00% 10126/2007 Zero Gas 0.0 0.0 0.00% 

### ' c:,hH),2 ...•.. -2.22% -2.22% :-..'. Upscale Gas 5.0 5.0 

## 1 0.00% 

### '" ';4.9,' 

## "1 -1.11% -1.11% 1012712007 Zero Gas 

## I 0.0 -0.2 -2.22% 

## I'C.'--~(li3 ':1 -3.33% -1.11% Upscale Gas 5.0 4.9 -1.11% 1"-4.9 .1 -1.11% 0.00% 1012812007 Zero Gas 0.0 -0.3 -3.33% I;, <0.2 

## ;1 -2.22% 1.11% Upscale Gas 5.0 4.9 -1.11% ·'.4.sH -2.22% -1.11% 1012912007 Zero Gas 0.0 -0.2 -2.22% 1"~;-_'-0.2!·':-j;1 -2.22% 0.00% Upscale Gas 5.0 4.8 -2.22% .c',','-"" -2.22% 0.00% - ;1 10/3012007 Zero Gas 

### 1:22=:];''),. 

### cl -2.22% 0.0 -0.2 -2.22% 0.00% Upscale Gas 5.0 4.8 -2.22% -2.22% 0.00% 10/31/2007 Zero Gas 0.0 -0.2 -2.22% 

### h>:'c .. cn'.,' :...,,] -2.22% 0.00% Upscale Gas 5.0 4.8 -2.22% 

## k'",,~--'.;:=,-=, -2.22% 0.00% 10/31/07 PM Zero Gas 0.0 -0.2 -2.22% 

## -,,'. ,eI -3.33% -1.11% Upscale Gas 5.0 4.8 -2.22% ,"'~'.': ' .:;:~';,'I -2.22% 0.00% 11/1/2007 Zero Gas 0.0 -0.3 -3.33% F- ,~0.3' ~'i -3.33% 0.00% Upscale Gas 5.0 4.8 -2.22% "4.7 -3.33% -1.11% 11/212007 Zero Gas 0.0 -0.3 -3.33% -0.3 -3.33% 0.00% Upscale Gas 5.0 4.7 -3.33% 4.7 -3.33% 0.00% System Callbralfon Bias

## = [(System Cal. Response - Analyzer Cal. Response) ISpan) x 100 Drift

# = [(Final System Cal. Response - Inilial System Cal Response)' Span) x 100 C02

# BARR EPA METHOD 7E ANALYZER CALIBRATION 

### Engineering Company Project Sample Loc. Dale Operators Hibbing Taconite line 2 (SV028) 10/24-11/212007 

### TYU Analyzer Modell SN Analyzer Range (span) Strlpchart Speed (units): ANALYZER CALIBRATION DATA Note: Difference must be less than +1-2 percent of span PJR Cvlinder Serial No. Certified Value Cal. Anal. 300CLD CA-NOx-2 Zero Gas CC126306 0 513 ppm Mid-range SA15839 47.5 Hloh-ranos SA10103 124.9 Unpar-ranqe CC73BO 513

Cylinder Analyzer Absolute Difference, Test Runs: _1_- 

### ...1Q... Value Callbrallon Difference % of Span Resoonse Zero Gas 0 0.5 0.5 0.10% Mld-raoe 47.5 47.4 0.1 0.02% Hlgh-ranoe: 124.9 123.3 1.6 0.31% UDPer-range: 513 502 11 2.14% PRETEST RESPONSE TIME Note: Time 10register 95% stepchange with high level gas. 3 Average: 52 52

SYSTEM CALIBRATION BIAS AND DRIFT DATA: Note: System Cal bias cannot exceed +1- 5 percent of span. Drift cannot exceed +1- 3 percent of span
Initial Values Final Values Analyzer Cal System Cal System Cal System Cal System Cal Drift, Response, Response, Cal. Bias Response, Cal. Bias Percent of 10/25/2007 PPM PPM % ot snan PPM % of Span span Zero Gas 0.5 0.02% I""'~", 0.02% 0.00% Uoscale Gas 47.4 0.12% 0.04% -0.06% 10/2612007 Zero Gas 0.02% 

### ,"" ','I 0.16% 0.5 0.6 r ,,'C' -I 0.14% Uoscale Gas 47.4 47.6 0.04% 

# },I -0.25% -0.29% 10/2712007 Zero Gas 0.5 1.3 0.16% ~':',~:0;6 

# ;:::1 0.02% -0.14% Uoscale Gas 47.4 46.1 -0.25% 

# ),~,':45:2',"d:: ·0.43% ·0.18% 10128/2007 Zero Gas 0.5 0.6 0.02% F"c"='" :,',::.:1 0.10% 0.06% Uoseale Gas 47.4 45.2 -0.43% '<~'45:1~'}1 -0.45% ·0.02% 10/29/2007 Zero Gas 0.5 1.0 0.10% I:,' 

## c." 0.14% 0.04% Uoscale Gas 47.4 45.1 -0.45% 

### "~'-45.1

# -:'.'~,! -0.45% 0.00% 10/30/2007 Zero Gas 0.5 1.2 0.14% ISC,f.,.1.1 .S 0.12% ·0.02% Uoscale Gas 

## ~'tf,t1&O~~~I ,0", ' • .". ,:.';c~~-',_'. 

# 'I -1.58% 123.3 -1.62% ,,·,115.2 0.04% 10/31/2007 Zero Gas 0.12% ,':cc', ·c 0.25% 0.14% 0.5 1.1 Uoseale Gas 123.3 115.2 -1.58% :'-:'-'Jl5.0; 

### ~ ".:.' -1.62% -0.04% 10/31/07 PM Zero Gas 0.5 1.8 0.25% I~£'{,,~{.f.o::•.

### q 0.27% 0.02% Uoseale Gas 123.3 115.0 -1.62% -1.52% 0.10% 11/1/2007 Zero Gas 0.5 1.9 0.27% 0.21% -0.06% Uoseale Gas 123.3 115.5 -1.52% ~:"", ;"'A~>' :;- -1.54% -0.02% 11/2/2007 Zero Gas 0.5 1.6 0.21% :,:'.~·2;8'·' 0.45% 0.23% Upscale Gas 123.3 115.4 -1.54% 

## :·::;"'~f113;6"t'k' -1.89% -0.35% System Calibration Bias

# = (System Cal. Response - Analyzer Cal. Response) ISpan) x 100 Drift

# = (FInal System Cal. Response - Initial System Cal Response) ISpan) x 100

# •• BARR S-Type Pitot Tube Geometry Check
Pitot Tube Number: 

# '6 - d-. 

# "'l..' Length: oJ Functlon:~ 

### I Free

1. Are faceopenings perpendicular to tuba axis? ~ES ( 90to 2) 

### 0 NO (go 101a) 

# ~ ffi

~- -~:---~--~-- 

# -------
, r_ 

# r--~" I

2
v •Are face openings paraael Io longitudinal axis? 

### ...g(YES ( go to 3) 

### 0 NO(go \02a)

.!-~ 3. Are legs

# orequallenglh? <> ~ YES (90to4) "~ 

### 0 NO (go to 3a)

I

4. Are center-finGs oflegs coJnc~nl? ~YES (go 106) 

### 0 NO(goto 4a)

6. Does Ihls pilOllube pass allorthe above criteria?



# --

Reviewed by:

•• O'°c".t ->.'~. 

### 'Inspection Date: 

# i-,I~o}- Technlcian.: 

## T_t(_L~ _

1a. IfN9, Is angle !ess\han 10'? DYES ( goto 2)



# =--~-~.

I - 

### I

2a. "NO, is angle less Ihan 6"'1 DYES (go Lo3) 

# o NO (discontinue use)



### ~ 

## .. __ I -:_ _,"",:_1 __ ~ 

### ! - .



# o NO (disconllnue usa) 

# ----3~·- : 

# --
•••_-- - I~

38. IfNO, Isdlfference less than 1/8inch? 

### EJYES ( go to 4) 

### 0 NO{discontinue usa}

-f- .":..: 

# --,,·t.-:..

# ;~y(

4a. IfNO. are centBr-llnes of tace openings less Ihan 1/321nch1 

# oYES (go to 6) 

### 0 NO(discoollnue usa)

DYES DNO 

# .•.

# THERMOCOUPLE CALIBRATION 

# BARR

Cal Date: 

### THERMOCOUPLE 10 TC3-2 1/9/2007 

### M-5 Probe CALIBRATION TECHNICIAN: TYL REFERENCE STANDARDS TRACEABILITY Hart Scientific 9103·AsInA1B289 Report No. A1B0718 Hart Scientific 9140sInA1BOB6 Report No. A1B2024 

### Temperature Calibration Points 32 212 Reference Oeg F (To) 32 212 Probe Temp (deg F) 32 208 Reference Temp (deg R) deg

### F+460 492 672 Probe Temp (degR), deg F

### +460 492 668 Difference (degrees) 0 

### 4 % Diff Abs. T 0.0% 0.6% Is difference less than 1.5% at all measured points? YES DATE LABORATORY 12/15/2005 Hart Scientific 12/15/2005 Hart Scientific 

## 400 650 Ambient 400 650 70 392 639 69 860 1110 530 852 1099 529

8 11 1 0.9% 1.0% 0.2%



## THERMOCOUPLE CALIBRATION 1700 1600 1500 ~ 1400 

## .., ~ 1300 ::l 

### ~ 1200 ~ 1100 

# § 1000 D. ::l 

### 900 

## 8 

# s 800 tJ: 

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


### Are extrapolated limits less than 1.5%? YES FAHRENHEIT CALIBRATION RANGE 1500 -20 1200 If not acceptable, describe corrective action: Tchnician signature 

# S,...." rifJ~ QA signature ~ 

# C. 1..«

# •• BARR S·Type Pltot Tube Geometry Check Pilot Tube Number: 

# .3:- \ 

# e Length: Funclion: M-5 :robe Free

1. he face openlngs perpendlcul.ar 10l~beaxis? ~ES(~90102) DNO(goto1a} 7"*Jm.

. 

# ~- --~---h----~-- ~-~---

. 

# -- I .,~

2. Are face openings paraliel to longfiudinalaxis? 

# oYES (go 103) ~O [go102a}

3, Arelegs ofequBllenglh? DYES (90 104)

4. Are center-lines of legs coincident? 

# oYES ( 90to5) ~O (go to49)

5. Does this pltot tube pass ag oftheabove critella?
'Technlclan Signalurs' 

### InspectIon Dale: 

# l~ d-

# 'f - 0 ~ "\T' 

### Technlclan: 

### I

# t

# L

18. If NO, Is liIn9~ less than 10'1 

# oYES (goto 2)

II+; I 

# --~--. I I 

## , 

# .

2e. If NO, Isangle less than 5~? .JQ-¥ES (go to 3) 

# o NO (dIscontinueuse) 

# h-\t 

# --~--. I _ •



# o NO (discontinue use)



# - 

# - -f ~- 

# it:-e -~- . --- -= . ._--- .",." 

# "'- 

# ----3~·.: -i?-" -=- .• - ---- - '=-

3a. IfNO. Is difference less !han1/6inch? ~ES (go 104) 

### 0 NO(dlsconUnue use)
IV 

### -d __. 

# '- -f;-

4a. If NO, are center-lines offaceopenings less than 1/32Inch? ~ES (go to 5) 

### 0 NO(dlsCQntinuB use)

DNO

# • BARR THERMOCOUPLE CALIBRATION

THERMOCOUPLE ID Cal Date: 1/9/2007 

### CALIBRATION TECHNICIAN: REFERENCE STANDARDS TRACEABILITY DATE LABORATORY Hart Scientific 9103·A

### sin A1 8289 Report No. A1B0718 

### 12/15/2005 Hart Sclentlflc Hart Scientrflc 9140

### sin A18086 Report No. A1B2024 

### 12116/2005 Hart Scientific 

### Temperature Calibration Points 

### 32 212 

### 400 650 Ambient Reference Deg F (To) 32 212 400 650 70 Probe Temp (deg F) 31 212 394 651 69 Reference Temp (deg R) deg F

### +460 492 672 860 1110 530 Probe Temp (deg 

### R),deg 

### F+ 460 491 672 854 1111 529 Difference (degrees) 1 0 6 -1 1 % DiffAbs. 

### T 0.2% 0.0% 0.7% 0.1% 0.2% Is difference less than 1.5% at all measured points? YES

1700 1600 1500 

# t 1400 

## Ii 1300 

# i1200 ~ 1100 

# § 1000 l>. 

# 8 900
o 800 ~ 700 

### 600 500 400400 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700 REFERENCE TEMPERATURE, deg.R 500 

### TC3-1 M-5 Probe



## TYL

Are extrapolated limits less than 1.5%? YES FAHRENHEIT CALIBRATION RANGE -20 1200 If not acceptable, describe corrective action: Tchniclan signature QA signature

# •• BARR S·Typo 

### Pltot Tube Geometry Check PitotTube Number: 

# I../-l Lenglh: 

# _:1...•..'__ Function: @-S 

### Pro0 Free

1. Areface openings perpendicular to lube axis? 

### (gJ YES (go to2) 

### D NO(go 10 1a) 

### ~~ I



# ~- 

# --.'._-

.... ~--f

2. Are face openings parallel to longitudinal axis? 

### ii'IYES (go 103) 

### 0 NO (goto 2a)

3. Are legs ofequal lenglll? 

# iZI YES (go 104) 

# oNo (go to 311)

4. Ne center·lines of legs coIncident? 

## III YES (goto 6) 

## 0 NO(go104a) 

## -~f~---.....s---(--)-----

Technician Signature: 

### 1-(~-01 lnspecfion Dale: Technician::.........:....;:N~(S;::!;..~;;;:,....

_

1a. JfNO, !sangle less tha1l10'? 

# oYES (got02) 

# o NO(dlsconllnue use) 

# --~~ --.--~d -_.

~ ~

29. IfNO. Is angle less than 5~? 

# oYEOS(goto 3) 

# o NO (cnsconUoueuse)



# =

# 4: -I:. ..;~"' ._- "'..,- 

# 'fE: -

# 3:·~:;f'; 

# ----~~=-

311. ItNO, Isdiffereneeless than 1/8Inch? DYES ( go

# '04) 

### 0 NO (dlscontin~8 user
IV -E--- ~-.

48. 1/NO, ere cenler-lines of face opeolngsles$ than 1/32 Inch? DYES ( go 105) 

### 0 NO (dlsconllnue use)

BfYES ONO

# THERMOCOUPLE CALIBRATION 

# BARR

Cal Date: 

### THERMOCOUPLE 

## 10 TC4-1 1/10/2007 

## M-5 Probe CALIBRATION TECHNICIAN: TYL REFERENCE STANDARDS TRACEABILITY DATE LABORATORY Hart Scientific 91D3-Asin A18289 Report No. A1B0718 

### 12/15/2005 Hart Scientific Hart Scientific 9140sin A1B086 Report No. A1 

### 82024 

### 12/15/2005 Hart Scientific Temperature Calibration Points 

### 32 212 400 650 Ambient Reference Deg F (To) 32 212 400 650 

### 70 Probe Temp (deg F) 32 210 395 646 69 Reference Temp (deg R) deg 

### F

### +460 492 672 860 1110 530 Probe Temp (deg R), deg F 

### +460 492 670 855 1106 529 Difference (degrees) 0 2 5 

### 4 1 % Diff Abs. 

### T 0.0% 0.3% 0.6% 

### 0.4% 0.2% Is difference less than 1.5% at all measured points? 

### YES 

# THERMOCOUPLE CALIBRATION 1700 1600 1500 ~ 1400 'tI 

### ~ 1300 

# i1200 ~ 1100 ~ 1000



### ~ 

## 5 900 ~ 800 rt: 

### ~ 700 600 500 400

### 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700 REFERENCE TEMPERATURE, deg.R
Are extrapolated limits less than 1.5%? 

### FAHRENHEIT CALIBRATION RANGE -20 1200 

### YES
If not acceptable, describe corrective action: Tchnician signature QA signature 

# I

> 

# I

I
I 

# I I

1 

# I

I 

# I

# •• BARR S-Type Pltot Tube 

### Geometry Check
PlIot Tube Number: 

### Length: . '/ ( Function:~~ 

### Free

1. Aleface openings perpendicular 10lube axis? ~ES(90I02) 

### 0 NO (goto 160) '::.!":J! 

### 1 

# ! 

# ~-f--:--Xu: __~n_~_- i-c?:

# ----I

2. Ive face openings parallel to longitudinal axls? li;fYES ( 90 II;)3) 

### 0 NO (go to 2a)

3. Arelegs of equal length? 

## l8( YES(go to 4) 

# o NO (go 10360)

4. Ive center-tines of legs colnc1<;lenl? ~ES (go 105) 

### 0 NO (90 to 48) 

# ~----~~----<:;l-----

5. Does this pltot lube pass all of the e'pOve criteria? 

### .lnspacuon Date: 

# I-I< -0

# fTechnician: 

# ItL

1B. If NO, Is angle less than 10'7 

# o YES (go to2)



# ---~--.

1 - I

28. If NO, Is angle less than 6"J>? DYES ( go 103)



# - 

# - o NO' (disconUnue use) 

# rL ..J1 : 

# --~--. I , 

# . ,



# o NO (discontlnue use) 

# --I:

~ a -- 

# ·---Ok -

3a. If NO, Is difference lass than 1/8 Inch? DYES (goto4) 

## 0 NO (disconllnue use)

48. IfNO, BrB C(Jnler-llnas 01lace openings less than 1132 Inch? DYES {gotoo} 

### 0 NO (dlsconUnue use)

e{vES DNO

# THERMOCOUPLE CALIBRATION 

# BARR
THERMOCOUPLE 10 TC4-2 M-5 Probe TYL Cal Date: 1/9/2007 CALIBRATION TECHNICIAN: REFERENCE STANDARDS TRACEABILITY Hart Scientific 9103-AsIn A18289 Report No. A180718 Hart Scientific 9140sIn A1B086 Report No. A182024 

### Temperature Calibration Points 32 212 Reference Oeg F (To) 32 212 Probe Temp (deg F) 32 210 Reference Temp (deg R) deg F + 460 492 672 Probe Temp (deg R), deg F

### +460 492 670 Difference (degrees) 0 2 % Diff Abs. T 0.0% 0.3% Is difference less than 1.5% at all measured points? YES DATE LABORATORY 12/15/2005 Hart Scientific 12/15/2005 Hart Scientific 

### 400 

## 650 Ambient 400 650 70 398 650 69 860 1110 530 858 1110 529

2 0 

### 1 0.2% 0.0% 0.2%



# THERMOCOUPLE CALIBRATION 1700 

### 1600 1500 

### ~ 1400 .g 

## !:! 1300 

### ~ 1200 ~ 1100 ~ 1000 ..J 

# 8 900 o o 

### 800 ffi j!: 

### 700 600 

### 500 400

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

# I I

I 

# !

r 

# I 

# I : I
I 

# I 

# l

I 

# I I Are extrapolated limits less than 1.5%? YES FAHRENHEIT CALIBRATION RANGE 

### -20 1200 If not acceptable, describe corrective action: Tchnician signature QA signature

# • BARR THERMOCOUPLE CALIBRATION

Cal Date: 

### THERMOCOUPLE 10 T - 31 Handheld

AGA 

### 8/24/2007 CALIBRATION TECHNICIAN: REFERENCE STANDARDS TRACEABILITY Hart Scientific 9103·A sIn A18289 Report No. A1B0718 Hart Scientific 9140 sIn A1B086 Report No. A182024 

### Temperature Calibration Points 32 212 Reference Deg F (To) 32 212 Probe Temp (deg F) 32 212 Reference Temp (deg R) deg F

### +460 492 672 Probe Temp (deg R), deg F + 460 492 672 Difference (degrees) 0 0 % Diff Abs. T 0.0% 0.0% Is difference less than 1.5% at all measured points? YES DATE LABORATORY 

### 12115/2005 Hart Scientific 

### 12115/2005 Hart Scientific 

### 400 650 Ambient 400 650 70 398 647 70 860 1110 530 858 1107 530

2 3 0 0.2% 0.3% 0.0%

1700 1600 1500 

### ~ 1400


## .., ~ 1300 

### ~ 1200 ~ 1100 ~ 1000 0- 

### S 900 u 

# s 800 a:: 

### ~ 700 600 500 

### 400 400 500 600 700 

### 800 900 1000 1100 1200 1300 1400 1500 1600 1700 REFERENCE TEMPERATURE, deg.R
Are extrapolated limits less than 1.5%? YES FAHRENHEIT CALIBRATION RANGE -20 1200 If not acceptable, describe correclive action: Tchnician signature ~~ QAsrgnature 

# c5~~~

# • BARR THERMOCOUPLE CALIBRATION

Cal Date: 

### THERMOCOUPLE 10 8/24/2007 

### CALIBRATION TECHNICIAN: 

### T·33 Handheld AGA REFERENCE STANDARDS NIST TRACEABILITY LABORATORY CAL. DATE Hart Scientific 9103·A sin A1B289 Hart Scientific 9140 sin A1BOB6 Report No. A1B0718 12115/2005 Northern Balance 

### &Scale A3717010 

### &A3205006 A3717010 & A3205006 Temperature Calibration Points Reference Deg F (To) Probe Temp (deg F) Reference Temp (deg R) deg F + 460 Probe Temp (deg R), deg F+460 Difference (degrees) % DiffAbs. T Is difference less than 1.5% at all measured points? 

### 32 32 32 492 492



## o 0.0% 

### 212 212 211 672 671

1 

### 0.1% 

### 400 400 401 860 861 ·1 

### 0.1% 650 Ambient 650 70 651 70 

### 1110 530 1111 530

·1 0 0.1% 0.0% YES

1700 1600 1500 

# i 1400 

## I:! 1300 ~ 1200 ~ 1100 ~ 1000 

# 8 900 u 

# i 800 

### F 700 600 500 400400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700 REFERENCE TEMPERATURE, deg.R
Are extrapolated limits less than 

### 1.5%? YES FAHRENHEIT CALIBRATION RANGE ·20 1200 If not acceptable, describe corrective action: Tchnlc1an signature 

# 4~
QA signature 

# S n-;. ~~

# - BARR Manometer Calibration Sheet

Manometer Number Date of Calibration Technician Alnor M·8 9/30/2007 AGA Leak Check: Negative Positive

0.06 Ital Manometer Pass/Fail Pass 0.20 Pass Pass 0.50 Pass 0.80 1.00 Pass 1.50 Pass Pass 1.99 Pass 2.53 Pass 3.04 Pass 3.54 Pass 0.06 Pass 

### 0.20 0.50 Pass 

### 0.80 Pass 1.00 Pass 1.48 Pass 2.00 Pass 2.54 Pass 

### 3.04 Pass 3.55 Pass/Fail based on +/- 5% of set value

Technician signilure: QA signiture: Pass 

### 0.0@3" 0.0@3"

# •• PYROMETER f 

## CALIBRATION 

# BARR f 

### Pyrometer Number: 0-9 TC1 

### Date: 9/28/2007 Pyrometer Reference: CL-300-1

### GOOFTechnician: AGA

r

r 

### Reference (CF) Reference CC} 

### Pass/Fail 1000 538 Pass 

# I 950 510 Pass 900 482 Pass 

# I 850 454 . Pass 800 427 Pass 

# I 750 399 Pass 700 371 Pass 650 343 Pass 

# I
600 316 Pass 550 288 Pass 

## [ 500 260 Pass 450 232 Pass 

# I 400 204 Pass 350 177 Pass 

# I 300 149 Pass 250 121 Pass 200 93 Pass 

# I 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 signiture: 

# 4~ QA signiture: 

# ;S~JY~Praxair Distribution, Inc. 145 Shimersville Road Bethlehem, PA 18015



### t 

# ,j 

# aEi~~~~,~~ifql~J&~t~~i~i~~ir~~~~~pp}~l\t$' Tel: (610) 691-247~ Fax: (61O) 758-9\03

CUSTOMER CHEROKEE lNSTRut1ENTS P.O NUMBER 3710340-04

COl\lPONENT NISTSRMNO. CYLINDER NO. CONCENTRATION 53.6 PPM NITRIC OX~~B GMIS VB 48.52 PPM 16B3b

R ~ !a1FERENCE STANDARD Z=ZEROGAS C",OAS CANDIDATE

1. COMPONENT 53.6 PPM NITRIC OXIDE 

### mus vANALYZER MAKE-MODEL-SIN ANALYTICAL PRINCIPLE ChemHl'minescence

_.' c FIRST ANALYSIS DATE 09/20/07

Z 0 R 53.4 C 47.,6 CONC. 47.7 R 5~.4 Z 0 C 47.0 CONC. 47.1 Z 0 C 47.1 R 53.5 CONC. 47.2 1)i;.-I ""::'\ MEAN TEST ASSA Y ~7. ~ 

### , j TECO MODEL 42C 42CH-61352-31t. LAST CALIBRATION DATE SECOND ANALYSIS DATE 

### R 51.9 

### C 46.1 Z 0 C 46.0 C 45.9 R 51.5 06/31/07 09/27/07 CONC. 47.8 CONC. 47.7 CONC. 47.6 

### Z 0 R SloB 

### Z 0 UIM PPM MEAN TEST ASSAY 47.7 

# !I ij 

# !I ji 

# r J .! 

## I!


# r 

# ,I
11 'j 

### I; 

# II 

# II I VALUES NOT VALID BELOW 150 PSIG UNCERTAINTY:NO±0.4PPM

r- ----~-------------'-----~-.'------------..

-- 

# jl~:~~'~'~~======~========~============~'~============================================1~ I ': THIS CYLINDER NO. SA15B39 CERTIFIED CONCENTRATION ' 

### , it' HAS'BEEN CERTIFIED ACCORDING TO SECTION 2.2 NITRIC OXIDE 47, 5PPM OF TRACEABILITY PROTOCOL NO. EPA-600/R97/121 NITROGEN BALANCE , PROCEDURE Gl NOx (FOR REFERENCE ONLY) 47. 5PPM

CERTIFIED ACCURACY ± 1% % l\'1ST TRACEABLE CYLINDER PRESSURE 2000 PSIG 

# Jill

CERTIFICATION DATE 09/27/07 EXPIRATION DATE 09/27/09 TERM



### ANALYZED BY CERTIFIED BY COLLEEN STRAUBINGER I 

### ~~.============ -----=-;,;.:.-".,~=.=====::~====== 

# II I,
, 

# IPraxair Distribution, Inc. 145 Shimersville Road Bethlehem, PA 18015

Tel: (6lO) 691-2474 Fax: (610) 758-9103

3629063-11

CYLINDER NO. CONCENTRATION 

# i' I CAL015588 97.71 PPM

08/31/07 09/21/07 CONC. 125.6 CONC. 124.6 CONC. 124.4



## i 

# .-----------.~·~'~·--~~~----------~~~~~'---- __~l. ~ ~~~~==~~==~·.~~:'~========~~1~~~.==~~~~~..==============================~==========~

THIS CYLIN.1Dl!l~rNO. . SAI0103 \! HAS BEEN CERTiFiED ACCORDING TO SEC'f.ION 2.2' 'I OFTRACEABILIrr PRO'fOCOLNO. EPA-600iR97/121f PROCEDURE." 01' : CERTIFIED ACCURACY. f H % NIST TRACEABLE ~,.~~ CYLINDER PRESSURE' .2000 PSJG CERTIFICA'I)Ol'{DATE .~9/21j'07 

### EXPIRATION DATE 09/21/09 •. 

### TERM CERTIFIED CONCENTRATION NITRIC OXIDE NITROGEN NOx (FOR REFERENCE ONLY) 124.9PPM BALANCE 124.9PPM 

# .·if

J { j 

# ~ ..~=======================~==========~ ANALYZED BY.'.'
; .-.-,-- ".. 

# { .:i.r··: ======0= (. 

# .--/': •.- I



### ~~

## :



# .. ~~j~~=========~=====~=====~=C==~~===~

z :

### j'. 

### ~. 1. ( j

~. ~lEL'isSA BORD!ERE

-

### .. -,'

. ~~..~.

. 

# . CERTIFIED BY 

# @> 

# 1/Ji//if-f .1 I



# ·1



# I "

:"4' .·~1J. 

# . I
,! i I 

# , 

# -ll r 1 

## /1 

# I II .I

. ~ : Ii 

# II i 

# I II Ii I' 

### II 

# II /1 

# I' 

# J

# SIIII SCOTT-MARRIN, INC. 6531 BOX SPRINGSBLVD. • RIVERSID~ CA 92507 TELEPHONE (951) 653 - 6780 • FAX (951 ) 653 - 2430 

# Report Of Analysis EPA Protocol Gas Mixtures
BARR01 TO: 

### Barr 

### Engineering Co 

### Attn: Jason McOann 4700 West nth Street 

### Minneapolis, MN 55435-4803 (952) 832-2890 REPORT 

### NO: 49471-03 REPORT DATE: 

### March 3, 20061 CUSTOMER PO NO: 

### 2006/02/08INJM

CYLINDER NUM~ER:n 

## ~C299.8t CYUt)lDE:R SIZE: 

### l&OA (141 

### std cu

# m.. CYLlNDE.B PRESS.URE: 

### 200Qp.slg __

COMPONENT CONCENTRATION 

### (v/v) REFERENCE ANALVZER :I: EPA UNCERTAINTY STANDARD IUlKE, MODEL. Shl. DETECTION EXPIRATION REPLICATE DATE ANALYSIS DATA 

### Nitric oxide NOx Nitro$len dioxide 91.5 

### ± 0.9 

### ppm 91.5ppm


### <0.5 ppm GMIS CYLINDER II: CA03023 @100.7ppmv 

### Monltor Labs Model 8440 

### Serial II 136 Continuous Chemiluminescence LAST CAL DATE: 2/8/2006 

### 2110/2008 1112{2006 91.6 ppm 91.8 ppm 91.7 

### ppm MEAN: 91.7 ppm 2/1012006 91.3 ppm 91.4 ppm 91.5 

### ppm 91.4 ppm C?2-freeNltr~en, Balance, " 

### ~ .. ~' ;: :.:-:'

\'+ .- _'c ••. f •. ,

# . ',' ", :,.::

### .. ' • ~. .:. • +.. ":.

T



# REe~~ MAR 09 ZOO6 8A~ E!N8tNf!!RtNGCO. ppm ., umol./mole %

### =mole-%- The above analyses ware performed In accordance With Procedure G1 of the EPA Traceability Protocol, Report Number EPA-600/R97/121, dated September 1997. ~heabov~ 'ff1~~es are Invalid jfth" cylinder pressure Isless than 150 pslg.

ANALYST: ~.~ 

### 8.M,Marrln APPROVED: ----I--~

_
The only liability 01thls company for gas which lalls tocomply wIIh 1hJs.1IIlB¥1S shall be replac(J entor rOMslysls thereof by the company Wllhoul extra cost, STANDARD CALIBRATION GASES IN ALUMINUM CVUNDERS

### ~ 

# SIIII SCOTT-MARRIN. 

# INC. 6531 BOX SPRINGS BLVD. • RIVERSIDE, CA 92507 TELEPHONE(95t) 653-6780. FAX (951) 653~2430 

# Report Of Analysis EPA Protocol Gas Mixtures BARR01 TO: Barr Engineering Co Attn: Pete Rossmiller 4700 West 77th Street Minneapolis, MN 55435-4803 (952) 832-2890 REPORT NO: 51880-04 REPORT DATE( June 12, 2007 CUSTOMER

# PO NO: 2007-0518TYL 1

CYLINDER NUMBER: 

### CC7380 CONCENTRATION COMPONENT (v/v) 

### ·CYLINDER SIZE:..t50A (78 sIdco ft) REFERghCE ANALYZER STANDARD MAKE, MODEL, SIN. mOll,cnOIl 

### CYLINDER PRESSURE: 1100 psig 

### EXPIRATION REPLICATE DATE' 

### ANALYSIS DATA 

### Nllrlcoxlde NOx Nitrogen dioxide 513± 3ppm GMIS Monitor Labs Model 8440 6/11/2009 6/11120Q7 513 ppm CYUNDER#: Serial# 136 515 ppm <3ppm CC29067 Continuous 616 ppm @566ppmv Chemllumlnescence 517 ppm 

### Balance LAST CAL DATE: 6/8/2007 MEAN: 

### 616 ppm

-, t'" --. 

## oz-tree Nitrogen

.. ;

### ~ 

# ·RECE\VEO· JUN.1:·8·io07 BARR ENGINEERING CO.

ppm 

### = umole/mole % '" mole·% The above analyses were performed

### in accordance with Procedure G1 of Ille EPA Traceability Protocol, Report Number EPA-6001R97/121, dated September 1997: The above analyses are invalfdifthe cylinder pressure Is less than 150 psl{j.

ANALYST: 

# S)c..~ 

# M~

D.C.Marrin The Dilly liabnity01this company for gaswtlichfaRs 10comply v.ith this analysis shall be rspla en! or reanalysis thereof by the company v.ithout exlta cost 

### APPROVED: 

## ----J.i.~~~----

STANDARD CALIBRATION GASES IN ALUMINUM CYLINDERS 

# I

1

1

1 

# I 

# I 

# I·
I
I [ ,



# I 

# I.:
[

1i

1 

# I.

# 51111 SCOTT-MARRIN, INC. 6531 BOX SPRINGS BLVD. • RIVERSIDE, 

### CA 92507 TELEPHONE 

### (95t) 653-6780. FAX(951) 653-2430 

# Report Of Analysis EPA Protocol Gas Mixtures
BARR01 TO: 

### Barr Engineering Co Attn: Jason McCann 4700 West 77th 

## street Minneapolis. MN 55435-4803 

### (952) 832-2890 REPORT NO: 

### 50223·02 REPORT 

### DATE: July 20, 20061 CUSTOMER PO NO: 

### 2006/06J081NJMM

CYLINDER NUM.BER: '.

## CC2B.Q42..... ._ CYUNDJ;p fjIZE' J5@ 

### (141 sid cu ft).. t;:YLINPER PR!:SSURE: 2000 ps\f} .

COMPONENT CONCENTRATION (v/v) REFERENCE .ANALYZER :!;EPA UNCERTAINTY STANDARD MAKE. "ODf.~,GIN. DETECTION EXPIRATION REPLICATE DATE ANALVSIS DATA
Nitric oxlde 

### NOx Nitrogen dioxide GMIS Monitor Labs Model 8440 CYLINDERII: Serial II 136 CC1839 Continuous @ 249.8 ppmv ChemilumInescence . lAST CAL DATE: 7/19/2006 7/19/2008 7(1112006 V19/2006 251.1 ppm 253.1 ppm 251.6 ppm 252.5 ppm 253.1

## ppm 252.2

## ppm MEAN: 252.0 ppm 252.6 ppm 252.3 

### ± 1.6 ppm 252.3 ppm <1.3 ppm

02·fre9 Nitrogen Balance

ppm

# =umote/mole %

## =mole·% The above B/lalyses were performed In accordance wtth Procedure G1 of the EPA Traceability Protocol, Report Number EPA·6OOIR97/121, daled September 1997. The above B/lalYGes ate Invalid Ifthe cylinder Pf8S$ure Is less thllll 160 pslg.



### D.C.Marrin 

# t>.C~M~ ANALYST: 

## --:..{!L......III:...- APPROVED: __ -I-~

_
The only llablHty ofthis com~y for 1/89 Y.tllch !alls 10 comJlly w111jM!!9analysis Wi De re ont orrOMalysI81h&reof bythe companywllhou1l1X1l'a COSI. STANDARD CAUBRATlON GASES IN ALUMINUM CYLINDERS

# 51111 SCOTT-MARRIN~ INC. 653 t 

### BOX SPRINGSBLVD. • RIVERSIDEt

### CA 92507 TELEPHONE (951) 653-6760· FAX (951) 653w

### 2430 

# Report Of Analysis , 'EPA Protocol Gas' Mixtures

BARR01 TO: 

### Barr Engineering 

### Co Attn: Pete 

### Rossmiller 4700 West 77th Street Minneapolis, MN 55435-4803 (952) 832-2890 REPORT NO: 50895-01 REPORT DATE: 

### November 3D, 20060 CUSTOMER PO NO: 20060926TL

CYLINDER NUMBER: 

## CC12009 ',CYLINDER SIZE: 

### 150A (141 stdcuft) CYLINDER. PRESSURE: 

### 2000 pslg"

COMPONENT CONCENTRATION 

### (vJv) REFERENCE ANALYZER 

### ±EPA UNCERTAINTY STANDARD MAJ(E,MODEl,SiN,DETEcnoN EXPIRATION REPLICATE DATE ANALYSIS DATA



### Oxygen 21.54±0.23 % GMIS CYLlNDER#: 

### AtM031591 @24.4% Varian Model 1860 Serial#None Thermal Conductivity Gas Chromatography LAST CAL DATE: 

### 10/30/2006 MEAN: 

### Varlan Model 1860 11/2012009 Serial#None Thermal Conductivity, GasChromatography LAST CAL DATE: 

### 11/3/2006 11/2212009 11/2212006 5.05% 

### 5.04% 5.03% 5.04% 11/2012006 21.57 % 21.55% 

### 21.49 % ME;AN: 21.54 

### % Carbon dioxide 5.04±O.08 % GMIS CYUNDER#: 

### CC42814 @B%



### Nitrogen Balance

ppm 

### =umole/mole % ••

### mole·% , The above analyses were performed In accordance with Procedure G1 of the EPA Traceability Protocol, Report Number EPA-600/R971121. daled September 1997. The above analyses are Inva 'difthe y1lndar pressure 16less than 150 pslg,

ANALYST:__ -l,..;~I-6,.l1!...!~x:::::l'"--- APPROVED:---/--.:..------- 

### M.S.Calhoun The only liability of Ihfs company forg8Swhich faQs to' comply with this analysis shall be replac men! or reanalysis thereof by the rompanywilhout exira cost. STANDARD CALIBRATION GASES IN ALUMINUM CYLINDERS

# 51111 SCOTT-MARRIN" 

# INC. 653 

## t BOX SPRINGS BLVD, • RIVERSIDE1 

### CA 92507 TELEPHONE (950 6S3N 

### 6780 • FAX (950 653M 

### 2430 

# Report Of Analysis EPA Protocol Gas Mixtures

BARR01 TO: 

## Barr Englneerlng 

## Co Attn: Pete Rossmiller 4700 West 77th Street 

### Minneapolis, MN 55435-4803 (952) 832-2890 REPORT NO: 50895-02 REPORT DATE: 

### November 30, 20060 CUSTOMER PO NO: 20060926TL

CYLINDER. NUMBER: 

### CA06683 CYLINDER SIZE: 15M (141 std

## cutt) .CYLINDER PRESSI)Re:·2000 

### pslg·.

COMPONENT CONCENTRATION (vlv) REFERENCE ANALYZER . :!: EPA UNCERTAINTY STANDARD MAXE. MODEL, SIN, 

### osrscnoa EXPIRATION REPLICATE DATE ANALYSIS DATA



### Oxygen 8.98±0.05 % GMIS CYLINDER#: 

### CC81204 @9.8B% 

### Varian Model 1860 Serial# 

### None Thennal Conductivity 

### Gas Chromatography L.ASTCAL DATE: 

### 11/2812006 MEAN: 

### Varian Model 1860 11/30/2009 Serial#None Thermal Conductivity 

### Gas Chromatography 'LAST CAL DATE: 

### 11/9/2006 11/28/2009 11/28/2006 8.98% 8.98% 8.99% 8.98% 11130/2006

9.00% . 8.96%

8.99% 8.98% Carbon 

### dioxide 8.SSt 0.09 % 

### GMIS CYLINDER#: CC42814 @8%

MEAN: 

### Nitrogen Balance

ppm= umole/mole % • mole-% The above analyses were performed In accordance with Procedure G1 ol the EPA Traceability Protocol, Report Number EPA-600/R97/121, dated September 1997. The above analyses are lnva d If the UnderpressureIslessthan 150pslg.

ANALYST: 

### _...:....:.--L~~AL!::::::::::::~'---- APPROVED: 

# --.-I-.!.------- M.S.Calhoun The only liability ofthiscompany forgas wh1ch Cadsto complywiih thIs Malysls shall be rapla men! orreanalysis \h&feQf by the companywithoUI eXll'a coat. STANDARD CALIBRATION GASES IN ALUMINUM CYLINDERS1 

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## Process Throughput Page 1 of2



## Thomas Y. Leier
From: Thomas Y. Leier Sent: Thursday, December 20, 2007 7:44AM To: Thomas 

## Y. Leier Subject: 

## FW; Process Throughput Importance: Low

From: Hayden, Andrea J [mailto:ajhayden@cleveland-cliffs.com] Sent: Wednesday, December 19, 2007 1:30 PM To: Thomas Y. Leier Subject: FW: Process Throughput Importance: LowHere you go Tom. This should helpAndrea

From: Jones, Jeffrey K. Sent: Wednesday, December 19, 2007 1:17PM To: Hayden, Andrea J Subject: RE:Process Throughput Importance: Low Anything above 470 LTPH green feed rate would be considered "high tons". tests 1=477,2=480,5=494,6=490,7=489,9=475,10=474, 11=471, 12=472

From: Hayden, Andrea J Sent: Wednesday, December 19, 2007 12:57PM To: Jones, Jeffrey K. Subject: FW: Process Throughput Jeff, I received this email from Barr. They are trying to put together the stack test report for the MPCA. What tonnage range would we consider "high tons"?ThanksAndrea



## This electronic message and any attachments included with this message are for the exclusive use of the individual or entity to which it is intended to be addressed. This message may contain information that is privileged or confidential and thereby exempt and protected from unauthorized 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, distribution 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,

12/20/2007

## Process Throughput Page 2 of2
please notify the sender immediately and permanently delete the original message from your e-mail system.

12/20/2007

### Condition 1 High tons - max process air - 2350 firing temps (10/24/073:00 pm to 10/25107 7:15 am) Condition 2 High tons - max process air - 2240 firing temps (10/25/079:00 am to 10/26/07 7:00 am) Condition 3 420 tons - max process air - 2240 firing temps (10/26/079:00 am to 10/27107 6:45 am) Condition 4 420 tons - max process air - 2350 firing temps (10/27/079:00 am to 10/27107 3:00 pm) Condition 5 High tons - max process air - 2350 firing temps (10/271075:00 pm to 10/28107 6:30 am) Condlflon 6 High tons - max process air - 2240 firing temps (10/28/077:00 am to 10/29107 6:30 am) Condition 7 High tons - max process air - 2200 firing temps (10/29/078:00 am to 10/30107 6:30 am) Condition 8 420 tons - lower process air - 2300 firing temps (10/30/079:00 am to 10/31107 2:45 pm) 

### Condition 9 High tons - max process air - 2350 firing temps (10/31/07 5:00 pm to 11/01/07 6:30 am) Condition 10 High tons - max process air - 2265 firing temps (11/01/07 8:30 am to 11/02107 12:00 am) Condition 11 High tons -' max process air - 2200 firing temps (11/02/077:30 am to 11/02107 3:00 pm) Condition 12 High tons - max process air - 2350 firing temps (11/02/074;30 pm to 11103/07 10:00 am) Conditions 1,5,9,12 are the same Conditions 2 and 6 are the sameI " I I 

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### TEST PLAN FOR A TACONITE MANUFACTURING FACILITY TEMPORARY NOx MONITORING INSTALLATION HIBBING TACONITE COMPANY HIBBING, MINNESOTA
Date test plan created/revised: August 29, 2007/0ctober 12,2007 Scheduled test date(s): October 21 "28, 2007

PART I. GENERAL INFORMATION Name and address of emission facility: Hibbing Taconite Company P.O. Box 589 Highway 5 north Hibbing, Minnesota 55736
Facility contact person and telephone number: Andrea J.Hayden ajhayden@cleveland"c1iffs.com (218) 262·6856 phone (218) 262-6877 fax
MPCA AQD Air Emission 10 Number: 13700061·002

Reason the Emission Unit is to be Tested: Testing is a voluntary effort to evaluate the variability of NO x emissions as is relates to normal operation oftaconite production. This testing will also provide HTC with additional data for generating a predictive equation for NOx emissions based on operating parameters that HTC currently monitors continuously.
Testing Company and Contact: Company: Barr Engineering Address: 4700 West 77fu Street; Minneapolis, MN 55435"4803 Contact(s): Tom Kuchinski Work: (952) 832-2727 Pete Rossmiller Cell: (612) 240"6695 Fax: (952) 832-2996

Page 1 of5

### PART II. TESTING REQUIREMENTS The table below gives a summary of the pollutants to be tested and test methods.

StacklVent 

### #: Limitation Basis of Pollutant Tested and Applicable Specific MethodslProcedures Source Pollutant Tested Emission Limit Required Citation Description 40 CPR Part 60, Appendix A
EPA Method 7E - Modified (daily zero 

### &span checks) 1 -test run ~ 7 days (~168 NOx hours) in duration reported in l-minute averages and l-hour SV025~028 Voluntary Testing is a voluntary effort to evaluate averages in PPM (dry), Ib/hour Waste Gas Research the variability of NO x emissions as it NOx, Ib/long ton, and

Stacks relates to normal operation of taconite lb/mmbtu, production. All four stacks will be tested simultaneously for ~ 168 hours. Modified EPA Method 2 Single Point Velocity Pressure Continuous temperature will be



## - recorded. Moisture check will be recorded daily (wet bulb/dry

bulb technique for moisture determination)

PART III. OPERATING CONDITIONS The table below includes a summary of the industrial processes and related control equipment.

Process Equipment Description for Unites) to be tested:
EU021/ SV025-028 Waste Gas Stack 

### IIndurating Furnace Line 2 Process Equipment Parameter Monitoring During Performance Test: Pellet Type: Standard Production Rate: in terms of tons/hour Fuel Type: Natural Gas Only Heat Input: in MMBtulhour Unusual Production Events: will be documented Ambient Air Temperature - measured at analyzer trailer Continuous monitoring of gas flow Various Temperatures throughout the indurating process (this test will determine which temperature parameters are applicable in determining a predictive equation for NOx) Various Pressures throughout the indurating process (this test will determine which pressure parameters are applicable in determining a predictive equation for NOx) Air Damper Position Ferrous iron content of green ball (shift report-not continuous)

Page 2 of5

### Pressure drop across 

### demist recorded continuously. Permit limit: 2: 0.1 psi across demist panel of the wet scrubber. Pressure drop across 

### venturi recorded continuously. Permit limit: 2: 0.5 psi across the venturi of the wet scrubber. Liquid flow rate recorded continuously. Permit limit: 2: 300 gpm. Control Equipment Description: Venturi Scrubber CE027-030 (SV025-028, EU02I) Venturi ScrubberlEnvironeeringIModel A33-200000 Control Equipment Operating Parameter During Test: (Identify parameters with normal operation limits and frequency/interval of records) CE027-030 SV025-028 EU021

PART N.TEST METHODS 1. The following is a description ofthe test methods, number oftest runs, length of test runs, and sampling rate for each pollutant A EPA Method I for the location of sampling ports and points. One determination per test location.
B. EPA Method 2 (modified) single point velocity pressure. Continuous temperature will he recorded. Moisture check will be recorded daily (wet bulb/dry bulb teclmique for moisture determination).
C. EPA Method 7E·- Modified for the determination of NO x concentration using a chemiluminescent analyzer calibrated with EPA protocol 1 calibration gases of NO in nitrogen (High and Mid concentration for initial calibration). Instrument precision and accuracy will be determined once per day using a zero gas and span gas to establish any instrument drift. Data wiII be bias corrected using the pre and post zero/span test results that precede and follow the stack gas NOx data. NOx emission data will be reported as I-minute averages and l-hour averages in the following units: PPM (dry), lb/hour NOx, lb/long ton, and lb/mmbtu,
D. EPA Methods 7E-Modified, will be conducted as specified in 40 CFR Part 60, Appendix A and as established in this test plan document.

PARTV.CEMS There are no CEMS located at the emission points to be tested.

Page 3 of5

### PART VI. OTHER Schedule Week of October 21-28, 2007

10/22/07 10/23/07 10/24/07 10/25/07 10/26/07 10/27/07 10/28/07 10/29/07 Monday Tuesday Wednesday Thursday Friday Saturday Sunday Monday Mobilize, Hookup Power to Analyze Trailer. NOx Test Installation NOx Test NOx Test NOxTest NOx Test NOx Test NOx Test (on SV025~ of (on SV025- (on SV025- (on SV025- (on SV025- (on SV025~ (on SV025~ 028) Temporary NOx 028) 028) 028) 028) 028) 028) (0000-1200)
Monitor (0000-2400) (0000-2400) (0000-2400) (0000-2400) (0000-2400) (0000-2400) (0600-1200) Demobilize (1200-1500)
NOxTest (on SV025- 028) (1200-2400)

Test Report:
The final test report will include a statistical analysis of the l-hour average NOx emission data to establish the mean and standard deviation of the NOx data. One complete test report (one hard copy) will be submitted within 45 days of the last date of testing. Electronic data will be submitted within 105 days of the test performance date.
Diagrams of the stack and approximate test locations will be included in the test report.

Page 4 of5

### Submittal Address:

CC: Ms. Mary Jean Fenske Minnesota Pollution Control Agency 520 Lafayette Road St. Paul, Minnesota 55155·3898

Mr. Andrew Place Minnesota Pollution Control Agency 520 Lafayette Road St. Paul, Minnesota 55155·3898

Page 5 of51 

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# Project Participants

Minnesota Pollution Control Agency Andy Place - Performance Test Coordinator



## Hibbing Taconite Company Andrea 1. Hayden- Section Manager, Environmental Department



## Barr Engineering Company Tim Russell- Vice President Tom Kuchinski - Project Manager Pete Rossmiller -;-AirQuality Technician Tom Leier - Stack Test Technician

(Primary contact information can be found in the test plan located in Appendix H)

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