## General Shal® Brick, Inc. SR 67, CR 1100 N Mooresville, IN 46158

Determination of HCL/HF/CL2 & HAPS Emissions

Proj ect #141.11

February 1 st, 2012

Prepared 

## by: Wileox Environmental Engineering, Inc. Air Analysis Division 5757 West 74`" Street Indianapolis, Indiana 317.472.0999 (.bRPOHATE oPFlc9
5559 Weff 74th Sfreat lndiana0ol6, IN 46298

phone 317,472.0999
fas31Z492.0993
uwmwilcaxenucom

## ~



# ~ ~~~ 

# W I t'cox Air Analysis Services
5757 West 74` h Street • Indianapolis, Indiana 46278 TEL 317.472.0999 . 877.683.8378 • FAX 317.472.0993



## Certification Page

Wilcox Environmental Engineering, Inc. - Air Analysis Division represents that the information provided in this report is true and accurate. We strive to remain true to our mission, that the people involved are people of integrity, the data is accurate, and the reporting timely.



### Sincerely, 

# ~ &4~

Joseph B. Kinder Field Operations Manager Air Analysis Division Wilcox Environmental Engineering Inc.

Date: 

# — ,;-' 4" 1 1-

STACK TESTING AND ENVIRONMENTAL SERVICES

# TABLE OF CONTENTS

1. EXECUTIVE SUMMARY (Page 2)

Test Summary, Table 1

2. RESULTS (Page 3)

Hydrogen Chloride (HCL) Emissions, Table 2 Hydrogen Fluoride (IF) Emissions, Table 2 Chlorine (CL2) Emissions, Table 2

3. DESCRIPTION OF PROCESSES AND FIELD NOTES (Page 4)

4. METHODOLOGY (Pages 5 & 6)

Summary of Sampling Procedures Description of Sampling Methods



## APPENDIX SAMPLE CALCULATIONS I

FIELD DATA PRINTOUTS II FIELD DATA III LABORATORY DATA IV CHAIN OF CUSTODY V CALIBRATION DATA VI PRODUCTION DATA VII

### General Shale Brick, Inc Project Number: 141.11

EXECUTIVE 

### SUMMARY Wilcox Environmental Engineering - Air Analysis Division was contracted by General Shale to perform ICR testing at the outlet of the new kiln during brick manufacturing in Mooresville, Indiana, on February 1, 2012. Sampling was performed for Hydrogen Chloride (HCl), Hydrogen Fluoride (HF), Chlorine (CL2) & HAPS Metals emissions. The following personnel were involved with the testing program Air Analysis Air Analysis Air Analysis Air Analysis Air Analysis General Shale Joe Kinder Mike Murphy Marcus Allen Dane Hadley Tony Wickliff Warren Paschal

The testing program was performed utilizing US EPA Methods 1-4, 26A and 29. Three one-hour test runs were performed on February 1 st, 2012.

Source Emissions Sampling Program

Parameter Methods Location Date
Traverse Point Determination EPA RM 1 Brick Kiln Outlet 02/01/12 Flow Rate / 

### Gas Velocity EPA RM 2 Brick Kiln Outlet 02/01/12 Molecular Weight Determination EPA RM 3 Brick Kiln Outlet 02/01/12 Moisture Determination EPA RM 4 Brick Kiln Outlet 02/01/12 HCL/IF & 

### CL2 EPA RM 26A Brick Kiln Outlet 02/01/12 HAPS Metals EPA RM 29 Brick Kiln Outlet 02/01/12

Wilcox Environmental Engineering, Inc. Air Analysis Division

### General Sha1e Brick, Inc Proj ect Number: 141.11

TEST SUMMARY 

## Table 1

Date Source Time Mass Emissions Mass Emissions

Brick Kiln Hydrogen Chloride Hydrogen Chloride 02/01/12 Outlet 11:55-5:00 1.3847 N/A Ibs/hr Ibs/ton Brick Kiln Hydrogen Fluoride Hydrogen Fluoride 02/01/12 Outlet 11:55-5:00 1.4117 N/A Ibs/hr Ibs/ton Brick Kiln Chlorine Chlorine 02/01/12 Outlet 11:55-5:00 0.2492 N/A Ibs/hr Ibs/ton Brick Kiln Lead Lead 02/01/12 Outlet 11:55-5:00 0.000221 0.000011 Ibs/hr Ibs/ton Brick Kiln Mercury Mercury 02/01/12 Outlet 11:55-5:00 0.000558 0.000029 Ibs/hr Ibs/ton Brick Kiln Antimony Antimony 02/01/12 Outlet 11:55-5:00 0.006701 0.000344 Ibs/hr Ibs/ton Brick Kiln Beryllium Beryllium 02/01/12 Outlet 11:55-5:00 0.000204 0.000010 Ibs/hr Ibs/ton Brick Kiln Arsenic Arsenic 02/01/12 Outlet 11:55-5:00 0.000393 0.000020 Ibs/hr Ibs/ton Brick Kiln Selenium Selenium 02/01/12 Outlet 11:55-5:00 0.002296 0.000118 Ibs/hr Ibs/ton Brick I<iln Cobalt Cobalt 02/01/12 Outlet 11:55-5:00 0.001020 0.000052 Ibs/hr Ibs/ton Brick Kiln Cadmium Cadmium 02/01/12 Outlet 11:55-5:00 0.0.000510 0.000026 Ibs/hr Ibs/ton Brick IGIn Chromium Chromium 02/01/12 Outlet 11:55-5:00 0.001020 0.000052 Ibs/hr Ibs/ton Brick Kiln Manganese Manganese 02/01/12 Outlet 11:55-5:00 1.574816 0.080760 Ibs/hr Ibs/ton Brick Kiln Nicl<el Nickel 02/01/12 Outlet 11:55-5:00 0.001020 0.000052 Ibs/hr Ibs/ton



### Wilcox Environmental Engineering, Inc. Air Analysis Division

### General Shale Brick, Inc Project Number: 14 1. 11

RESIILTS TFST CONDITIONS 

## Table 2 Brick Kiln Outlet - HCL/HF/CL2 Gas Conditions 1 2 3 Avg Ts Stack Temperature 308.583 304.083 299.583 304.083 Bwo Moismre (volume %) 6.28 5.47 5.82 5.85 Oz Oxygen (dry volume %) 17 17.3 17.3 17.2 CO Z Carbon Dioxide (dry volume %) 3.0 2.5 2.5 2.66 Volumetric Flow Rate Qa Actual Conditions (acfin) 41,231 45,133 42,417 42,927 Qstd Standard Conditions (dscfin) 26,308 29,217 27,518 27,681 Pollutant Results Ec E(me) Emission Rate, (lbs/hr) HCI

Emission Rate, (Ibs/hr) H/F Emission Rate, (lbs/hr) C1,2 154.7128 1.5411 31.4399 2.4154

1.6949 0.4436 0.3539

1.1284 0.0549 1.3847

1.4117 0.2492 

## *HCL& CL2 lbs/hr Avg. of Runs 2&3 only Brick Kiln Outlet - 

## (HAPS Metals) Gas Conditions 1 2 3 Avg Ts Stack Temperature 310.083 307.750 305.083 307.639 Bwo Moisture (volume %) 6.37 5.86 5.48 5.90 O 2 Oxygen (dry volume %) 17.3 17.3 17.3 17.3 CO z Carbon Dioxide (dry volume %) 2.0 2.0 2.0 2.0 Volumetric Flow Rate Qa Actual Conditions (acfin) 47,269.07 47,465.18 46,157.49 46,963.91 Qstd Standard Conditions (dscfin) 30,051.98 30,434.60 29,817.81 30,101.46 Pollutant Results Ec Emission Rate, (lbs/hr) Lead 0.000371 0.000166 0.000126 0.000221 E(me) Emission Rate, (lbs/ton) 0.000019 0.000009 0.000006 0.000011

Emission Rate, (Ibs/hr) Mercury 0.000756 0.000581 0.000336 0.000558 Emission Rate, (Ibs/ton) 0.000039 0.000030 0.000017 0.000029 Emission Rate, (lbs/hr) Antimony 0.005381 0.006951 0.007771 0.006701 Emission Rate, (lbs/ton) 0.000276 0.000356 0.000399 0.000344 Emission Rate, (Ibs/hr) Beryllium 0.000025 0.000276 0.000311 0.000204 Emission Rate, (Ibs/ton) 0.000001 0.000014 0.000016 0.000010 Emission Rate, (lbs/hr) Arsenic 0.000000 0.000545 0.000634 0.000393 Emission Rate, (lbs/ton) 0.000000 0.000028 0.000033 0.000020 Emission Rate, (Ibs/hr) Selenium 0.000064 0.002894 0.003929 0.002296 Emission Rate, (lbs/ton) 0.000003 0.000148 0.000201 0.000118 Emission Rate, (Ibs/hr) Cobalt 0.000127 0.001379 0.001554 0.001020 Emission Rate, (lbs/ton) 0.000007 0.000071 0.000080 0.000052 Emission Rate, (lbs/hr) Cadmium 0.000064 0.000690 0.000777 0.000510 Emission Rate, (lbs/ton) 0.000003 0.000035 0.000040 0.000026 Emission Rate, (lbs/hr) Chromium 0.000127 0.001379 0.001554 0.001020 Emission Rate, (Ibs/ton) 0.000007 0.000071 0.000080 0.000026 Emission Rate, (Ibs/br) Manganese 0.000505 4.723438 0.000503 1.574816 Emiasion Rate, (lbs/ton) 0.000026 0.242228 0.000026 0.080760 Emission Rate, (lbs/hr) Nickel 0.000127 0.001379 0.001554 0.001020 Emission Rate, (lbs/ton) 0.000007 0.000071 0.000080 0.000052 

### Wilcox Environmental Engineering, Inc. Air Analysis Division

### General Shale Brick, Inc Proj ect Number: 141.11

DESCRIPTION OF SOURCE PROCESSES AND FIELD NOTES



### One (1) brick manufacturing line, identified as New Plant, consisting of the following:One (1) brick making room and sand system (mill room), identified as EUNPMR, equipped with a baghouse, identified as CD-MRBH and exhausting to Stack MRBH, capacity: 72.5 tons of clay and shale per hour. One (1) coal/natural gas frred brick kiln, identified as EU-NPK, equipped with a dry hydrated lime, sodium bicarbonate, or dry hydrated lime/sodium bicarbonate combination dry lime injection baghouse, identified as DIFF-03, and exhausting to Stack DIFF-03, capacity: 20.55 tons of bricks and 25.0 million British thermal units per hour. One (1) nataral gas/propane brick dryer, identified as EU-NPBD1, exhausting to Stack NPBD 1, capacity: 20.55 tons of bricks and 13.29 million British thermal units per hour.

Actual recorded production material information is in Appendix.

Wilcox Environmental Engineering, Inc. Air Analysis Division

### General Shale Brick, Inc Project Number: 141.11

METHODOLOGY 7hesamplingproceduresusedbyflirAnaly.sisDivisionareasfollow.s:


## TITLE 40 CFR PART 60 APPENDIX A Method 1"Sampling of Velocity Traverses for Stationary Sources" Method 2"Determining of Stack Gas Velocity and Volumetric Flow Rate" Method 3"Gas Analysis for the Determination of Molecular Weight" Method 4"Determination of Moisture Content in Stack Gas" Method 26 "Determination of Hydrogen Halide" Method 29 "Determination of Metals Emissions from Stationary Sources"


## SAMPLE POINT DETERMINATION-EPA METHOD I Sampling point locations were determined according to EPA Reference Method 1. Sampling Points Locations Dimensions Ports Points Per Port Total Points Outlet 45" I.D. 2 6 12


## ** @xact measure points and de'stances to disturbancea are listed tn gppendix- Field Data


## VELOCITY AND VOLUMETRIC FLOW RATE — EPA METHOD 2 EPA Method 2 was used to determine the gas velocity and flow rate at the stack. Figure 5-1 includes the components of the EPA Method 2 sampling apparatus. Each set of velocity detenninations included the measurement of gas velocity pressure and gas temperature at each of the Method 1 determined traverse points. The velocity pressures were measures with a Type S pitot tube. Gas temperature measurements made with a Type K thennocouple and digital pyrometer.
GAS 

## COMPOSITION AND MOLECULAR WEIGHT — 

## EPA METHOD 3 In order to determine the oxygen and carbon dioxide concentrations, a sample of gas was obtained and analyzed in accordance with EPA Method 3. The gas sample was collected using a Fyrite analyzer. The results were used to detennine gas molecular weight.


## MOISTURE CONTENT — EPA METHOD 4 The flue gas moisture content at the testing locations was determined in aceordance with EPA Method 4. Figure 5-1 includes the Method 4 sampling components. The gas moisture was determined by quantitatively condensing moisture in the chilled impingers and silica absorption. The arnount of moisture eondensed was determined gravimetrically. A dry gas rneter was used to measure the volume of gas sampled. Moisture content is used to determine stack gas velocity.


## HYDROGEN HALIDES DETERMINATION — 

## EPA METHOD 26A Stack gas is withdrawn isokinetically and haiides are collected on the nozzle, probe and filter, sulfuric acid and sodium hydroxide. The probe temperature and filter are maintained at temperatures of 248 degrees F. HCL is collected in 0.1 N 142SO4. Chlorine is collected in 0.1 N NaOH. The irnpinger temperature and exit gas is maintained at temperatures at or below 68 degrees F. The impingers and connecting glassware are rinsed twice with de-ionized water and captured in a sealed container.

Wilcox Environmental Engineering, Ine.

Air Analysis Division

### General Shale Brick, Inc Project Number: 141.11



## METALS DETERMINATION — 

## EPA METHOD 29 A stack sample is withdrawn isokinetically from the source, particulate emissions are collected in the probe and on a heated filter, lead particulate is captured in the first impinger; this impinger contains 0.1 N Nitric Acid a blanlc impinger divides impinger 3 and 4; gaseous emissions are collected in an aqueous acidic solution of hydrogen peroxide (analyzed for all metals including Hg) and an aqueous acidic solution of potassium permanganate (analyzed only for Hg). A fourth and final impinger contains about 200 grams of silica gel. The probe temperature and filter are maintained at temperatures of 248 degrees F(=/-25 deg. F). The impinger temperature exit gas is maintained at temperatures at or below 68 degrees F.

Wilcox Environmental Engineering, Inc. Air Analysis Division

### General Shale Brick, Inc Proj eet Number: 141.11



## APPENDIX I

SAMPLE CALCULATIONS

Wilcox Environmental Engineering, Inc. Air Analysis Division

## SAMPLE CALCULATIONS Ttwtrblapcerrndrtgtbemuhsaeegmvat

~ etavo

~ aliyfromnwdsf; itmaymtbepom'bto0oaacelydnplir.tadrsemsultsmtmgaatculaur. The scfrresmmrilwd dsn, raul7s aM aA alwfations:rc wricd io sbften dccieul placo throngbuut. ibe finsf bble Ls Iumutkd to an apptoprote numba of signi6ant 6gures. • • 

### 1, Volume of water collected (wscf)
Y,, a *(0.04707)(P Y ,)



### Where: V i , total volume of liquid colleMed in impingers and silicra gel (mn V, 4 volume of water collected at standard conditions (tP) 0,04707 conversion factor (ft'/rnl)

2. Volume o£ gas metered, standard conditions'(dscf)

(17.64)(Y

~ XP ma ' a" XYa) j
.O e (4 60 23.L

+7 )



### Where: P y „, barometric pressure (in Hg) T m average dry gas meter temperature (°F) V, volume of gas sample throngh dry gas meter at meter corlditions (tt) V,,,,,d volume of ga.s sample through dry gas meter at standard conditions (R') Y d gas meter correction factor (dimensionless) DH average pressure drop across meter 

### box orifice (in Ii z O) 17.64 conversion factor (°R/in Hg) 13.6 conversion Factor (in H z 0/irt FIg) 460 °Fto °Rconversionconstant

3. Samplc gas pressure (in Hg)
pf P P t 136 )



### VJhere: i'y,,, - barometric pressure (in Hg) 

### P s sample gas static pressure (in H

~ 

### O) P, absolute sample gas pressure (in HZO) 

### 13.6 conversion factor (in H z O/in Hg)

### 4. Actuai vapor pressure ('ut Hg)
P,=P,



### Where: P„ P,

5. Ninisture Content (%a)

B— V.uv'Y,.sw



### Where: B. V,, w V,n,a

6. Saturated moisture content (%)

B (P) „ (P,)

Where;
B~ 

### P

, 

### P s vapor pressure, actual (m Hg)

absolute sample gas pressura (in Hg)

proportion of water vapor in the gas stream by volume volume of gas sample through the dry gas meter at standard conditions (ftO) volume of water collected at stsndard conditions (fl )

proportion ofwater vapor in gas stream by volume at saturated cronditions (%) vapor pressure, actual (in HS) absolute sample gas pressure (in Hg)

7. Molecular weight of dry gas stream (lb/lb-mole)

41d=,tlro11CO2) + L ,~ (02) r c

~ o y (CO+N2) ( 1 00) (100) (100)

Where: 

### Md dry molecular weight of sample gas (lb/1b-mole) MCM molecular weight ofcarbon dioxide (lb/lb-mole) Mo: molecular weight of oxygen (lbJlb•mole) Mco , r< rrrolecular weight of carbon monoxide and nitrogen (Ib/lb-mole) CO 2 proportion of carbon dioxide in the gas stream by volume (%) 0 = proport'roa of oxygen in the gas stream by volume (%) CO +N 2 proportion of carbon monoxide and nitrogen in gas stream by volume (%) 100 conversion factor, %

### &. Molecular weight ofsarnple gas (lb/Ib-mole) 

## M,=(.w

~ 

## ct -e.d •(M,

~ 

## xe. ~



### Wfiere: Md dry molecular weight of sample gas ([Wlb-mole) B. proportion of water vapor in the gas shtam by volume M M molecular weight of water (Ib/lb-mole) Ms molecular weight of sample gas, wet basis (lb/lb-mole)

9. Velocity of sample gas (ft/sec)

~ 

### .`(RoXC,X

~ 

### 3f 

### t,+a6o> 1

(M xP.)



### Where: Kp velocity pressure coefficient (dimensionless) Cp pitot tube constant Ms molecular weight of sample gas, wet basis (Ihllb-mole) Ps ' absolute sample gas pressure (in. Hg) t, average sample gas temperature (°F) Vs average sample gas velocity (ft/sec) 460 °F to °R conversion factor



### 10. Total Bow of sample gas (acfrn)



### Q,-c6ox.,.xv>

Where: As cross section area of sampling location (ft) Qs volumetric flow rate at actual conditions (acfm) Vs sample gas velocity (ft/sec) 60 eonversion factor, seconds to minutes

### 11. Total flow of sample gas (dscfin)

Q..2 t(?.XP.X17.64xt-B,J

. 

### V,•W)

Where: Bwo proportIon of watervapor in the gas stream by voitlme Ps absolute sample gas pressure (in. Ilg) Qa ,. volumetric flow rate at actual conditlons (acfrn) Qstd volumetric flow rate at standard conditions (dscfm) t, average sample gas temperature (°F) 11.64 conversion factor, (t"Rlin,Eg) 460 

### °F to °R conversion factor

12. Total flow of sample gas (dscfli)



### (QoxP,x 17

. 64 

## x 1— B ,o) R60) (t,1a6o)



### Where; Bwo proportion of water vapor in the gas stream by volume Ps absolute sample gas pressure (in. Hg) Qa volumetric flow rate at actual conditions (acfm) Qstd hr volumetric flow rate at standard conditions (dsc8nx60) t, average sample gas temperature ("F) 17.64 conversion factor, (t°R1in.Hg) 460 °F to °R conversion factor

### 13. Percent Isokinetic (%)

f= (0.09450xT,xrj (P.xV:X tDtR1 1tOXt

- B.b) (144J(4)

Where: 

### Dn diameter of noazle, inches Bwo proportion of water vapor int he gas stream by volurne I percent ofisokinetic sampling (%) Ps absolute sample 

### gas pressure (in. Hg) T. average sample gas temperature (°R) V,,,,, d voltutte ofgas sample through the dry gas meter at standard conditions (ttx) Vs avtrage sample gas velocity (81sec) 9 total sample time, minutes O.D94S0 constant

14. Poltutant concentration (gr/dscf)
(IS.43)(m,a 

## c°„e A
a



### Where: Cwd.r measured concentration in gas stream, gr/dscf Mn pollutant collected, corrected for reagent blank, grams V m „ d volume of gas sample through the dry gas meter at standard conditions (S ) 15.43 conversion factor, grams to grains

15. Pollutant Emissions, Mass Emissions Rate lbsrhr

(Ng„ c ,)(21046e-9 (0,,,,x60) Emrr=— (yW) -



### Where; E 6

~ 

### Mass emissions rate, pounds per hour pg pollutattt micrograms of pollutant emissicns Q„ d volumetric flow rate at standard couditions, dry basis (dscf 

### u r ) V, a Volume Standard conditions 2.2046e-9 conversion factor, pounds per microgram 60 conversion factor, minutes per hour

# VIA -

Figore 26&~1^ Saopliog %raio1527 'Refer to EPA publication SW-846 (Reference 2 in Section 16.0).

E

~ a

~ c ~ J

~

N a
~ ? ~ a a N W Ey = 

# _ = ~ J
~ Ua, >(7 

## f o N

'a

~ m s c
~ > ~ a

~ 

### 2 F' E

— N N a O ~ 0 ~ 6 A —J E m ~

W 

## m Z 4 

## = a

— _ — J n ` w o m ~ C7 d
=J En d o a 1 0 

### d

~ v
No 

# _ m N ~ 

# `

N 

# W

V , a
ac O o_ a Ey

F =' 1

~ a 

# e o a~ c 

### y J ~ W

~

a n E a a 

### - m 1- N 

### _N

~



### Figure 29-1. Sampling Train.

### General Shale Brick, Inc Project Number: 141.11



## APPENDIX II

FIELD DATA SPREADSHEETS

Wilcox Environmental Engineering, Inc. Air Analysis DivisionSTACK EMISSION SUMMARY
SOURCE TESTED: Kiln COMPANY NAME: General Shale Brick DATE OF TEST: 02/01/12

Pollutant Emissions Run 1 Run 2 Run 3 Avera e Lead Emissions Iblhr) 0.000371 0.000166 0.000126 0.000221 Lead Emissions Iblton 0.000019 0.000009 0.000006 0.000011 Mercury Emissions Ib/hr 0.000756 0.000581 0.000336 0.000558 Mercu Emissions Ib/ton 0.000039 0.000030 0.000017 0.000029 Antimony Emissions (Iblhr) 0.005381 0.006951 0.007771 0.006701 Antimony Emissions Ib/ton) 0.000276 0.000356 0.000399 0.000344 Beryllium Emissions (Iblhr 0.000025 0.000276 0.000311 0.000204 Beryllium Emissions Iblton) 0.000001 0.000014 0.000016 0.000010 Arsenic Emissions (Ib/hr 0.000000 0.000545 0.000634 0.000393 Arsenic Emissions Ib/ton 0.000000 0.000028 0.000033 0.000020 Selenium Emissions Ib/hr) 0.000064 0.002894 0.003929 0.002296 Selenium Emissions (Iblton 0.000003 0.000148 0.000201 0.000118 Cobalt Emissions (Ib/hr) 0.000127 

### 1 0.001379 0.001554 0.001020 Cobalt Emissions Ib/ton 0.000007 0.000071 0.000080 

### 1 0.000052 Cadmium Emissions (Ib/hr 0.000064 0.000690 0.000777 0.000510 Cadmium Emissions Ib/ton) 0.000003 0.000035 0.000040 0.000026 Chromium Emissions Iblhr) 0.000127 0.001379 0.001554 0.001020 Chromium Emissions (Iblton) 0.000007 0.000071 0.000080 0.000052 Man anese Emissions (Ib/hr 0.000505 4.723438 0.000503 1.574816 Manganese Emissions (Ib/ton) 0.000026 0.242228 0.000026 0.080760

Nickel Emissions Ib/hr 0.000127 0.001379 0.001554 0.001020 Nickel Emissions (Ib/ton) 0.000007 0.000071 0.000080 0.000052

Av

. Stack Vol. Flow Rate ACFM 47,269.07 47,465.18 46,157.49 46,963.91 DSCFM 30,051.98 30,434.60 29,817.81 30,101.46

Av

. Stack Temp. 310.083 307.750 305.083 307.639 Stack Gas Velocity 71.330 71.626 69.653 70.870

Av

. Velo ily Head 1.0712 1.0856 1.0317 1.0628 Av

. Sq. Rt of Delta P 1.0350 1.0419 1.0157 1.0309
ISOKINETIC TESTING SUMMARY

%Isokinetics: 96.40 95.93 96.81 

### 1 96.38 Allowable isokinetic 90-110% % Moisture of Slack Gas 6.37% 5.86% 5.48% 5.90 % ' Sam le Volume 53.632 

### 1 54.049 53.442 53.708COMPANY NAME: GenoralSDale 9rluk LOCATION: Mooresollle In, SOIIRCETESTED: Mlln DATE BFTEST: O2I01112 RVN NO,: 1 POLLDTANT: MehlNOaxea
Molecular WeIPM o151aok Gai OrV Basls, Mtl bc02 2 %02 to i 3 Ma 29. 2
Volume utwarer Vapor Colleorea 0 sr0. CONO., vwu vle ]i6 Vwrsral 5.650
volume et Orv cas Culbtlm @ STO, cOND.. Vm(sM rmff) 9e]s0 '51 PnIlnAbesHp) 20600 tlemH 3sn1 Vm151tl) 53.632 MalsNreCantemal9rack0aa,Owo Bwo fi.3]"k I6wo 9363% MolecularWelAF[ot5tack Gas,Ms Ma Aree olStack(enlertllamelerinlncM1eal,Fa Deplo-m o Wimh m Elameier 45 No.otGtacue 1 Aaa`WI o Aemla) 11.oan6523a
Su1lePressure,Pa 614c 11,OOC) Pa 29.53 FIELDDATq 9tMnma 1ss K-Fador= 2.3] 5b llmeI 1 105

AYn OeIhN Slaoklemo OGM ' DGM

1.100 1,cJ9 2604 311 64 2 1'001 1095 I.M. 312 69 64

I Cal 1.049 3 ].604 311 69 60 4 1 mal 1 a49 ].604 311 68 5 1 ID.1 1400 2367 311 71 65

1 1001 1449 311 ]2 65 7 0990 0 991 1.]43 309 ]1 6B
e 0690 0 943 2.107 306 75 69

1.200 1095 3340 ]] 70 10 1?00 1.095 2.ab 30e I] 13 11 1a0o 1.000 2.3W 311 76 13 12 1000 1000 3.367 310 79 79 13 1a 1s 16 1] 16 19 20
22 1B5>16 131565 29 qe¢ Av .SO 0 ~~~: VBlume ` ~ Dalle H Av TaIFI 't - Av MelerT

0]3 035 1 53]51 2541 69]50

mckGasVeloolN.VS.Ips Co 0.09 sqr(Eellapl 1-035 Ta 033 Vs ]1,930
Slaak Gas Flnwrzh. Os, acim Aa 1149465234 Oe 4]2v^3
Smok Gna Flnwrme r@ sTD. CBNO., O ry Oasia, Gattl. Oaltlltlacpml = 30c5i,96 Oattll

~ llrl = 180311664
VemallVaillu Noaale,Vn DIa.oMOssle 0.35 M(nossle): 0.0003q1 rmeolRnn 66 Vn 69.]fi
1ISOklne6q%I %I 96.40 YelsoMlnetic measuretltromlmermetllareValues bl 9F/]

PolMnt lu Mass Emisslon Ra@, PM0., Ibs.11n. Mn1g1 = o.000n0501 000001020 PMR Qbinr) = 0.D0037146 000)5661 PMR(Ibsncn)= O,n0001905 0.000056i] LEAO MENCURY Gralnsperact grlacl = 0.o00001 0 000602

or er per asn gnaacl = 0,o00001 O.o00oo6 Gralns permglGs[1 mgla9ct = 00610 0.00]1

Pollubn[ Mas Emlaalun 0.ate, PMR, Ibs.mr, Mn(A) ' 0.O60o]260 0.00000o34 PMR (Ib/nr) - 0.00536102 000002550 PMRIIbtlion)= 0.00027595 OLOOOO131 Antlmony Beryllium GrzlnsPera rla ct gcf = 000001< 0.000000

Grnlns Pertlaar a naaat = 0.000021 O,6m6o6
Gralns permAltlicl mplaam = 00151 O.0001

PollufamMasa Entlsslan Rare,PMR,Ibs.IM1r. MnIA) - 000000000 000000066 PMR (Iblbr) = O,OOOOOOOO oDO0o63]4 PMR(Ibanon) = 0.00000000 00000032] Arsenic Selenium Gralns peract Anan1 - 0 6o0oo0 O.o06000
Grains pertlsot Arlaset = O.o0o00o Bo0c00o
Grzlnz permgltlsct mgltlacl = 0.0000 0.0002 Leatl Mercury F111er 0 0 HNO3 5902 0 HNO3M2 H2SWMm 127 ROO CTON iolalug 5.932 13]

Tonslhr 19.5 LeaEblank MemuryDlanN R11 0 O HNw D9] HNO3IH2 H290alKm

~ TOaIUn 0

, 971 25

UG 1 5 012 102

Antimony Beryllium FIXer 0 HNC3 92 1,12 RNO31H2 0 25041Km O preoo c lo ]nslnA I n,j 1.12

TonslM1r 19.5 AlNmonyblenk BeIYIIlum9lenM

nor O 0 HNO3 194 0776 HNO3IH2 H2509IKm Totalllg 194 0]]6

UG s a 344

Arsenic Selenlum ercer o 0 HNO3 2.6 2,8 HNO3IH2 0 H25cLMm 0 PROOUCTION TotzluA fle 20

Tonslhr 19.6 qrsenloWanM 0e1e11vm9lana 0 HNO3 &BB 1 64 HNrRM2 H29O4Mm TrACUg 1 3,881 1.94
llG O O66PoIIWnlMassEmisslonRale,FMR,Ibs.IM. Cobalt CaEmIYm Mnlgl = 0.000001>1 0.00000066 Fiker 0 0 PMF (IblM1rl = 0.000121a9 c.00005]T4 HNO3 6 29 PMR(Ibshon) = 0.00000654 0.00000321 HNO3IH2 0 Coball Catlmlum H2504IKm 0 Glalnsperac/ PROUl1C O io1s1u0 5.fi 3a glac1 = 0.000000 0.000000 ianslM1r t9.5 CoballblanM Letlmlum 91enk G,alns perasuY Fiber 0 0
a baaar = o 000000 0060000 HNOa ]61 194 HNO2lnx Gnlna per m9/asm H23o9mm rngrEap = 0.o004 c IT.t.1U ] 881 1 94
pollotantMassEmisslon Rale PMR,Ibclht. UG 1.)2 0.06 Mnlp) ° 0.000001]2 PMR (Ib/br) = 0,00012]a6 0 0005054p CM1lomlYm Manganese PMftllbsflan) = 0.00000654 000002692 Fltter 0 0 Chromlllm Manganese HNO3 $c B76 Gralnsperac! HNO3/H2 0 grlad = 0.000000 0000002 H35O411(m 0 PRODUCTION Tohlug 66 B]6 Gralre pe,ESSI gbbscl = 0.000000 0000002 Tons/F! 19.5 Guomlumblenk Manganese 9lanit 0 0 Gminspermglasq HNO3 3Ba 1,94 m0laacf = 1o004 o.0oz1 HN09IH2 H250a/Km PolluCntMassEmisslonRate,PM0. 1Tota1U 3 881 1.94 Mn(0) = D DODGD172 000000000 PMR IlbiTr) = 0.0001x>46 000000000 UG 1.I2 6,82 1
PMRIIbsllonl = 0 00000654 LL00000000 Nickel Nickel crams peracl FiNer 0 0 grlaC = 0.000000 0000000 MNO3 56 HNO3/H2 Gralns pm Esct H2504/Km 0 Oelasel = 0000000 0.000000 1 PRODUCTION Totalup 58
Gralnz permglbscl Tons/frt IB.5 Nrtltalblenit m0/aacr = OOOOa O.o00a FOIe ~ 0 HNO3 ]ae HNO31H2 H3504IHm To1al U 3.00 0

G 1]2 031ack Gas Fhwrale, Oa, a<tm Aa 11.04465234 On 4Bfi

Shak Gaa Flowrale MSTD. CONO., Ory Baals, ositl. pa11 3o434 60 Osltlltlsc9M1r1 = 1326076.20
VelocltVal n1e NDxzle, Vn Ota.5lNOSle 025 An(nm21e1 0.000341 Tme o1 Run F. Vn 68]1
%ISOkInellqW°I

Y.ISOkIne4c meesoreCfremlmermmbtevaluea :61 a830
Pollulan[Mass Emisslan Rah,PMRlbslryr. Mnlg) = Da00a0xx9 nn0000]BO PMR (Iblbr) = n000100q] 0.0005809] PMkllballon) ' 0 OOOo0BE4 0.00002979 LEAO MERCURY Gralnz perecl pnan = o.a00000 ooa9a92

e per Lsa 9tlaacf = oo00om Do0o0o2 Gralnsparmglaact m9laa<1 = O.00aS o.001B

PollulantMeaa Emlaslon HaIe,PMR.lba.lryn Mn191 = Da0a0933] O.n00003]0 PMR Ilblhr) = oao6950B2 O.00OP5B9 PMRllbaltonl = 0.000356q5 D.o0001415 Antlmony Beryllium Gralns peracf prleal = oD0oo19 0000001
Gralnepertla5l gntlscf = 0.0000]] D000001
GraNS permelasn m9lae{ = 1.o192 0AOa6
PollutantMassEmissionRale,PMR,IbsJhr. Mnlg) = O.00Oam32 n0a003B65 PMR (IbIM) = O.00OSq52z na30944q PMR(Ibsnon)= 1O100996 0.00mqB43 Araenla Selenlum Gralnaperecl pr/acl = 0000001 0 Oo0000
Gmins perESCf 9r/oecl = 0.000002 Da0a011
Grzlns per m9lESq m9ltlanl = 40m5 000060 COMPNNYNHME' Generel31a1eB11ck LOCATION: Moor¢avlle,ln, SOURCETESTCn: kiln oATEarTEST: o2rotn2 RUNNO.: z POLLUTNNT: Me1a14Gaaee EnmrDam McleSmarWelphrclsfa<x Gaa,Dry 9asIa,ML bCC2 %O3 1].3 Mtl 3901R Volume af Waler Vapor Callecha l9! 9T0. COND., VV/v Vlo 15 VWlslpl 9.563

Volume ofOrV Gaa Cullechtl M 3iD. COND., Vm(s[41 Tm (FI ]4.333 Vm YVI PbfincryesH91 19600 aalla H 'L610 q ama m 002 vmrhal 14a4e
Molslure Contenlof5tack Gea,Dwa Bwo SB6% 1-RVro 8q14%° MolecularWelpMaf8ta5kGaa.Me Me 2B.3] preaalStacklenlerGlamehrinlncryeal.As oepP-m 8 wlallnm o aainehr qs rva.olsladn 1 AaILWt A<I61a1 11.04456234
5lallcPressme. Ps 9\atic 11.0001 Pe 29 53 Srsck GaaVeloclly,VS.lps DB4 aarGlena pl 1.Oq2 Tc 3a)]s0 Va ]1 626 FIELD OATN SIe

~ rlTlme 20a K

- Eanor= z.4o sloorme 3:0]

.=Runz De1hP'

~ 6 SuareDelpP

~ 'tVaNme OeIUN a5tackTem '-9GM "'OGM 1 1.10C 10q9 2.bqo 3n9 70 70 z v9a 1aq9 z.6ao 3De ]x 71

0990 0895 4.3]9 309 ]c 73 6 oa38 3cq z.z3z ]5 ]z 5 D.ecq x.z3x 309 ]B 73

1200 1.095 3.BB0 306 ]B 73 7 1.100 1 049 2640 30] ]5 74 6 1.100 1.049 3.640 307 15 74

1100 1.049 3.fid0 30> P ]3 10 1300 1095 2890 307 7/ ]5 11 I100 1.o49 2.6<0 507 ]] 75 12 1100 1,n95 2060 307 76 ]B 13 14 15 1fi 1] 16
20 x1 0203 23 165,655 24

Av s Dp d-Valuma Oe11aH SAV Ts(FI AJFMemiil

1.068 1042 6A020 2.fi10 3a]]50 ]4333

m

Leatl Mercury Flxer 0 HNO3 3.1a5 10.3 HNO3IH1 0 H39O41Hm 0 PRODUCTION Tolalup I 3205 10.3

Tons/hr 19.5 LeeE blank HpBlank Fllhr 0 O NNO3 09] 2.5 HNO0H2 Hx504Mm TofalU 097 25

UG 8

Antimony Rerylllum Fllrer 0 HNO3 112.7z 4.49 HNO31Hx a 29oqIKm 0 PROOUCTo To[alug I 112.72 Aqe

Tons/Fr 19.5 Anfimanyblank 9eryllium6lank Flner 0 0 HNa3 194 0.716 HNO3/H2 H2Sa41Km Total Ug I194 0]]6

UG I93,32 3]04

Arsenic selenium Filter 0 O NN0.9 112 40 6 HNO31112 0 H2Sa4IKm 0 PROOUCTION Totalu9 1t3 qoa

Tanslhr 19,5 Araen/cblanN SelenlumBlank Fmer 0 HNO3 3BB 1 gq HNO3/H2 H28oqIKm Total Ug 1 3 88 1.94

UG 1 7.32 38 86PalluhnlMass EmissionRare,PM0., ibs.lhr. M n ( p ) _ 0,80081852 000000828 CuEal[ CatlmlYm PMR Ilblhr) = 0.0013]e94 a00809]2 Filhr 0 PMR nbshonl = 0.0000]0]4 a0353] HNO3 224 11.2 Coball Catlmium HNO6IH2 0 Grzlns peracf H25O41Km 0 grlacl = 0.080884 0 000002 RODUCTION Toblu OAJ 112

Gralnspertlsal TonSIM 19.6 CoM1ah0lanR CaEmiumB/enh prltlscl = e ➢ 00005 0.000003 F111er 0 0 HNO3 ]Be 1,94 Gralns per mp/tlscf HNO3M1 mp/tlsaF = a0888 0.0019 H260C/Km T,talUO 9 66 1 5E Pallupn[Mass Ernlsslon Rete,PMR,l4a.lhr. M r (p) = 0,000010fi2 006341516 IUG 1 18.62 9.26 PMR (INnr) = 0.08137e0 4.72343781 PMR pbMcn) = e.eeoo]8]4 o0423Z159 Chromium Manganese CM1romium Manganese FlI1er o 0 Gralneperacf HNOI 234 6341],] pelecl = 0.000004 O.OtZt66 HNO3IH] 0 H2504IKm O erelns pm tlsct PFODUCTION Totalup 22 T7EPDl ].] Br/tlsd = 0000006 a018104 Tons/hr 19.5 CM1mmiumblenN Mangenece6lanh
Gralns Verm9laecf FRer o 0 mg/tlsol - a,8836 19.0292 HNO3 9,86 1.94 HNO31H2 PallutlntMass Embsion Ra[e.PMR,lbs.lhr. H2504IKm Mn(g) = 0.00001652 n80000090 Ta1d U 3 88 1.94 PMR Q6/nr) = 000131844 0,08000000 PMR(Ibsncn) = 0 o0007074 O.00OOOOOe luG 18,521 63415,76 ]
Nickel Gralnsperaal Nlckel gnaal = 0000004 O.oeeoeo Fltter 0 O HNO3 224 Gralns perJSCf HNO3M3 0 pr/tlsR = OOOOOa5 G000000 H26041Km 0 oOUCTION Ir. 'a 1 22,4 0 Grams parmglEecf mgltlssl = O,o038 00000 TonslM1r 19.6 Makelblanit Fi9er 0 FNOe ues HNN/H2 H2304Mm Total Ug 3 08 0

UG 8.52 0COMPANVNAME: GeneralSnaleOrlck LOCATION: Mooresullle.ln. SOnRGETE6TE0: Klln DATEOFTEET: 02101112 RIIN NO.: POLLIITpNT: Me1aISlGases Enrerpala MolesulerWelpM o151ack Gas,OryOasis,Mtl 6CO2 40] 113 Mtl %2
voiume atwaler va>or conecma

~ m GTG. GONG., Vwv Vlc 65.p Vwlsttll 3.100
vMeme cmrv Gas conemee A sTD. COND., vmptat TmIFI TSrzOB Vm 54.1a1 PEnnUea Hpl 29500
pa mma ? a B 2 Vmisltll 58442
Molelme CSnlent cl9tack Gas Bwo Bwo 141 1 0 1-cwo 9452%
Molcaular WeiBm o151acx Gas. Ms 2841 flreaot6task(enlertllameRrinlnchest,ps oeam-m o wiauln alamNei 45 Nc.ct9lacka AstLNVI 0 Aqala) 11.09465239
Slallc Pressura Ps smno n.9661 Ps Stacx GasVeloslly,Va.iGs Cc 0 Bd snntlelten) 1016 Ts 305 053 Vs 68653 9feckGas FloWrale,OS,aclm r685239 pa d616/ Slacx Gaa Flcwra[e tW STD, GONO.. Gry 9as15, Gattl. G51tl. 39B11 51 Osltlltlaormrl - 1]8906883
VeloclNatthe Noaxle.Vn OIa.olNome O.rzS rmeclRun Vn 6/13 Mlncsslav o.0oa391 FIELOOATA K-Facior= 3.d0
' r. ' • _ ....,...

Q

~ ~~_~!~

~ ®

®

.. •. . .®•. • '®' ' ' ~'~' ~' ® ~'
~~ -®

%Isoxlnetic,W.l %I %Isoxlnellc measuretlM1omintermaLlalevalues %I 9/19
polluttnlMass Emisslon Rare,PMft,Ibs.IM1r. Mnlg) ` 0001]1 O.00000955 PMR 9nlnr) = 0.0001]635 0.00065500 PMR(Ibvnon) = 0 0000069c 00001TI2 LEAG MERCURV Gralns perec/ gr/aer = 0 000000 0.000001

GralnsPerGS<1 9naaal . = 0.000000 0000001
Gmins Germolaael mgltlacl = O,OOOd 0.0009

PclluOnrMaes EmisslonRate,PMft.lOS.lhr. Mn19) ° 800010550 o00421 PMR (I6IM1n = 00]]]140 0.00091100 PMR 9naM1On) = 0.00039B53 0.00001695 Antimony Berylllum OralnsPeracl grlaq = 8000021 0.000001

Gralns Pertlsc! Pr/tlsq = 0000030 0.000001

Grzlns Perm9/tlssY maltlscl = 0.0219 00009
PollulantMass emisslon RaIe,PMR,IGs.lhr. MI = OOnn0oB59 0.00005323 PMR pEmO = a o0oc3396 oo03ezc5o PMR ~ Lsitrnl = 0.00003]51 000020146 Arsenic Selenium GAlns peracl 9rlavt = 0000002 O.000010
Gralns perEsct ONtlaof - 0L00002 c,000015
Graina perm9lESC1 m9laaar = 0.00+6 80111 Leatl Mercury Flldr 0 0 HNO3 2602 1.05 HNO3IH2 0 Hrz909Mm 0 PROOUCTIO Totelug a6B2 ]A5

Tanslhf 19.5 LeatlNenk Ng9lanlr
mer 6 0 HNO3 LL9] 5 03IH2 H2GOd/Km NOW ug 1 0.0 25

UG I1]12 4.55

AnSlmanY Beryllium FINer 0 0 HNo3 124] 4.99 HNO3IH2 0 H2GOdIKm 0 P O CTION ToMU 1247 499

Tuns/hr t9.5 Anr]monyblanh Beryl11um9lanM Flltar 0 0 HNO3 1B 4 0.1 7 6 HNO3IN] H230d/Km TUW1 Ug 194 0]]6

UG 1053 4214

Arsenic Selenlum D er a 0 HNm 12.41 55.17 HNO3IH2 0 H2909Mm o pRODUCTION Tmalug 1217 5517

Tonslhr i9.6 Arsenlcblan4 SelenNm9lanh Fiker n 0 HNOI 36B 1 9 4 HNOyH2 H2GOdIKm Total U 366 1.94

UG 1 8591 5323PollursntMessEmisslonftar6 PMI{IbxlM1r. Mn(p) y 0OOOc106 0.00001053 CDE31t Catlmlurrl PMR (IbIXr) = 0.00155428 0.000'P)14 F111er 0 PMR(Ibshcn) = 0.00CC]9]1 r 1.1.111, HNO3 24.94 12,47 Cobali Catlmium HNOaM2 0 Gralnsperacf H]504Mm O gr/ecl = 0 000004 0.000002 PRO CTION Tclalu9 24 94 12,41

Gralnspertlscf TonslM1r 19.5 Ccbellblank Cetlmlum Blanh
9rmsol = O0000ae O.00OOW Flrcar o O HNOS e,ee 1.94 na permglascl HNG9IH2 m9lascf = Oca44 1.w22 H2sa4Mm Trial Ug 3bill 1.94 FoIlrltantMass EmisslonRate,pMR,Ibs.IN,

- o ( g ) = 0.00003106 0.00000692 I UG I 21.06 10.53 PMR (Ib/b) - 0,110151425 0.00050333 PMRIIbsllon) = 0.0000]g11 1.1000259f Cllrernlum MaIlQaneSe ObromWm Manganese Filter g 0 Gralns peracl HNO3 3494 9.76 grlacf = 0.000004 0000010 HN09IH2 0 H2504/Km 0 GralnsperESCf PRODUCTION ictalug 2a 941 Ye gr/tlscl = 0000006 0000002 TonalM1l' 19,6 Chrommmblank Mangen se BIanX Gralns permglCacl Filler 0 0 mgltlsC = 00044 00108 HNO3 ] 0B 1,94 HNO3IH3 PolluhntMacs EmisslonRatq PMR,Ibslbr, H2S01/Km Mn(p) ' 000002100 0.01100010 T0131Ue 3 96 1 94 PMR (Ib/bi) — 0,00155429 O.00OOOCDO PMR Ilbs/1on) = 0.0000i911 0 00000000 UG 21.66 6.62 Nickel Gralns peracf Nlckel grlacr = 0 o0aoo4 O.o00000 Flttar 0 0 HNO3 2<.94 Grainspertlscf HN93IH2 0 gr/tlscl = 0000006 c.oc0000 H2504IKm 0 PRODUCTION iomlug 9494 emins permpltlscf mg/tlsc! = 0.c044 00000 ioms/br 19.5 NicltelblanR bar o D HNO3 HNO3M2 H2504Mm TOfdUO 5BB 6

UG 2106 O

### STACK EMISSION SUMMARY
SOURCE TESTED: Kiln-Outlet COMPANY NAME: General Shale DATE OF TEST: 02/01/12 

### * 

### Av

. 

### of Runs 2& 311! Pollutant Emissions Run 1 

# I Run 2 Run 3 Average HCL (Ibs/hr) 154.7128 2.4154 0.3539 1.3847 HF Ibs/hr) 1.5411 1.6949 1.1284 1.4117 CL2(Ibs/hr) 31.4399 0.4436 0.0549 0.2492 Avg. Stack Vol. Flow Rate ACFM 41,230.85 45,13102 42,416.50 42,926.79 DSCFM 26,307.78 29,217.00 27,517.57 27,680.78 Avg. Stack Temp. 308.583 304.083 299.583 304.083 Stack Gas Velocity 62.218 68.107 64.008 64.778 Avg. Velocity Head 0.8214 0.9910 0.8792 0.8972 Avg. S. Rt of Delta P 0.9063 0.9955 0.9377 0.9465
ISOKINETIC TESTING SUMMARY

%Isokinetics: 100.97 99.09 102.62 100.90 Allowable isokinetic 90-110% 

### % Moisture of Stack Gas 6.28% 5.47% 5.82% 5.85% Sample Volume 49.177 53.599 52.277 51.684FIELOOATA SfaN:Tlme 145 K-Factor= 2.3] $(o

~ Time'. 4:50

l Avg. b< Ayq.Sq. Do Volume Delta H 

# I Av .!Ts Fl I Av . Meter T F : ~ 0.842 0.906 53.670 1.992 308.563 59.]50 OOMPANyNAME: GeneralShale LOCATION: Mooresville SOURCETE3TED: Kiln-Outlet DATE OF TEST: 02I01/12 RUN NO.: 1 HCIJHF/CL2 Malecular WeigM1t ofStack Gas, Dry Basis, Md %CO2 3 %02 1] Mtl 29.16

Valume ufWa[er Vapor Collectetl (A STD. COND., Vwv Vlc ]0 Vw(sttl) 3.293 Volume of Dry Gas cuneeted Q srD. COND., Vm(atrl) Tm(F) 59.750 Vm 53fi]0 Pb(Inches Hg) 29.600 deltaH 1.992 gamma 0.904 Vm(std) 49.177
Moisture Oontent of Stack Gas, Bwo Bwo 6,28% 1-Bwo 93 ]2%
Molecular Weight Df Stack Gas, Ms Ms 28.46 Area of Stack (enter tliameter in incM1es), qs DeptM1 in 0 Width-in 0 tllemeter 45 No. of 61acFs 1 As(L't ) 0 As(tlia) 11.04465234
Static Pressure, Ps 6tatic (0750) Ps 29,54 Stack Gas Velocity, Vs, fps Cp 0.04 sqr(delta p) 0.906 Ts 308.583 Vs 62218
Stack Gas Flowrate Os, acfm As 11.04465234 Os 41231 Stack Gas Fluwrate @ STD. COND., Dry Basis, Ostd. Ostd(dscf/m) = 2630]]8 Osttl (tlsoflhr) = 1578466.84 Velocity at the Nozzle, Vn Dia. of Nozzle 0.25 Time of Run 60 Vn 62.82
%ISokinetic, %I °hl 100.9] %Isakinetic measuretl frvm In[ermediate values %1 101.36
Pollutant Mass Emission Rate, PMR, Ibs./hr. Mn (g) = 2.1064 0.0218 PMR (Iblhr) = 154.7128 1,5411 PMR (Ib/MMBtu) = 5.1363 0.0512 LCL H Grains per acf gnaci = 04646 0.0646 0.10]5 An(nozzle): 0.000341

0.444299 31.4399 1.0438 CLI

00944
Grains per tlscf gpdscf = 0.6860 00068332 0.139406 Grains per mgldscf mg/dscf = 4956]]4 4.93]4 100.7386COMPANY NAME: General Shale LOCATION: Mooresville SOURCE TESTED: Kiln-Oullet DATE OF TEST: 05126/11 RUN NO.: 2 POLLUTANT: HCl/HFICL2 EnterData Molecular WeigM1t of Stack Gas, Dry Basis, Mtl %CO2 3.5 %02 1],3 Md 29.093 Volume of Water Vapor CDllected gD STD. COND., Vwv Vlc 65 9 Vw(sttl) 3.100 Volume of Dry G. Collected @ STD. COND., Vm(sttl) Tm(F) 6B.167 Vm 59391 Pb(InchesHg) 29600 tleltaH 2347 gamma 0.904 Vm(sttl) 53599
Moisture Gontent of Stack Gas, Bwo Bwo 5.4]% i-Bwo 94.53% Molecular Weight of Stack Gas, Ms Ms 28.49 Area of Stack (enter tliameter in tnches), As Depth-in 0 Widm-In 0 diameler 45 NO.ofStacks 1 As(CV ) 0 As(dia.) 11.04965234
Static Pressure, Ps Stetic (0750) Ps 2954 Stack Gas Velocity, Vs, fps Cp 0.84 sqr(delta p) 0.995 Ts 304,083 Vs 68.10]
Stack Gas Flowrste, Os, acfm As 11.04465234 Os 45133 Stack Gas Flowrate Oq 9TD. COND., Dry Rasls, Ostd. Ostd. 29217.00 Ostd(tlscflhr) = 1753019.96 Veloclty at the Norzle, Vn Dla. of Nosle 025 An(nozzle) 0.000341 Tlme of Run 60 Vn 6749
% Isokineflo, %I %1 99.09 %Isakinetic measured from intermediate values %1 99.4]
Pollutant Mass Emission Rate, PMR, Ibs.lhr. Mn (g) = 00335 0.0235 0.D06152 PMR (Iblhr) = 2.4154 16949 0.4436 PMR (IbIMMBtu) = 0.0182 0.0549 00144 XCL HF CZI Grains per aef gtlad = 0.0066 0.0046 0.0012 FIELDDATA &fadTlma 8.15 K-Fac[or= 2.J] S1bTime 11:10

RUn2 DeIWE S uareDelte'P Volume DeItaH2 I Stack Temo DGM DGM 1 0950 0.975 2.249 1 304 1 69 66 2 0.950 0.975 2.269 304 69 66 3 095D 0.975 2.2<9 304 70 66 4 1 000 1000 2.367 305 70 66 5 0950 0.975 2.269 304 70 66 6 1.100 1049 2.604 305 70 66 7 1.100 1.049 3.603 305 70 66 B 0.950 0975 2.349 305 70 66 9 0.950 0.975 2.249 305 ]D 66 10 1.000 1000 2.96] 3D4 72 66 11 1.000 1.000 2.367 302 72 66 12 11100 1.000 2.367 302 72 66

1041.]24 982,333

Av .-0 " Av .5 .O I Volume :- fxitaH Av .TS F = Av . MetwT F 0992 0.995 59,391 2.34] 304.083 68.16]

Gralns per dscf gpdscf = 0,0096 0.006766925 0.001]]1
Grains Per mgldscf mgltlscf = 6.9492 48762 1.2762COMPANY NAME: Gener'el Shale LOCATION: Mooresville SOURCETESTED: Kiln-Outlet DATE OF TEST: 05126111 RUN NO.: 3 POLLUTANT: HCL/Hf/CL2 Enler Data Molecular Weight of Stack Gas, Dry Basls, Md %CO2 2.5 %02 17.3 Mtl 29092 Volume of Water Vapor Collectetl @ STD. COND., Vwv Vlc 68.7 Vw(std) 3,232
Volume of Dry Gas Collectetl L ID STD, COND., Vm(sttl) Tm(F) 60.542 V. 56,106 Pb(lnahes Hg) 29.600 tlelta H 2091

. gamma 0904 Vm(sttl) 50565
Molsture Content of Stack Gas, Bwo B. 6.01% 1-Bwo 93.99% Molecular Weight of Stack Gas, Ms M. 28.43 Area of Stack (enler tliameter in inches), As Depth-in 0 Witlth-in 9 diameter 45 No. of Stacks 1 A6(L`W) 0 As(dlaJ 11.0446523
StaHc Pressure, Ps Static (0750) Ps 29.54 Stack Gas Velocity, Vs, fps Cp 0.84 sqr(tlella p) 0938 Ts 299.583 Vs 64.031
Stack Gas Flowrate, Os, acfm As 11 0446523 Os 42432 Stack Gas Flowrate @ STD. COND., Dry Basls, Clstd. Ostd. 27473.35 Osttl (tlscf/hr) = 1648401.08 FIELDDATA K- Factor = 2.39 StartTime 1230 Sto Timo` 3:30

Run3 DeltaP I :SuareDeltaP Volume DeItaH2 StackTemp DGM 1 0.550 0.742 1.302 278 68 2 0800 0.094 1.894 303 60 3 0.850 0.922 2. 0 12 303 68 4 0.950 0.975 2.249 304 70 5 0.950 0.975 2.249 304 70

q68 6 0.950 0.975 2.249 304 70 7 0.9 0 0 0.949 2.130 300 70 8 0950 0.975 2.269 301 70 9 0.900 0949 2.130 302 70 10 0.900 0.949 2.130 302 70 11 0950 0975 2.249 297 70 12 0.950 0.9751 2.349 1 297 70 68

1098 355 1042.250

Av.D

~ AV S.D -'VOlume ':DeltaH Av.TS I Av.MeterTF 0,8831 09381 68 542

Velocity at the Nozzle, Vn Dia. of Nozzle 0.25 An(nozzle) 0.000341 Time of Run 60 Vn 63.66
% Isokinetic, %I %1 99.42 % Isokinetic measuretl from intermetliate values %1 99.80
Pollutant Mass Emission Rate, PMR, Ibs./hr. Mn(g) = 0.0051 0.0162 0.000788 PMR (Ib/hr) = 0,3653 1.1648 0.0566 PMR (Ib/MMStu) = 00126 0.0401 0.0020 XCL NF CL1 Grains per acf grlacf = 0.0011 00034 0.0002 Grains perdscf gr/tlscf = 0.0016 0.004946 000024 Grains par mg/tlscf mg/tlscf = 11308 3.6054 0.1753

### General Shale Brick, Inc Proj ect Number: 141.11



# APPENDIX III

FIELD DATA

Wilcox Environmental Engineering, Inc. Air Analysis Division10 11 12 Kiln Outlet

Mooresville, In.

41 61 81 10 12 45 3.02 1.98 1.44 

### 1 1.17 0.95

11.25 6.57 4.73 3.69 3.02 33.75 13.32 8.73 6.57 5.31 41.99 31.68 14.54 10.17 7.97

38.43 30.47 15.39 11.25 43.02 36.27 29.61 16.02

40.28 34.83 28.98 4156 38.43 33.75

41.31 37.04 43.83 39.69

41.99 44.06 VELOCITY TRAVERSE POINT DETERMINATION (EPA Method 1)

General Shale Brick @ Circular Stack Taverse Points on Diameter: Stack Dia.(inches)? Points:

45" I.D.

A=252"

B=420"l

~

.~ 

### 9

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~ 

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### General Shale Brick, Inc Project Number: 141.11



## APPENDIX IV

CALIBRATIoN DATA

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## Wilcox Environmental Engineering, Inc. Air Analysis Division
PITOT TUBE CALIBRATION Reference: 40 CFR 60, Appendix A, Method 2, Section 2.1



### Calibration Date: 

### January 7th, 2012
Probe Number/ID: 

### FIVE (5) FOOT PROBE E6cternal Tubing Diameter 

### 0.95 cm Base to Opening Plane Distance (Pa) 

### 1.25 cm Base to Opening Plane Distance (Pa) 

### 1.25 cm

Measured --._ 

### A//owab/e

Pb/Dt 1.32 cm 1.05Dt <_ 1.5Dt 0.9975cm 

## — 1.42cm

Ps/DT 1.32 cm 1.05Dt <_ 1.5Dt 0.9975cm 

## — 1.42cm

An le a 1 1 deg a 1 and a 2:5 10.0 De rees

An le a 2 1 deg a 1 and a 2<— 10.0 De rees

An le 

## P 1 0 deg 

## p 1 and 

## P 2<— 5.0 De rees

An le 

## P 2 0 deg 

## p 1 and 

## P 2:5 5.0 De rees

Z cm 0.0 Z is less than 0.32cm 1/8 tn "



### W cm 0.0 W is less than 0.08cm 1/32 ndn If all criteria are met, Pitot Coeffcient is 0.84 Pitot Coefficient: 0.84

Contro/ Factor Mercur Thermometer °P Probe Res onse ICE 

### 32 0 34 0
AMBIENT 

### 60 0 57 0 HOT BATH/H20 

### 250 0 253 0

Signature 

## Joseph B. Kinder Date 

### January 7 th , 2012

## Wilcox Environmental Engineering, Inc. Air Analysis Division
PITOT TUBE CALIBRATION Reference: 40 CFR 60, Appendix A, Method 2, Section 2.1



### Calibration Date: 

### January 7th, 2012
Probe Number/ID: 

### SIX (6) FOOT PROBE A External Tubing Diameter 

### 0.95 cm Base to Opening Plane Distance (Pa) 

### 1.25 cm Base to Opening Plane Distance (Pa) 

### 1.25 cm

Measured A//owab/e

Pb/Dt 1.32 cm 1.05Dt <_ 1.5Dt 0.9975cm 

## — 1,42cm

Ps/DT 1.32 cm 1.05Dt <— 1.5Dt 0.9975cm 

## — 1.42cm

An le a 1 1 deg a 1 and a 2!5 10.0 De rees

An le a 2 1 deg a 1 and a 2:5 10.0 De rees

An le 

## P 1 0 deg 

## p 1 and 

## P 25 5.0 De rees

An le 

## P 2 0 deg 

## p 1 and 

## 0 2:5 5.0 De rees

Z cm 0.0 Z is less than 0.32cm 1/8 th,

W cm 0.0 W is less than 0.08cm 1/32° a " If all criteria are met, Pitot Coefficient ie 0.84 PItOt COeffltient: 0.84

Contro/ Factor Mercury Thermometer °F Probe Res onse ICE 

### 50 0 50'
AMBIENT 

### 71 0 70 0 HOT EATH/H20 140 0 140 0



### Signature 

## Joseph B. Kinder Date 

## January 7` i ', 2012

### General Shale Brick, Inc Proj ect Number: 141.11



## APPENDIX V

LABORATORYDATA

Wilcox Environmental Engineering, Inc. Air Analysis Division

# Wilcox Environmental

Engineering, Inc.

5757 West 74 th Street Indianapolis, IN 46278



# General Shale Client # 141.11


# Analytical Report (0212-68)

EPA Method 2" (NaOH Matrir) Chloride 

# EPA Method 2" (H 2 SO 4 

# Matrix) Hydrogen chloride, Hydrogen fluoride



# Enthalpy Analytical, Inc. Phone: (919) 850 - 4392 / Fax: (919) 850 - 9012 / www.enthalpy.com

800-1 Capitola Drive Durham, NC 27713-4385 

# m

### I certify that to the best of my knowledge all analytical data presented in this report: • Have been checked for completeness • Are accurate, error-free, and legible • Have been conducted in accordance with approved protocol, and that all deviations and analytical problems are summarized in the appropriate narrative(s) This analytical report was prepared in Portable Document Format (.PDF) and contains 122 pages.

Y 

## QA Review Perfornied by — Valgena Respass

Report Issued: 02/28/2012

F'' 

# 0 

# M OU

EA# 0212-68 Page 2 of 122

# Summary of Results

F' 

# 7
~ O 

# A

EA# 0212-68 Page 3 of 122Company Wilcox Env Engineering Client # 141.11 Analyst EDE Job # 0212-68 Parameters EPA Method 26A # Samples 6 runs & 1 blank



### und

Hydrogen Fluoride Hydrogen Chloride

Hydrogen Fluoride Hydrogen Chloride 

## Outlet-R1-H2SO4 21,778 2,186, 355

C3-R1-H2SO4 70,991 13,554 Outlet-R2-H2SO4 23,506 33,499

C3-R2 H2SO4 73,656 19,441 Outlet-R3-H2SO4 16,207 5,083

C3-R3 H2SO4 94,495 24,504

Blank-H2SO4 Hydrogen Fluoride 

## 105 ND Hydrogen Chloride 

## 175 ND

0212-68 H2504_m26a Results 2/27/2012 EA# 0212-68 Page 4 of 122Company Wilcox Env Engineering Client # 141.11 Analyst EDE Job # 0212-68 Parameters EPA Method 26A # Samples 6 runs & 1 blank



## Outlet R1-NaOH Outlet-R2-NaOH Outlet-R3-NaOH Chloride 444,299 6,152 788

C4-R1-NaOH C4-R2-NaOH C4-R3-NaOH Chloride 695 133 J 87.0 ND

Blank-NaOH Chloride 35.8 ND

0212-68 NaOH m26a Results 2/27/2012 EA# 0212-68 Page 5 of 122

# Results



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❑ 

## _

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~ 

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## O N O Q L ° U 

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## J p Q E

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# Narrative Summary



# ~

EA# 0212-68 Page 13 of 122

# Entbalpy Analytical Narrative Summary

Company Wilcox Env En ineerin Analyst EDE Parameters EPA Method 26A Client # 

### 141.11 Job'# 0212-68 # 

### Samples 6 Runs and 1 Blank
Custody Lindsey Chatterton received the eamples on 2/10/12 after being

relinquished by Wilcox Environmental Engineering, Inc (formerly Astbury Environmental Engineering). The samples were received at 12.7°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 hydrogen chloride and hydrogen fluoride using the analytical procedures in EPA Method 26A,

Determination of Hydrogen Halide and Halogen Emissions from Stationary Sources Isokinetic Method (40 CFR Part 60, Appendix A). All samples and standards are prepared, stored, and analyzed using high-density polyethylene containers. The Metrohm 861, High Performance Liquid Chromatograph ("Mr Burns" S/N 1861004003180) was equipped with a Metrohm 861 Conductivity Detector and a Metrosep A Supp 5- 110/4.Omm (S/N # 7908297) column.
Calibration The calibration curves are included in the Calibration Curve

Chromatograms section of this report and referenced in the Analysie Method column on the Detailed Results page. For each calibration curve used, the first page of the eurve contains all method specific paraineters (i.e., eurve type, origin, weight, etc.) used to quantify the samples. The calibration curve section also includes a table with the Retention Time (RetTime), Level (Lvl), Amount (corresponding units), Area, Response Factor (Amt/Area) and the analyte Name. The calibration table is used to identify (by retention time) and quantify each target compound. Chromatographic "The acquisition method (METROHM.M) is included in the Calibration Conditions Curve Chromatograms section of this report.

EA# 0212-68 Page 14 of 122

# Enthalpy Analytical Narrative Summary (continued) QC Notes The samples were analyzed within the 4-week holding time specifled by

the method. The analyses of the field and laboratory reagent blanka did not contain hydrogen fluoride or hydrogeri chloride at concentrations greater than the detection limit. Duplicate matrix spikes were prepared using aliquots of sample C3-RIH2SO4 and exhibited spike recovery values of 99.4% and 97.9% for hydrogen fluoride and 90.4% and 91.0% for hydrogen chloride. The analysis of the second source standard was also used as the LCS and exhibited a spike recovery values of to 102% for hydrogen fluoride and 96.8% and 97.4% for hydrogen chloride. A confirmation analysis was performed on satnple Outlet-RI-H2SO4 to confirm the high hydrogen chloride result. Reporting Notes The H 2 SO4 matrix samples were analyzed for Cl- and F- but are

reported as HCl and HF. The results were converted using an acid conversion factor of 1.028 for HCl and 1.053 for HF. 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.



# u EA# 0212-68 Page 15 of 122

# Enthalpy Analytical Narrative Summary

Company Wilcox Env En ineerin Analyst EDE Parameters EPA Method 26A Client # 

### 141.11 Job # 0212-68 # 

### Samples 6 Runs and 1 Blank
Custody Lindsey Chatterton received the samples on 2/10/12 after being

relinquished by Wilcox Environmental Engineering, Ine (formerly Astbury Environmental Engineering). The samples were received at 12.7°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 chloride using the analytical procedures

in EPA Method 26A, Determination of I-Iydrogen Halide and Halogen Emissione from Stationary Sources Isokinetic Method (40 CFR Part 60, Appendix A).

All saniples and standards are prepared, stored, and analyzed using high-density polyethylene containers. The pH of the NaOH fractions as measured at the laboratory were 3 or less, except for the field blank, which was at pH 14. The Metrohm 861, High Performance Liquid Chromatograph "Mr Burns" (S/N 1861004003180) was equipped with a Metrohm 861 Conductivity Detector and a Metrosep A Supp 5- 110/4.Omm (S/N # 7908297) column, for these analyses. Calibration The calibration curves are is included in the Calibration Curve

Chromatograms section of this report and referenced in the Analysis Method column on the Detailed Results page. For each calibration curve used, the first page of the curve contains all method specific parameters (i.e., curve type, origin, weight, etc.) used to quantify the samples. The calibration curve section also includes a table with the Retention Time (RetTime), Level (Lvl), Amount (corresponding units), Area, Response Factor (Amt/Area) and the analyte Name. The calibration table is used to identify (by retention time) and quantify each target compound. Chromatographie The acquisition method (METROHM.M) is included in the Calibration Conditions Curve Chromatograms section of this report. 

# M

EA# 0212-68 Page 16 of 122

# Enthalpy Analytical Narrative Summary (continued)
QC Notes The samples were analyzed within the 4-week holding time specified by

the method. The analyses of the field and laboratory reagent blanks did not contain chloride at concentrations greater than the detection limit. Duplicate matrix spikes were prepared using aliquots of sample 

### OutletR2-H2S09 and exhibited spike recovery values of 92.4% and 91.9%. The analysis of the second source standard was also used as the LCS and exhibited a spike recovery value of 97.0%. A confirmation analysis was performed on sample 

### Outlet-Rl-NaOHto confirm the high chloride result. Reporting Notes These analysea 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.

P' 

# 157 Ar O

d Ad EA# 0212-68 Page 17 of 122

# 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 detennine 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 iuterest 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 analytc 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 talcen from a taboratory 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 lmown amount of analyte so that a percent recovery value can be determined. This shows what effect the sainple 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 Spilce 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 perfonning 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 tlie Sample ID represents an Alternate Dilution. The analyst prepares an additional aliquot af a different dilu6on factor (usually double the initial factor). This analysis helps con£irm 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 1D 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 con£irm that the analyte could be recovered from the media, separate from the samples whicb were used on the project and which may have been affected by source matrix, sample collection and/or sample transport.



# ~

EA# 0212-68 Page 18 of 122

# 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 incorrectly by 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.



# ~

EA# 0212-68 Page 19 of 122

# Sample Custody

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EA# 0212-68 Page 20 of 122~ 

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Chromatograms



# ~

EA# 0212-68 Page 23 of 122Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\051-3401.D Sample Name: Outlet-R1-H2SO4*100 0212-68

Acq. Operator 

## __ ___________________ : EDE Seq. Line 34 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 9:59:44 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC(37PG0 0610 51-34 01.D) uS/cm 90 

## 80
70 60 I II : 50 I I~i 40-I D

o ~ 30 i 20l 10

..... ✓ t ~__ _,__ ........ _...--__ ...... ....... .... --, 0 2 3 4 5 6 7 8 9 min



## =========-__---_--__---____--_- External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDe Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

## [min] [uS/cm*s] [ug/mLj 

# ------- I ------ I ----------I---------- i ----------I ------------------ 3.042 BB 51.23235 1.49259e-2 7.64689e-1 Fluoride 4.929 e"' -4 ' ~ Re ort From A[t¢rnate Di[ution EDE 

## I P ~ Totals : 7.64689e-1

1 Warnings or Errors : Warning : Calibrated compound(s) not found



## ----------------------------------------- *** End of Report ***

Eli Ellis 2/20/2012 9:52:39 AM Eli Ellis EA#0212-68 Page24of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\051-3402.D Sample Name: Outlet-Rl-H2SO4*100 0212-68



# ________________________________ ________________________ Acq. Operator : EDE Seq. Line 34 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 10:12:04 AM Inj : 2 Aoq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE

. Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\051-3402.D) uS/Cm 

## 90 7 80 y

~ 70 i 601 , 

## 50 i I I 

## 40
~ 

## I 30

20
10 -1 S.,_ ~

~.~_~_ i

—~ i..... .._....— —._.._—
......... ,J.....

...... -:.-. ~ 

## o- .-- 2 3 4 5 6 7 8 9 min

External Standard Report 

# ----------------------------------------- — - Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

## [min] [uS/cm*s] [ug/mL] 

# - - -I------ I ---------- I---------- I ---------- 1--i------------------ 3.043 BB 51.30753 1.49264e-2 7.65836e-1 Fluoride Re ort From Alternate Dilutian (EDE 

## Totals : 7.65836e-1
1 Warnings or Errors :
Warning : Calibrated compound(s) not found



## -------------------------------------------- *** End of Report ***

Eli Ellis 2/20/2012 9:52:48 AM Eli Ellis EA# 0212-68 Page 25 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\052-3501.D Sample Name: Outlet-R1-H2SO4*10000 0212-68

___ 

# ______________ ________________ Acq. Operator : EDE Seq. Line : 35 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 10:24:23 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Laet changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNB\DATA\FE8\HPLC67PG006\052-3501.D) us/cm i 80
70 - I 60- 50 ~I ~ I 40-
30 - 0

20
10 0

.._...-.... ".. 0 ,- I
- T

-

_ --- r~~~ - 2 3 4 5 6 7 8 9 min



# ------------- ------------------------ ____ ----- _________ External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDS Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------I---------- I ---------- I ----------I ----------------- Re ort From Alternate D[lution (EDE 4.048 BB 31.41202 2.49376e-2 7.83341e-1 Chloride
Totals : 7.83341e-1

1 Warnings or Errors : Warning : Calibrated compound(s) not found

------------------------------------------------------------------- *** End of Report ***

Eli Ellis 2/20/2012 9:53:01 AM Eli Ellis EA#0212-68 Page26of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\052-3502.D Sample Name: Outlet-Rl-H2SO4*10000 0212-68

Acq. Operator : EDE Seq. Line : 35 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 10:36:43 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC 1 A, ADC1 CHAN NEL A(H:\HPLC2012Q 1\M R BURNS\DATAIFEB\HPLC67PG006\052-3502.D) uS/cm 

## ~ 90 

### 80

I 70
60 - 

### I ' 50 ; 

### ~
40 

### ~

~ I 

### 30 ~ 0 I 

### 20

~ 

### v 0



### __ 0

r 

### . 2 3 4 5 6 7 8 9 mi 

### n



## __ _ _- -----

External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I---------- I ---------- 1--i------------------ Re ort From Alternate Dilution (EDE) 4.047 BB 31.78193 2.49220e-2 7.92070e-1 Chloride


### Totals : 7.92070e-1

1 Warnings or ErrorS : Warning : Calibrated compound(s) not found



### _----------------- - - -- -- ----- - — ------ ---- - -- -- - - ---- --- --- - *** End of Report ***

Eli Ellis 2/20/2012 9:53:10 AM Eli Ellis EA#0212-68 Page27of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\053-3601.D Sflmple Name: Outlet-R2-H2SO4*10 0212-68

Acq. Operator 

# _______________________________________ : EDE Seq. Line 36 Acq. Inetrument : Mr_Burne Location Injection Date : 2/17/2012 10:48:03 AM Inj ; 1 Acq. Method : C:\HPLC2011Q4\MR BIIRNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:53:40 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

### ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\053-3601.D) uS/cm 90 i 80 70 `o

0 60 LL ~o I 50- c `o

O L 40- m U a 30 ; ~i m I 20 i 0

~

......_
__ , -,.. _..—_.. _.... ~ 0 ~_ . _~~_7T..7__~___r._~_.r__,_.__~ r_~__-_7_T~.__T 2 3 4 5 6 7 8 9 min



# __________________________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [miri] [uS/cm*s] [ug/mL] 

# ------- I ------I----------I---------- I ---------- I--i ------------------ 3.043 BB 528.78070 1.52311e-2 8.05391 Fluoride 4.340 BB 500.31830 2.36833e-2 11.84919 Chloride

Totals : 19.90310



# --------------------------------------------------------------------- *** End of Report ***

Eli Ellis 2/20/2012 9:53:44 AM Eli Ellis EA#0212-68 Page28of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\053-3602.D Sample Name: Outlet-R2-142SO4*10 0212-68


# _______________—__-____

_ 

# _ ___________ Acq. Operator : EDE Seq. Line : 36 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 11:00:23 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:53:40 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\053-3602.D) uS/cm 

# I 

# ~ 90 80

v

J 70 o 0 60 ~ ~ J

~ o 

# 50 N 

# ° O L M U 

# 40 n 30- ~ 

# °

~ 

# I

n i 20 i N 10 N /

0 3 4 5 B 7 8 9 min



# ____________ ____________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Uee Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I------ ---- I------ ---- I ---------- 1--I----- ------------- 3.025 BB 536.09320 1.52315e-2 8.16553 Fluoride 4.305 BB 500.36551 2.36833e-2 11.85030 Chloride

Totals : 20.01583



# _______—_



# ____________ _______________ *** End of Report ***

Eli Ellis 2/20/2012 9:53:54 AM Eli Ellis EA# 0212-68 Page 29 Of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\055-3801.D Sample Name: Outlet-R3-H2SO4*10 0212-66

____ ____________________ Acq. Operator : EDE Seq. Line 38 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 12:01:20 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:54:34 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

ADC1 A, ADC7 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FE6IHPLC67P6006\055-3801.D) uS/cm 90 80 I 0 70 °-
60, LL 50 o I

M ~ 40 I ~ o 30;

~ U
20 0 o 

# ~ M I



### . ._. _.... ,._._ a 

### /

_ _ .____.__ .._._ ..._. .._.... . 0 .- I --- ~ 2 3 4 5 6 7 8 9 min



## __ ___-___-________________________ External Standard Report

Sorted By

. signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------ I ---------- I ---------- I ---------- --1------------------ 3.031 BB 503.64569 1.52295e-2 7.67026 Fluoride 4.300 BB 102.28159 2.40103e-2 2.45581 Chloride

Totals . 10.12607

----------------------- — ---- ----- - ---- --- - --- - *** End of Report ***

Eli Ellis 2/20/2012 9:54:37 AM Eli Ellis EA#0212-68 Page30of122 page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\055-3802.D Sample Name: Outlet-R3-H2SO4*10 0212-68 

# _______— --________________

_____________ 

# __ Acq. Operator : EDE Seq. Line 38 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 12:15:28 PM Inj : 2 Acq, Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:54:34 AM by Eli Ellis (modified after loading) Metkiod Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H_\HPLC2012Q1\MR BURNS\DATA\PEB\FIPLC67PG006\0553802.D) 

# ~
uSlcm I 90 ;
80 - ~ 

# 70 °

60 

# 50 0

ri 

# 40

~



# a ) ~ c

0 30 

# 20

10

_...... ~ . 0 2 3 5 _. 6 

## 8



# ___________________ _ 

# ______________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL]

- - - I---------- I ---------- I ----------I ------------------ 3.021 BB 506.04080 1.52296e-2 7.70681 Fluoride 4.280 BB 103.65685 2.40048e-2 2.48827 Chloride

'Potals : 10.19508 

# _______— —______________

____________ 

# ________________________ *** End of Report ***

Eli Ellis 2/20/2012 9:54:48 AM Eli Ellis EA#0212-68 Pdge31of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\057-4001.D Sample Name: C3-R1-H2SO4*100 0212-66 

# ---_______________ _ Acq. Operator 

# ___ 

# _______________

: EDE Seq. Line 40 Acq. Instrument : Mr_Burne Location Injection Date : 2/17/2012 12:57:51 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column; Metrosep A Supp 5 Mobile Phaae: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

- ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATAIFEB\HPLC67PG006\057-4001.D) u8/cm 90 -1

60 

# ~ i 70 60 i I

50 - m
40 -

~ a ~ 30 - m

r °

U 20 -', 0

oi j 1 

# 10 , ~



# a

~ _... — 'I 0 ~~ ~r,—~ r Tn

2

_ 3 4 5 6 - 7 8 9 mi_n



# __________ ____________________________ 

# ___________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- 1--1------ ------------ 3.038 BB 142.10037 1.51420e-2 2.15168 Fluoride 4.019 BB 16.19972 2.61944e-2 4.24341e-1 Chloride

Totals : 2.57603

*** End of Report ***

Eli Ellis 2/20/2012 9:55:25 AM Eli Ellis EA#0212-68 Page32of122 page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\057-4002.D Sample Name: C3-R1-H2SO4*100 0212-68

_____________________ Acq. Operator : EDE Seq. Line 40 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 1:11:59 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellie (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Re.te: 0.70mL/min Suppressed Ion Conductivity

~ ADC1 A, ADCt CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\057-4002.D) u8/cm

~ ; 90

~ 80

I 70- ~ 1 i 60
50- a i 

### 40 30 - o

~ U ° 20 m ~ ~

~ N i 10 ..-_ :. ......_. ......_ _ —.______ ...... -, 0 2 3 r 4 5 6 7 8 9 min



# ===____________________________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I---------- I---------- I---------- 1--I------------------ 3.040 BB 141.29683 1.51413e-2 2.13942 Fluoride 4.023 BB 16.07133 2.62151e-2 4.21311e-1 Chloride

Totals : 2.56073



# ______________________________

*** End of Report ***

Eli Ellis 2/20/2012 9:55:35 AM Eli Ellis EA#0212-68 Page33of122 Page 1 of 1Data File H:\HPLC2012Q1\MR 13URNS\DATA\FEB\HPLC67PG006\060-4301.D Sample Name: C3-R2 H2SO4*100 0212-68

Acq. Operator : 

# _ ________ _____________ EDE Seq. Line 43 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 2:22:39 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\PEB\HPLC67PG006\060-4301.D) uS/cm 90
80 .
70 60 I



### a I 

### 50 d ~ 40 LL

~ 2 ~o V L I~ 30 a

o U I i 20 m o ~ 10~ \

~...... ~...._ ~ ....~L_"~.....

_ .......___.... .. . ....- ,.___- l Q T ,--r r -- 2 3 4 5 6 7 8 9 min

_-_-__-_______________-____-_ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I---------- I ---------- 1--i------------------ 3.044 BB 161.37254 1.51566e-2 2.44585 Fluoride 4.019 BB 26.17786 2.52052e-2 6.59818e-1 Chloride

Totals : 3.10567

*** End of Report ***

Eli Ellis 2/20/2012 9:56:39 AM Eli Ellis EA#0212-68 Page34of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\060-4302.D Sample Name: C3-R2 H2SO4*100 0212-68

Acq. Operator 

# ____ ________________.____ : EDE Seq. Line 43 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 2:36:47 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

' ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\060-4302.D) I, uS/cm 90 

## ~
sa 

# 70 I i
so i 

# 50 ~ 

# I

0 

# 40 LL a 30 0

M L

~ o U 20 

# !\ o 10

0

. 2

_ 3 4 5 6 7 8 9 min



# _______________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL] 

# - - - I------ I ---------- I ---------- I ---------- I--1------------------ 3.043 BB 162.18027 1.51571e-2 2.45818 Fluoride 4.017 BB 26.49560 2.51859e-2 6.67317e-1 Chloride

Totals : 3.12550



# _ _________________--- *** End of Report ***

Eli Ellis 2/20/2012 9:56:51 AM Eli Ellis EA# 0212-68 Page 35 of 122 Page 1 of 1Data File 14:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\061-4601.D Sample Name: C3-R3 H2SO4*100 0212-68



# ________________________________ Aaq. Opera-tor : EDE Seq. Line : 46 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 3:47:36 PM Inj : 1 Aoq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM-M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADCt CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\061-4601.D) u5/cm ' 

# i B0 80 l i I
I 70 60 i

d 50 0 40 LL a a
~ o 30 - M V I 1 20 - o \

~ J 10

_ .. ~ r _.... _.... .. ...... 2 3 4 5 6 7 8 9 min



# ________________________________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCS A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL1 

# ------- I ------ I ---------- I ---------- I ---------- 1--1------------------ 3.047 BB 199.65015 1.51771e-2 3.03012 Fluoride 4.014 BB 32.33255 2-48995e-2 8.05064e-1 Chloride

Totals : 

# 3.83518

-----------------------------



# __________ _____-___-____---______________

__ __ *** End of Report ***

Eli E11iS 2/20/2012 9:57:37 AM Eli Ellis EA#0212-68 Page36of122 page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\061-4602.D Sample Name: C3-R3 B2SO4*100 0212-68

Acq. Operator 

# _ _____________________________________________ : EDE Seq. Line 46 Acq. In5trument : Mr_Burns Location Injecti.on Date : 2/17/2012 4:01:44 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analyeis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\061-4602.D) uS/cm
~ I

90 

# ~ 80 I 70 I 60 ~ 50

~ 40 u o 30 r `

o t

o U c6 20 ^ i \ c ~ i ~ o I ~

....._ ., ~ '• _
, _–...... _ ... ____..—_ / 0- 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- i ---------- 1--I------------------ 3.047 BB 200.82625 1.51776e-2 3.04807 Fluoride 4.013 BB 32.58372 2.48895e-2 8.10992e-1 Chloride

Totals . 3.85906



# _________________ *** End of Report ***

Eli Ellis 2/20/2012 9:57:45 AM Eli Ellis EA#0212-68 Page37of122 Page 1 of iData File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\062-4701.D Sample Name: Blank-H2SO4*10 0212-68

Acq. Operator : EDE Seq. Line 47 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 4:15:52 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\062-4701.D) uS/cm 

### 90 

# ~ 80 

# ~ 70 60 I 50 40

30 a
20
10 i l \

.

. 0 2 3 4 5 6 7 8 9 mi


# _____________________.-----__-____________

-------------- 

### __________________ External Standard Report



### --------------------------------------------------------- ------ ------ 

### --------------------------------------------------------------------- Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I---------- I ---------- 1--i------------------ 3.074 - - - Fluoride 4.100 - - - Chloride

Totals : 0.00000


### 1 Warnings or Errors .
Warning : Calibrated compound(s) not found

Eli Ellis 2/20/2012 9:58:27 AM Eli Ellis EA#0212-68 Page38of122 Page 1 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\062-4702.D Sample Name: Blank-H2SO4*10 0212-68



## ----------------- _____-_ --- ---- 

## ________-____ Acq. Operator : EDE Seq. Line : 47 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 4:30:00 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Laet changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

-' us/cm ADC1 A, ADC 1 CHAN NEL A(H:\H PLC2012Q1 \M R BU RNS\DATA\FEB\HPLC67PG006\062-4702.D) 

## 90 ! I I 80 70 60 I I I

50 

## 40 I 

## 30 I 

# 20

~ ~ 

## v

~ ~ .._._. 101

........ .

~ r

- • -- ~ - r~r~r":~~__~ — 1 2

_ 3 _ 4 5 6 7 8 9 min 

# ______—__________

_______________ 

# ________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amou.nt Grp Name 

# [min] [u5/cm*s] [ug/mL] ------- I ------ I I ----------I---------- --1------------------ 3.074 - - - Fluoride 4.100 - - - Chloride

Totals : 0.00000

1 Warnings or Errors : Warning : Calibratedcompound(s) not found

B1i Ellis 2/20/2012 9:58:37 AM Eli Ellis EA#0212-68 Page39of122 Page 1 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\007-3301.D Sample Name: RB/0.01N-H2SO4/0.01N NaOH 

# _______—____________________________________ Acq. Operator : EDE Seq. Line 33 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 9:35:04 AM Inj : 1 ACq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity



### uS/cm ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS \DATA\FEB\HPLC67PG006\007-3301.D) 

### 0 90 ~ I °
i 80 , I II 70 I I 60 ~
50 ii 40 30 ' i I

20 ~ ~ 10 ~ \,

........ ~.-__. ........ ..._ 2 3 4 5 6 7 8 9 min



# ---------------------- External Standard Report --__----------_-_----__

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I---------- I ---------- 1--1------------------ 3.074 - - - Fluoride 4.029 - - - Chloride

Totals : 0.00000

1 Warnings or Errors : Warning : Calibrated compound(s) not found

Eli Ellis 2/20/2012 9:52:05 AM Eli Ellis EA#0212-68 Page40of122 Page 1 of 2Data File H:\HPLC2012q1\MR BURNS\DATA\FEB\HPLC67PG006\007-3302.D Sample Name: RB/0.01N-H2SO4/0.01N NaOH

Acq. Operator 

## _______— _ —



# _____________ __ ___ : EDE Seq. Line : 33 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 9:47:24 AM Inj : 2 Acq. Method : C:\HPLC2011p4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

— ADC1 A, ADC1 CHANNEL A(H:\FIPLC2012Q1\MR BURNSIDATA\FEB\HPLC67PG006\007-3302.D) 

# n F USIcm _ 90 4 

## °

80 .



## ~ I 

## ~ 701 

## ~ 

## 60 i 50 l i
40 

## ~ ~ i 

## 30 20 

# I

6 o 2 3 4 

## 5 6 7 8 9 min



# ____ ______ __________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Muitiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- 1--I------- ----------- 3.074 - - - Fluoride 4.029 - - - Chloride

Total.s : 0.00000

1 Warninge or Errors : Warning : Calibrated compound(s) not found

Eli Ellis 2/20/2012 9:52:14 AM Eli Ellis EA#0212-68 Page41of122 Page 1 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\058

- 4101.D Sample Name: MS/C3-R1-H2SO4*100 0212-68

Acq. Operator : 

# —_—_____________

__________________________ 

# _______________________ EDE Seq. Line : 41 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 1:26:07 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli E11is Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
Additional Info : Peak(s) manuallv integrated

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\058-4101.D)

— ~ uS/cm ~ 

# 90 ° I i i

~ $o ~ 70 m 0 ~ 

# I
604

- b 50 -

40 - p U g

' ) ~ 30 ~ ,~'~'
a 20 I 1 

# 10

~ __.. ~ .. .... 0 2_

. 3 4 5 6 7 8 9 min



# _______ ___ ____ 

# ______________ External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL]


# ------ I ---------- I ---------- I---------- 1--I-- --------------- Manua[Int."II"(EDEI 3.047 MM 339.93423 1.52129e-2 5.17139 Fluoride 4.025 MM 131.37939 2.39193e-2 3.14250 Chloride 

### ManualInt."II°(EDE
Totals 

# 8.31389

________________ ______ *** End of Report ***

Eli Ellis 2/21/2012 3: 35:36 PM Eli Ellis EA# 0212-68 Page 42 of 122 Page 1 of 1

### Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\058-4102.D Sample Name: MS/C3-R1-H2SO4*100 0212-68 

# __________--- Acq. Operator ------------



### : EDE Seq. Line : 41 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 1:40:14 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METH01)S\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 F1ow Rate: 0.70mL/min Suppressed Ion Conductivity

uS/cm ADC1 A, ADCt CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATAIFEB\HPLC67PG006\058-4102.D) 

# --

~

90 

# 80- 70- v

0 60 '.. JJJ 50 - 

### ~ ~

rn g I 

### 40 1 ] n

4 t

U I I 30

~ N 20 

### N N 10 ~ r

-. Tr --- , 0 - 2 3 4 5 6 7 8 9 min



# _____________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDS Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL]


# - ---I- ---------- I ---------- I------ ---- 1--i----------------

- - 3.049 BB 336.02182 1.52123e-2 5.11167 Fluoride 4.028 BB 129.53470 2.39238e-2 3.09897 Chloride

Totals : 

### K~ SfflTJ



### ______________________*** End of Report *** 

# ____---_______________

Eli Ellis 2/20/2012 9:56:00 AM Eli Ellis EA#0212-68 Page43of122 Page i of 1Data Fi1e H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\059-4201.D Sample Name: MSD/C3-Rl-H2SO4*100 0212-68



# __ __________ Acq. Operator : EDE Seq. Line : 42 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 1:54:23 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 3:03:13 PM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
Additional Tnfo : Peak(s) manuallv intearated

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC(37PG006\069-4201.D) 

### uS/cm ~ 90 ~ 80 1 ~ il , I 70 d

a 60 ~ o i IIII

3 U 50 - ro a_ I 40 U by1 30 29 -:: N 1

I ~ N N ~ 10

, a .--- ~-- — 2 3 4 5 6 7 8 9 min



# ______________________________________ External Standard Report

Sorted By

. Signal Calib, Data Modified . 2/20/2012 3:06:20 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADCl CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [u5/cm*s7 [ug/mL] 

# - I---------- I ---------- I---------- I--1-------- ---------- 3.048 BB 332.76486 1.52118e-2 5.06196 Fluoride 4.026 MM 131.46719 2.39191e-2 3.14457 Chloride 

## Manuallnt."II"(EDE

Totals : 8.20653



# __ _________

*** End of Report ***

Eli Ellis 2/20/2012 3:21:01 PM Eli Ellis EA#0212-68 Page44of122 Page 1 of 1Data Fi1e H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\059-4202.D Sample Name: MSD/C3-Rl-H2SO4*100 0212-68 

# _—__ —__________ Acq. Operator 

# —___

___ ____________ 

# __ : EDE Seq. Line Acq. Instrument : Mr_Burns Location Injeotion Date : 2/17/2012 2:08:31 PM Inj Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 3:03:13 PM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5

. Mobile PhaSe: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

n~ ti., al rnfl • nPak(c) mannallv infParate(7



# _

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEBIHPLC67PG006\059-4202.D) 

# _ .. 

# ~ uSlcm,

~ 

# 90 °

80 

# 70 a I I
60 ~ `o

~ 

# 50 w ro a i 40

s ~ i m 6
30

20 ~a

C~ 10~

0 2 3 4 5 6 7 8 9 _min 

# _______ — ___________

______________ 

# ________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 3:06:20 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A

RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------------------ ----------I - - ------ 3.048 BB 

# I ----------

332.14279 

# I ---------- I

1.52117e-2 5.05246 Fluoride 4.014 MM 131.12566 2.39199e-2 3.13651 Chloride 

### ManualInt."II°(EDE

Totals : 8.18897



# ____________ _____________________ *** End of R2pOrt *** 

# 42

2

Eli Ellis 2/20/2012 3:21:22 PM Eli Ellis EA#0212-68 Page45of122 Page 1 of 1Data Fi1e H:\HPLC2012Q1\MR BURNS\1)ATA\FEB\HPLC67PG008\HPLC67PG008\031-1101.D Sample Name: Outlet-Rl-NaOH*2000 0212-68

Acq. Operator : 

# ______________ ______ ________________

EDE Seq. Line : 11 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 8:13:49 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity ADC1 A,ADC1 CHANNELA(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\031-1101.D) uS/cm 90 ~ I 80. ~ 1 I 70 1 60 I 50 40 ° a

_ 30 ° s U I 20 .- 0 0 ~ 10 ~ v ~ 0

-,--- -T

- 7

-- -7

-- -T

- r - 7~ 2 3 4 5 6

_ 7 8 _9 min

___________ ___________________________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/Cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- 1--1- ----------------- 4.004 BB 31.42122 3.20561e-2 1.00724 Chloride

Totals : 1.00724

____ _____ --------- - -- _ *** End of Report ***

Eli E11is 2/21/2012 4:56:15 PM Eli Ellis EA#0212-68 Page460f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG008\031-1102.D Sample Name: Outlet-Rl-NaOH*2000 0212-68

°-
_ Acq. Operator : _________________ EDE Seq. Line 11 Acq. InStrument : Mr_Burns Location Injection Date : 2/20/2012 8:27:58 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, AD01 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\PEB\HPLC67PG008\HPLC67PG0082\031-1102.D) I uS/cm

-

I ~ 90 

# ~

~ 80- ~ 70 I
60
50
40 

# ~ I 30 7 r ° 20 j M

!~ T ...—.. ....._._ ....... __ ... ......- ._

~ .
2 3 4 5 6 7 8 9 mi

_ External Standard Report

Sorted By.

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL]


# - - ------ I ---------- I ----------I----------- --1------------------ 4.003 BB 31.58813 3.20469e-2 1.01230 Chloride

Totals . 1.01230

° ° ° ° ° ° ° --------------------------------------------- ~ ---- *** End of Report ***

Eli Ellis 2/21/2012 4:56:25 PM Eli Ellis EA#0212-68 Page470f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BIIRNS\DATA\FEB\HPLC67PG006\083

- 5001.1) Sample Name: Outlet-R2-NaOH*10 0212-68

---------------- 

# _______________________ Acq. Operator : EDE Seq. Line : 50 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 5:38:48 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column< Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADCt CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\0835001.D) us/cm

90 

# I 80
70 I I 60 m 50 L ~ 40 U I
N 30 -

20

1 10^

]{ O

2

. 3 4 _ 5 6 7 8 9 m in

----------- 

# __________ ___________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADCl CHANNEL A
RetTi-me Type Area Amt/Area Amount Grp Name [inin] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- --1------------------ 3.954 VB 205.64374 2.38037e-2 4.89508 Chloride

Tota1S . 4.69508

-------------

__________ ___ ____________ *** End of Report ***

Eli Ellie 2/21/2012 4: 04:10 PM Eli Ellis EA# 0212-68 Page 48 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\083-5002.D Sample Name: Outlet-R2-NaOH*10 0212-68



# _________ --_______—__



# ___ ________________ Acq. Operator : EDE Seq. Line 50 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 5:52:36 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysie Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL .M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/mim Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\083-5002.D) WS/GM 

# 90 

# ~

80 -

70 - 

# 60 50

40 L v I i I 

# 30

~



# rn i 20 m m 

# r 0 

# ~

r ry q CJ / I 0 2 3 4 5 _6 7 , 8 9 min



# _____ _ ____________-___ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilu.tion Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

### [min] [us/cm*s] [ug/mL] 

# ------- I ------ I-- -------- I- --------- I-- -------- 1--i- ----------------- 3.956 VB 191.B6115 2.38184e-2 4.56982 Chloride

Totals : 4.56982



# _________________________ _______________________ *** End of Report ***

Eli Ellis 2/21/2012 4:04:18 PM Eli Ellis EA# 0212-68 Page49 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\086-5301.D Sample Name: Outlet-R3-NaOH*10 0212-68

________________________________ Acq. Operator : EDE Seq. Line 53 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 7:01:36 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/imM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity ADC1 A,ADC1 CHANNELA(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\086-5301.D) uS/cm d
90 80 i 70

60 ?,

~ 

### 50 ~
40 ~ 

### I 30- 

### o s U 20
10

0 ..r--T"

. , . 2 3 4 5 6 7 8 9 min

------------------------- _-------- _______ ----- _____________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I---------- i ---------- I ---------- 1--i------------------ 3.957 VB 22.71484 2.54SOOe-2 5.78093e-1 Chloride

Totals . f. '>AlE:IWeS

~ I

_____________ "** End of Report ***

Eli Ellis 2/21/2012 4:05:19 PM Eli Ellis EA# 0212-68 Page 50 of 122 page 1 of 1Data File H:\HPLC2012Q1\MR 13URNS\DATA\FEB\HPLC67PG006\086-5302.D Sample Name: Outlet-R3-NaOH*10 0212-68

------------- —_ 

# ______________________________ Acq. Operator : EDE Seq. Line 53 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 7:15:24 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analyais Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BLIRNS\DATA\FEB\HPLC67PG006\086-5302.D) ~ i uS/cm 90 80 70
60. i 50 40 ~ i 30 s U I

I~ M 20

M j 10 

## - N


## ..,. ~ i~ n p i 

## l

. .. ~C~~ 

## __ ..... 

# - cd

~ 

# ....:

~~ 

# _ ......., y ...._ ....._. ,..._._.

~ 0 

## ' 2 3 4 5 

## —. 6 7 8


## _

—_ 9 min



# ________ ______ 

# ______________________________

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADCl CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL]


# - ------ I ---------- I ----------- I------- --- 1--i--------- --------- 3.963 VB 21.45212 2.55590e-2 5.48294e-1 Chloride

Totals 5.48294e-1

- - - - — - ------- - - ------- ---- -------- - ---- *** End of Report ***

Eli Ellis 2/21/2012 4:05:28 PM Eli Ellis EA#0212-68 Page510f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FE2\HPLC67PG006\087

- 5401.D Sample Name: C4-R1-NaOH*10 0212-68


# —__ —__=________- —



# ___________ _____________________ Acq. Operator : EDE Seq. Line : 54 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 7:29:12 PM Inj : 1 ACq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

"

F US/c z ADC1 A, ADC7 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\087-5401.D) 

## i 

# ~

80 -

70

~ ~
~ I

I 1

50 -
40 - 

# ~ I 30 - ° L n 20 U

10 

### " 0 

### i

~ 

### ._ r 

### J _

. ~ 

# ~

~ 

### _:.: _ r . --......— .__ ~ 

### / \..

-..._ ..._ J ._... ...... -1

---------

T-

. 2 3 4 5 6 7 8

_ 9 min



# --------------

___________ ______ 

# __________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDe Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL] ------- I ------I I ---------- 1--i-------- ---------- 3.960 BB 9.96691 2.78172e-2 2.77252e-1 Chloride

Totals . 

# 2.77252e-1
°°°'°°°°°---------------- ----- ------------------------ *** End of Report ***

Eli Ellis 2/21/2012 4:05:55 PM Eli Ellis EA#0212-68 Page52of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\087-5402.D Sample Name: C4-R1-NaOH*10 0212-68



### __ 

# ______________ Acq. Operator : EDE Seq. Line : 54 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 7:43:00 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phaee: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
(- ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q11MR BURNS\DATA\FEB\HPLC67PG006\087-5402.D)

. j uS/cm 90 - 

### 80 I 

### I I 70 60
50 j 

### I 

# ! I 

# ~ 40 i a 30 - °
20 O L N I

10 .

- N ~

~ ! ~ J

0

4 -r ~ ._,- .

-

~~ i._

~ TT-r-'

~ T_

~ T..,.._,__ 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal - Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Uee Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- i ------ I---------- I---------- I ---------- 1--I------------------ 3.967 BB 9.58215 2.79866e-2 2.68171e-1 Chloride

Totals . 2.68171e-1

--------------------------------- *** End of Report ***

Eli Ellie 2/21/2012 4:06:04 PM Eli Ellis EA#0212-68 Pdge530f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\089-6001.D Sample Name: C4-R2-NaOH*10 0212-68

Acq. Operator : 

# _____ ___________________

EDE Seq. Line 60 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 10:17:26 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

Arlr3itinnal Tnfn - Peak(s) manuallv inte c x rat ed

~ ADC1 A, AD01 CHANNEL A(H_\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\089-6001.D) uS/cm I 90 

## I I 80 70 - i 60 J i 50 i 40 a i I 30
10, w 20 a`p `~ ......_—.—_.. ..—...... __—.. , _.. _~T .T ~ .. ,..,_T ....~_ ~ ......... --_..,._. 2 3 4 5 6, 7 8 9 min



# ____________________ _________________________ External Standard Report

8orted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal l: ADC1 A, ADCl CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL]


# - ---------- I ----------I---------- --1------------------ 3.958 NIM 3.01507 2.98800e-2 9.00902e-2 Chloride 

## Manuallnt."II°(EDE

Totals : 9.00902e-2

____________________ *** End of Report ***

F.li Ellie 2/21/2012 4:07:28 PM Eli Ellis EA# 0212-68 Page 54 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\089-6002.D Sample Name: C4-R2-NaOH*10 0212-66

Acq. Operator : 

# ------------- —__________
_____________ EDE Seq. Line : 60 Acq. Instrument : Mr_Burne Location Injection Date : 2/17/2012 10:31:14 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2(CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 F'low Rate: 0.70mL/min Suppressed Ion Conductivity

TAriii-i—1 Tnfn • DPablcl mannallv ini'earatPf'l

~ ADCIA.ADCICHANNELA(H:\HPLC2012Q1\MRBURNS\DATA\FEB\HPLC67PG006\089-6002.D ) uS/cm 90 

### 80 - 70 i
60 " 50- I 40 l~

5~- V 1~ ~
30-~ L r I
20 N r ,1 ' '8h 10 ._i~ ~ .>~ .a._...~.-~. ......._.. ......... . _..a. ...._ ._ . 2_._ 3 ._. 4 5 _ 6 7 8 ._ 9 min 

# ________—___-____-_ _ _____________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDe Signal 1: ADCl A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s1 [ug/mL]

- ------ I ---------- I ---------- I ---------- --1 3.944 MM 3.35784 2.98800e-2 1.00332e-1 Chloride 

## Manuallnt."II"(EDE)

Totals : 

# 1.00332e-1

-------------

___________ 

# ____________ _____________________ *** Erid Of Report ***

Eli Ellis 2/21/2012 4:07:44 PM Eli Ellie EA#0212-68 Page55of122 Page 1 of 1Data Fiie H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\090-6101.D Sample Name: C4-R3-NaOH*10 0212-68

Acq. Operator 

## __ 

# _____ _ _____________

: EDE Seq. Line : 61 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 10:45:01 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2(CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity Additional Info : Peak(s) manuallv integrated 

# r usic:
ADC1 A,ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\090-6101.D)



## 80 ~ 

## I 70 I 60

~ 

## I
50 - 

## 40 m i I
30


### ^ N ry 9 20 :, 

### ~ 

## ' 1 .i_...

~ 

### ...._ ~ 

### ....__-. ..._. -..__ _ ... 0 2 3 4 5 6 7 8 9 mi n



# ___ _______________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

## [min] [uS/cm*s] [ug/mL]

- ------ -- ---------- ---------- ----------

~ - 3.955 MM ---- 

### ~ ~ ~ ~--~

7.B9166e-1 2.98800e-2 2.35803e-2 Chloride 

### ManualInt."II°(EDE)

Totals 2.35603e-2

-------------------------------------------------------------- *** End of Report ***

Eli Ellis 2/21/2012 4:08:01 PM Eli Ellie EA#0212-68 Pege56of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\090-6102.D Sample Name: C4-R3-NaOH*10 0212-68 

# ------ ___ ----------- _=== --------

- 

# -___________________ Acq. Operator : EDE Seq. Line : 61 Acq. Instrument : Mr_Burns Location Injeation Date : 2/17/2012 10:58:49 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analyeis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
7additional Info : Peak(s) manuallv inteqrated

ADC1 A, ADCt CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\090-6102.D) us/cm 

# 90 °

80 . 

## ~

~ I 

# 70

~ 

# I

60 i 

# i 50 i I 

# 40-

a i i 

# 30

~ 0 i 

## 0

0y tLj b

q°' ~ 

## I \ 20

~ ,h ° ' ~ ~M 

## ..._..._.._.__'.
10 n ~ ,

~~ e


## ,. 2 

## .,.,N 8 -" 0 

## ~- T- 6~~ -

3~ 

# 5 8 min
_______— _________

_________________ 

# __ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL]
— ----- I -- — — I ---------- ---------- ---------- ---------- ------ 3.959 MM 7.44894e-1 2.98800e-2 2.22574e-2 Chloride 

### ManualInt."II°(EDE)

Totals . 2.22574e-2

--------------------------**« End of Report ***

Eli Ellie 2/21/2012 4:08:11 PM Eli ElliS EA#0212-68 Page570f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\091-6201.D Sample Name: Blank-NaOH*10 0212-68



# _ ______ __________ Acq. Operator : EDE Seq. Line 62 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 11:12:38 PM Inj : 1 Aoq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : G \CHEM32\1\METHODS\HPLC67PG006-2(CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
Additional Info : Peak(s) manuallv intecrrated

ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\091-6201.D) uS/cm 

## ~ 90 `9 l i 80
70 i I 60
50
40

i 

## ~ 30

20

19 N

2 3 4 5 6 7 8 9 min



# __ 

# _____________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL]

. 

# - ~ 

# ---------- I ---------- I ---------- 1--I------- ----------- 4.029 - - - Chloride

Totals : 0.00000

1 Warnings or Errors : Warning : Calibrated compound(s) not found

Eli Ellis 2/21/2012 4:09:23 PM Eli Ellis EA# 0212-68 Page 58 Of 122 Page 1 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\091-6202.D Sample Name: Blank-NaOH*10 0212-68

----------------------------------------------------- Acq. Operator : EDE Seq. Line : 62 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 11:26:26 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analyeis Method : C:\CHEM32\1\METHODS\HPLC57PG006

- 2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 F1ow Rate: 0.70mL/min Suppressed Ion Conductivity

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\091-6202.D) uS/cm

~ , 90

80
70 

### ~ i l

~

60
50 - i i 

### i

, I i
40 ~ 30-



### ~ 20

~ i 10 N 

# ._.. .-..-- .._.. —r 0 .- .-_----- r-_ 2 r

3 4 5 6 7 8 9 min 

# ______— ---

------------------------------- 

# -------------------------- External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiulier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDa Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL7

- -~ 

# ----------I---------- i ---------- --1------------------ 4.029 - - - Chloride

Totals : 0.00000

1 Warnings or Errors : Warning : Calibrated compound(s) not found

Eli Ellis 2/21/2012 4:09:05 PM Eli Ellis EA# 0212-68 Page 590f 122 Page 1 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\007-0601.D Sample Name: RB/ 0.01N H2SO4/ 0.01N NaOH

Acq. Operator : 

# _ ______________.________

EDE Seq. Line 8 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 5:52:31 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADCi CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\007-0801,D) uS/cm ~ 90 -- 

## 4 °~ 

## ( 80 70 ~ 

## i 60 I

~~ I
50 

## 40 i

30 1
~ I ~ 

## 20

. 10~ 

### A 

## i

~~ ...... 

## .,. _*

. ...._. ........ ...... . ~~ 

## ' O

~ 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal l: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

## [minl [uS/cm*s] [u.g/mL] 

# ------- I ------ I---------- I ---------- I ---------- I--1------------------ 4.006 - - - Chloride

Totals : 0.00000


## 1 Warnings or Errors .
Warning : Cal.ibrated compound(s) not found

Eli Ellis 2/21/2012 4:55:34 PM Eli Ellis EA# 0212-68 Page60of122 Page 1 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG00B\HPLC67PG0082\007

- 0802.D Sample Name: RB/ 0.01N H2SO4/ 0.01N NaOH

Acq. Operator : 

### ---------------- 

# _________ _____________--______________-_________ EDE Seq. Line 8 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 6:06:39 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADCi CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\007-0802.D) uS/cm 901 ° 

### 80 I 70 60 I 50
40 -,
30 ~ 

### 20 i \
10 j 

### \

_..... _ .__.. ...._ - .....

~

._—

- T ---- I --- I --- I --- T --- r''—. ~ ~T 2 3 4 5 6 7 8 9 m in



### ____________ _____________

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I---------- I---------- 1--I------------------ 4.006 - - - Chloride

Totals : 0.00000

1 Warninge or Errors . Warning : Calibrated compound(s) not found

Eli Ellis 2/21/2012 4:55:45 PM Eli Ellis EA#0212-68 Page61of122 Page 1 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\084-5101.D Sample Name: MS/Outlet-R2-NaOH*10 0212-68



# __________ ______________ 

# _ _________________ 

# ___________________________ Acq. Operator : EDE Seq. Line : 51 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 6:06:24 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analyeie Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli El1iS Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

### ADC1 A, ADC1 CHANNEL A(H;\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\084-5101.D) _ — 

### uS/cm I ~ 90 , °P 80 I 70

~ v III a 60 a ~ 50 -, U
v 40 30 N rp 20 i 10 N / m

2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDe Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# - -I---------- I---------- I ---------- 1--I------------------ 3.954 VB 322.98996 2.37294e-2 7.66437 Chloride

Totals : 7.66437



# __ ____ -------- 

# ---

-



# _ *** End o£ Report ***

Eli Ellis 2/21/2012 4:04:31 PM Eli Ellis EA#0212-68 Page620f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\084-5102.D Sample Name: MS/Outlet-R2-NaOH*10 0212-68 

# ---____-___-___— _______

________ 

# ____________ Acq. Operator : EDE Seq. Line : 51 Acq. Inetrument : Mr_Burns Location Injection Date : 2/17/2012 6:20:12 PM Inj : 2 Aoq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Laet changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\084-5102.D) 

### ~ uS/cm 

### ~ 90 - 

### ~ 

### 1 ° 

### ~ ~ 80 701 60 

### a o II 50
1 L U I I 

# 40 o 

# m I



# j

30

20 N 

### \~\~

... 

### ~ .:` 

### ~ ._ 

### ~ . r M 

### ✓
~ I.I \


### ~ - Lq

\~~ 

# :_—.. ~ `\ 

### ~ - i 

# _.. ~..' N ~~~ 

# ,,, // _-

~~ 

# r:

~ 

# i

......... .. ....-I

Q 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------I----------I---------- I ---------- --1------------------ 3.960 VB 309.46771 2.37351e-2 7.34525 Chloride

Totals : 

# 7.34525

_____---- ------------------------------------------------- *** End of Report ***

EA# 0212-68 Page 63 of 122 Eli Ellis 2/21/2012 4:04:40 PM Eli Ellis Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\085-5201.D Sample Name: MSD/Outlet-R2-NaOH*10 0212-68

Acq. Operator : EDE Seq. Line : 

### 52 Acq. Instrument : Mr_Burns Location : Injection Date : 2/17/2012 6:34:00 PM Inj : 

### 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 F1ow Rate: 0.70mL/min Suppressed Ion Conductivity
A1DC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNSIDATA\FEB\HPLC67PG0 0610 8 5-52 01.D)

— ~ uS/cm ~ 90 1
80 ~ 70 m I 

### 60 0 ~ 

### 50 O 

### j ~ 40 ~ m ~ t M 

### 30 m

~

~ N ~
~ 20 M N ~ ~ 0

~ 10 N I ~ ~ O 1 0
~ \ ~

~ , ° 'J ~ ...._. \, ~ N ~ N
~ /

_
._ 0 2 3 ,_- 4 5 6

. 7

_ 8

_ 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs
Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------I----------I I 1--I------------------ 3.956 VB 325.54779 2.37284e-2 7.72473 Chloride

Totals : 7.72473

*** End of Report ***

Eli Ellis 2/21/2012 4:04:52 PM Eli Ellis EA#0212-68 Page64of122 Page 1 of 1Data File H:\HPLC2012Q1\MR 13URNS\DATA\FEB\HPLC67PG006\085-5202.D Sample Name: MSD/Outlet-R2-NaOH*10 0212-68

__________ __ __________ Acq. Operator : EDE Seq. Line 52 Acq. Instrument : Mr_Burns Location Injeotion Date : 2/17/2012 6:47:48 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Laet changed : 12/1/2011 6:52:23 PM by SJE Analysie Method : C:\CHEM32\1\METHODS\HPLC67PG006-2 (CL).M Last changed : 2/21/2012 10:11:33 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/imM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

u5/cm ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPL067PG006\085-5202.D) 

### ~

80 ' I

~ i 70 i 60 °- `o 50

~ U

40 

### ~ I ri 30

~ N N 

### 10 20

~ N ~



### N ~ ~ m ✓ \~ / 

### ` O

~ 

### ~ \~ r J \

,.~ . , ✓

~ i \_

~ .... .__.

. ~ ...._ T .... __. ~ -_.. . .. Q 

# 2

3 4 5 6 7

_ 8

_

9 m in



# ____ ______________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/21/2012 10:11:20 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [us/cm*s] [ug/mL] 

# ------- I ------ I ----------I---------- I ---------- --1------------------ 3.963 VB 305.54947 2.37369e-2 7.25279 Chloride

Totals : 7.25279

*** End of Report ***

Eli E11is 2/21/2012 4:05:02 PM Eli Ellis EA#0212-68 Page65of122 Page 1 of 1

# Calibration

Curve Chromatograms

~

EA# 0212-68 Page 66 of 122Method C:\CHEM32\1\METHODS\HPLC67PG006-2.M

____________________ Calibration Table

Calib. Data Modified

. 2/20/2012 10:05:18 AM

Rel. Reference Window : 5.000 % Abs. Reference Window : 0.100 min Rel. Non-ref. Window

. 5.000 0 Abs. Non-ref. Window

. 0.100 min Uncalibrated Peaks

. not reported Partial Calibration

. Yes, identified peaks are recalibrated Correct All Ret. Times: No, only for identified peaks
Curve Type

. Linear Origin

. Connected Weight

. Linear (Arnnt) Recalibration Settings: Average Response
. Average all calibrations Average Retention Time: Floating Average New 75%
Calibration Report Options : Printout of recalibrations within a sequence: Calibration Table after Recalibration Normal Report after Recalibration If the sequence is done with bracketi.ng: Results of first cycle (ending previous bracket) Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Lvl Amount Area Amt/Area Ref Grp Name [min] Sig [ug/mL]

- - ---- ~ -- ~ -- I

---------- I ---------- 3.050 1 1 2.000OOe-1 13.09429 

# i
---------- 1.52738e-2 Fluoride 2 1.00000 68.90009 1.45138e-2 3 5.00000 352.35578 1.41902e-2 4 10.00000 667.78113 1.49750e-2 5 15.00000 947.58615 1.58297e-2 4.100 1 1 2.000OOe-1 7.18247 2.78456e-2 Chloride

2 1.00000 38.03643 2.62906e-2 3 5.00000 209.08857 2.39133e-2 4 10.00000 425.16600 2.35202e-2 5 15.00000 633.69385 2.36707e-2

Peak Sum Table

***No Entries in table***

Eli Ellis 2/20/2012 2:57:22 PM Eli Ellis EA# 0212-68 Page 67 of 122 Page 1 of 2Method C:\CHEM32\1\METHODS\HPLC67PG006-2.M

_____ _____________________ Calibration Curves

Area



### ~ ~ /+ / l 

### 5
800 

### ~ 

## ~ 600 +/



### ~ 4

400 - 

### /

3 

### ~ ~

~ 200 2 

### ~ 0 1 0 10

Amountfug/mLl Fluoride at exp. RT: 3.050 ADCl A, ADC1 CHANNEL A Correlation: 0.99904 Residual Std. Dev.: 25.90373 Formula: y = mx + b m: 65.51429 b: 1.13430 x: Amount y: Area Calibration Level Weights: Level 1 : 1
l"J1 I I Level 2 : 0.2 Level 3 : 0.04 Level 4 : 0.02 Level 5 : 0.013333

F Area . 600 '' /5
500

z 400 - /4 i 300-1 3 200 i

i 100 2 

### /~

~
0 0 10


### ~ _A mountfug/m LL Chloride at exp. RT: 4.100 ADC1 A, ADC1 CHANNEL A Correlation: 0.99991 Residual Std. Dev.: 2.45431 Formula: y = mx + b
m: 42.37418 b: -1.78139 x: Amount y: Area Calibration Level Weights: Level 1 : 1 Level 2 : 0.2 Level 3 : 0.04 Level 4 : 0.02 Level 5 : 0.013333

Eli Ellis 2/20/2012 2:57:22 PM Eli Ellis EA#0212-68 Page68of122 Page 2 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\001

- 2701.D Sample Name: hp1c67p9006 41

Acq. Operator 

### °°°°°°°°°°°°_____________°°°°°°°°------ -------------

: EDE Seq. Line 27 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 7:07:07 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

Additional Info : Peak(s) manually integrated

FuS/cm ADCIA,ADC1CHANNELA(H:\HPLC2012Q1\MRBURNS\DAIA\FEB\HPLC67PG006\00 1-27 0 1 .D ) 

### ~

~ ~ 

### 90 ° 80 I 70

_ 

### 60 50 

# 1 40 1 301 0

LL

~

h e o U { 1 

### 20 ry



### ~ ^
ea o e

a. 10

07

-- 

### ~ - T 2 3 ~ T ~"~~_ 4 5 6 7 ." S -" 9 mi

External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

## ------- I --

---- I ---------- I - I -- -- 1 ----------------- ManualInt."II"(EDE) 3.038 MM 12.61576 1.40477e-2 1.77223e-1 Fluoride 4.047 MM 7.02247 2.95857e-2 2.07765e-1 Chloride Manuallnt.'YI"(EDE

Totals : 

### 3.84988e-1

°------------------------------------ *** End of Report ***

Eli Ellis 2/20/2012 9:49:47 AM Eli Ellis EA#0212-68 Page69of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\001-2702.D Sample Name: hp1c67p9006 #1

----- _____ ---- ________ ----------- __ ------- ______---- ____
-------------
_____________ __ _______________________ Acq. Operator : EDE Seq. Line : 27 Acq. Inetrument : Mr_Burne Location Injection Date : 2/17/2012 7:19:27 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

Ad di.tional Tnfo : Peak(s) manuallv intearated

ADC1 A,ADC1 CHANNELA(H,\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\001-2702.D) 

## ~ F uS/cm 90 -~ i 80 70 - I 60 _ 50 I

40 a a 30
~ra 20 ' ry ' U O~

t 9
OL — o -~ I__ 2 3 4 5 6 7 8 9 min

__ ___________________._____ External Standard Report

Sorted By

. Signal Calib, Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amou.nt Grp Name [min] [uS/cm*s1 [ug/mL]


# - - - - ---------- I ---------- I ---------- --1---------- 3.039 MM 12.66428 1.40477e-2 1.77905e-1 Fluoride 

### ManuulInT."II"(EDE 4.050 MM 7.02665 2.95822e-2 2.07B63e-1 Chloride 

### Manual Int. "II" (EDE Totals : 3.85768e-1

-------------------------------------------------------------- *** End of Re p ort ***

&li Ellis 2/20/2012 9:49:59 AM Eli Ellis EA# 0212-68 Page 70 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\101-6501.D Sample Name: hp1c67p9006 #1

------------------------------- Acq. Operator ____ ------ _______---- ______

____ _____________ : EDE Seq. Line Acq. Instrument : Mr_Burns Location Injection Date : 2/18/2012 12:37:16 AM Inj Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellie (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity Additional Info : Peak(s) manuallV integrated

- ADC1 A, ADC1 OHANNEL A(H:IHPLC2012Q1\MR BURNSIDATA\FEB\HPLC67PG006\101-6501.D) u5/cm N 90 80 I I
70 I I

60 - ~ l I 50 ' i 40 o a 30 ~ o

20 1 ~ ~ g. ~ ,1, I ( 1 10
0

~ 2

. _ 3

. 4_ 5 6 7 8 9 , min



# __________ ___________________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [u5/cm*s] [ug/mL]



# ---------- I ---------- I--------- - 1--i------------------ 3.045 MM 13.50830 1.40477e-2 1.89761e-1 Fluoride 4.029 MM 7.25683 2.93924e-2 2.13296e-1 Chloride
Totals : 4.03057e-1

*** End of Report *** 

### Manual Int."II" (EDE Manual Int. "II" (EDE 65
1

Eli Ellis 2/20/2012 10:09:45 AM Eli E11isEA#0212-68 Page710f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\101-6502.D Sample Name: hp1c67pg006 #1

Acq. Operator : _°°°°==== ----- -------------------------------------q------ EDE Se Line Acq. Instrument : Mr_Burne Location Injection Date : 2/18/2012 12:51:24 AM Inj Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0..70mL/min Suppressed Ion Conductivity

nrM;r;nnal T.,fn - p eak(S) manuallv in tearate d

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNSIDATA\FE8\HPLC67PG006\101-6502.D)

— 

# ~ uS/cm μ 90 - 

# ~ °
80 - 70 -_ 

# I I

~. ~ 60
50
40 a a I 30 ~

G 20

>._ 0 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib, Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 . Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A

RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL]



### ------ -- -- ~ 

### --- ---------- ~ 

### - - ~ 

### --- ManualInt."II"(EDE 3.044 MM 13.58881 1.40477e-2 1.90892e-1 Fluoride 4.028 NID7 7.42393 2.92620e-2 2.17239e-1 Chloride 

### ManualInt."II"(EDE
Totals . 4.08131e-1 

# _______ —_______

________ *** End of Report *** 65

2

Eli Ellie 2/20/2012 10:09:55 AM Eli El1ieEA# 0212-68 Page 72 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\002-2801.D Sample Name: hp1c67pg006 42

Acq. Operator ------ ------------------------------------------- -------- -------

: EDE Seq. Line 28 Acq. Instrument : Mr_BurnS Location Injection Date : 2/17/2012 7:31:46 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last ahanged : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A eupp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

External Standard Report

Sorted By , Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000

. Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

## ------- I ------ I ---------- I-

------- - - I---------- 1--1------------------ 3.038 BB 68.53515 1.50112e-2 1.02880 Fluoride 4.046 BB 38.31137 2.46966e-2 9.46160e-1 Chloride

Totals : 1.97496

*** End of Report ***

Eli Ellis 2/20/2012 9:50:08 AM Eli Ellie EA#0212-68 Page730f122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\002-2802.D Sample Name: hp1c67pg006 #2

------------- -- Acq. Operator ---------------------------------------------------------- — -------- ---------------------------------------- : EDE Seq. Line : 28 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 7:44:06 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last ohanged : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q7\MR BURNS\DATA\FEB\HPLC67PG006\002-2802.D) ' us/cm ' d 

## I 80 

### I l 70 f 1 ~ I 60 50 I i 40 ~ a

~ 30 o

V ~ 20

~ - 6 0 10

. / ~ ° ~ q

.—, ....... ._. : a 0. I —T

~ - , - r
— '~~'

-

~ T-

- -T-7

- ~ T - . -,— ; 2

.. 3

. 4 5 6 7 8 9 min

External Standard Report

------- ___ ------- _____ ---- ______ ------------

___ _______________________ Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDS Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- I--1-------

- ---------- 3.040 BB 68.73705 1.50120e-2 1.03188 Fluoride 4.049 BB 37.80478 2.47113e-2 9.34205e-1 Chloride

Totals u 1.96608



# _ _______ _ ------- 

# ______ ----



# __ _____ ------------ 

# _________ *** End of Report ***

Eli Ellis 2/20/2012 9:50:17 AM Eli Ellis EA#0212-68 Page74of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\102-6601.D Sample Name: hp1c67pg006 #2

- - ------ —------ ---- - - - - - - — — ---------------------

---- -----

---- ------------ ------------- ------------------- --- Acq. Operator : EDE Seq. Line : 66 Acq. Instrument : Mr_Burns Location Injeotion Date : 2/18/2012 1:05:31 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\102-6601.D) us/cm ~s 

# ~

90 -
80 j °} I

~ 70

60 

# l i

50
40 - ~

a m
30 

# 20 , L



# 0 O h M M N N O .~
2

.. 3

. 4 ._ 5 ,. 6 7 8 , 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I---------- _-1 ------------------ 3.045 BB 69.20535 1.50137e-2 1.03903 Fluoride 4.027 BB 38.03796 2.47045e-2 9.39708e-1 Chloride

Totals . 1.97873 

# ____--- —__------ ---- ---- - - ----------- - ------- - - -- - - -- -- - - --- *** End of Report ***

Eli Ellis 2/20/2012 10:10:09 AM Eli E1lisEA#0212-68 Page75of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\102-6602.D Sample Name: hp1c67pg006 #2

Acq. Operator -----------------------------------------------------------------

: EDE Seq. Line : 66 Acq. Instru.ment : Mr_Burns Location Injection Date : 2/18/2012 1:19:40 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by E1i Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\102-6602.D) uS/cm 

# ~

90 °l
80 i I 70 a

4 60
50
40 o I



### O

~ o 30 

### 20 0 ) 1 O ~ M 10

... .-. ~ ...\- ~ _J... ~ T ._- ........\

.. 0 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal l: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s1 [ug/mL] 

# ------- I ------ I---

---- --- I ---------- I----- ----- 1--i----------------- - 3.045 BB 69.12280 1.50134e-2 1.03777 Fluoride 4.028 BB 37.99160 2.47058e-2 9.38614e-1 Chloride

Totals : 1.97638

*** End of Report ***

Eli Ellis 2/20/2012 10:10:19 AM Eli S11isEA#0212-68 Page76of122 page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\003-2901.D Sample Name: hp1c67pg006 #3

Acq. Operator 

# _________ ________________________ : EDE Seq. Line 29 Acq. Inetrument : Mr_Burns Location Injection Date : 2/17/2012 7:56:26 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analyeis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellie Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADCt A, ADC1 CHANNEL A(H:\HPLC201201\MR BURNS\DATA\FEB\HPLC67PG006\003-2901.D) uSlcm
901 

# ~ 80 70

~ 

### I i

a 60 - 0



### ° I LL 50

~

O L 40 oi U i
30 ~ 

# ° o v l i 20
10 ~ ti \

r ~ r 0 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- 1--I-- ---------------- 3.047 BB 352.89804 1.52148e-2 5.36927 Fluoride 4.045 BB 208.83170 2.38006e-2 4.97032 Chloride

Totals : 10.33958

*** End of Report ***

Eli Ellis 2/20/2012 9:50:27 AM Eli Ellis EA#0212-68 Page77of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\003-2902.D Sample Name: hp1c67pg006 #3

---- --- ----- ----- -

— ----- —

--- -

-------------------- -- -------- ---- - - - -- ------------------------------- --- - Acq. Operator : EDE Seq. Line : 29 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 8:06:46 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Laet changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
I~ ADC1A,ADCICHANNELA(H1HPLC2012Q1\MRBURNS\DATA\FEB\HPLC67PG006\003-2902.D) 

### uS/cm ~ I ~ 

### 90 ~ 80 ~ 70 - ~ I

o I 60 °

~ 50 d L I

M j 30 ~~ o 40 ~ o U N ~ i

v I I I n pJ 20 10 ~/— ~. —~/__ .~—.— .~~+ — I ~._ ✓ _ ~ .~.~ . .__ .__. ... 0.—
2 3 4 5 6 7 8 9 min



# _____ _________________________________ External Standard Report

Sorted By

. signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] (uS/cm*s] [ug/mL] 

# ------- I ------ I---------- I ---------- I---- ------ 1--I------------------ 3.047 BB 352.52576 1.52147e-2 5.36358 Fluoride 4.046 BB 208.81038 2.38006e-2 4.96981 Chloride

Totals . 

### 10.33340

_____ —___________ -- __________________ __________ _____________________ *** End of Report ***

Eli Ellie 2/20/2012 9:50:37 AM Eli Ellis EA#0212-68 Page78of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\103-6701.D Sample Name: hp1c67pg00643

°°°°°°°°°°°°°°°__ ----- Acq. Operator : EDE Seq. Line : 67 Acq. Instrument : Mr_Burns Location Injection Date : 2/18/2012 1:33:48 AM Inj : 1 Aaq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity



### uS/cm ADC1 A, ADCt CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\103-(3701.D)



### ~ ~

; 80 II 70 ~

a 60 ~

u, m 50 ro o ~

h r o O ~ 40 oi f 30' ~~ o 20 N h 10

0 6 I ..2_

. _7 8 . 9 min



# _______ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDe Signal 1: ADC1 A, ADCl CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I -- I ---------- I ---------- --1------------------ 3.058 BB 352.24374 1.52147e-2 5.35928 Fluoride 4.029 BB 209.28003 2.38002e-2 4.98090 Chloride

Totals : 10.34018

*** End of Report ***

Eli Ellis 2/20/2012 10:11:49 AM Eli E11isEA# 0212-68 Page 79 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\103-6702.D Sample Name: hp1C67p9006#3

Acq. Operator -------------------------------------------------------------------

: EDE Seq. Line 67 Acq. Instrument : Mr_Burns Location Injection Date : 2/18/2012 1:47:55 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Laet changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity ADC1 A, ADCi CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\103-6702.D)

— ~ u ~ 

### 90 ~

I 80 - 70 g 60 Eq ~ 50 -~ o 40 30 ~ ~o
201 ~ I !~

~ i \ 10, N ^

_ I

... ,~ . _..7_.. ~ .._..__~ .. _~ ~...._~. ... _U~r ....__ 6 ~

, 2 3 4 5 6_ 7 _ 8 ._ 9 _ min

________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ----------I---------- I--i ------------------ 3.054 BB 351.75558 1.52146e-2 5.35183 Fluoride 4.027 BB 209.43217 2.38000e-2 4.98449 Chloride

Totals : 10.33632

---_____-------------------------------------------- *** End of Report ***

Eli E11is 2/20/2012 10:12:50 AM Eli E11isEA# 0212-68 Page 80 of 122 Page 1 of 1Dflta File H:\HPLC2012Q1\MR 13URNS\DATA\FEB\HPLC67PG006\004

- 3001.D Sample Name: hp1c67pg006 #4 

# ------- __-------- ______ --------- ________ Acq. Operator : EDE Seq. Line 30 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 8:21:05 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2.M Last changed : 2/20/2012 9:44:27 AM by Eli E11iS Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

' ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\0043001.D)

90 I ° P

~ 

# 80

~ 

# 70 r
~ 

# 0 o I

~ 

# ri
60 U 

# 50 i l i a

i 0
40
30
20

10 r

0~

..... ~~ T

. r 

### 4

~ T-

~ T 6 7 

### 8 m in

External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADCl CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# - I ----------I---------- I -- - --1-- 3.057 BB 666.59576 1.52379e-2 10.15750 Fluoride 4.044 BB 423.08209 2.36986e-2 10.02647 Chloride

Totals : 20.18397



# ________ *** End of Report ***

Eli Ellis 2/20/2012 9:50:47 AM Eli Ellis EA#0212-68 Page81of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\004-3002.1) Sample Name: hplc67pg006 #4

Acq. Operator ---------------------------------------------------------------------

: EDE Seq. Line 30 Acq. Instrument : Mr_BUrns Location Injection Date : 2/17/2012 8:33:25 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADCi CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\004-3002.D) uS/cm ~ I ~



## a 90 

## i °

80 ~ ~ 70 a ~

O 

## a

O ) 60 M

i t

U I

~ 50
~ ~ I 40 =
30
F 20 

## M M O I

10-
0 2 3 4 5 6 7 8

_ 9 m in

External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL7 

# ------- I ------I----------I---------- I ---------- --1------------------ 3.058 BB 667.18414 1.52379e-2 10.16648 Fluoride 4.047 BB 423.12930 2.36986e-2 10.02759 Chloride

Totals : 20.19407



# ________ _____________________ *** End of Report ***

Eli Ellis 2/20/2012 9:50:56 AM Eli Ellis EA#0212-68 Page82of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\104-6801.D Sample Name: hp1c67pg006 #4 

## °°°°°°=== ----- ___________------- Acq. Operator : 

## °====== -

--------- 

## --------------------- EDE Seq. Line : 68 Acq. Instrument : Mr_Burns Location Injection Date : 2/18/2012 2:02:04 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
[- ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PGOOB1104-6801.D) 

## ~ uSlem 

## a ~ 

## 90 0

~ 

## ~ 

## LL 80

~ 

## 9 i s 70 -



### ~ I 60 ~ v

~ 56 I ON

li 

# a

~ il 40 - j 30 I

20 i I i 6 

### 10

\ 4 !O-_,a

~ n\,_

... J

~.~ _..._

~ ~ T ..—... ~. , i

...~ ~ ~ 1 . ....

~~ —T ---- F --- T ~r T~ 0 2 3 4 5 6 7

. 8 9 _._ min



# ______________ External 8tandard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- --1------------------ 3.065 BB 669.30054 1.52380e-2 10.19879 Fluoride 4.027 BB 426.91238 2.36978e-2 10.11686 Chloride

Totals : 

## 20.31565
°°°°°°°°_°°°°°°°_______-_--------------------------- *** End of Report ***

Eli Ellis 2/20/2012 10:13:23 AM Eli E11isEA# 0212-68 Page 83 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\104-6802.D Sample Name: hp1c67p9006 #4

°°°°°°°°°°°----------------------------------------------- -------- Acq. Operator : EDE Seq. Line : 6B Acq. Instrument : Mr_Burns Location Injection Date : 2/16/2012 2:16:11 AM Tnj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli E11is (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

# ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\104-(3802.D) ~
uS/cm ~ "~

a 90- o °j

~ LL I

~ L I 70 O C

~ O 60 n li 50 i o v 40 30 1 I 1~

I ~ N 20 N

~ I ,n rn i 10 0 _--------T_..T~T"-.-

_ 2 3 ._._ 4 5

_ 6 _ 7 _8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/ASea Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------ I ---------- I ---------- I- --------- I--1-----

- ------------ 3.064 BB 668.04407 1.52379e-2 10.17961 Fluoride 4.027 BB 427.54022 2.36976e-2 10.13168 Chloride

Totals : 20.31129

_______ *** End of Report ***

Eli Bllis 2/20/2012 10:13:33 AM Eli El1isEA#0212-68 Page84of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\005-3101.D Sample Name: hp1c67pg006 45

-------------------------- Acq. Operator : -------------------------------------------------------- - -------- -- ------- -------- ----- --- ------ EDE Seq. Line : 31 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 8:45:45 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analyeie Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli ElliS Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

- --------------------------------------------------------------- External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

## ------- I ------ I---------- I ---------- I ---------- 1--i------------------ 3.066 BB 946.38153 1.52456e-2 14.42811 Fluoride 4.049 BB 630.94940 2.36659e-2 14.93199 Chloride

Totals : 29.36010

__________ 

### __________________ _ *** End of Report ***

Eli Ellis 2/20/2012 9:51:06 AM Eli Ellis EA#0212-68 Page85of122 Page 1 of iData File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\005-3102.D Sample Name: hp1c67pg006 #5


# ------------ ____________------

- Acq. Operator 

# __ ________ 

# _ : EDE Seq. Line : 31 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 8:58:05 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Laet changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

~ ADC1 A, ADC1 "CHANNELA (H:\HPLC2012Q1\MR BURNSIDATA\FEB\HPLC67PG006\005-3102.D) ~

~ uS/cm 

# 90 `o 80. t

70 

# I 60

~ 

# 60

40 

# l 30

20 M

10
~ ~ .... ... _. ..."__-_ I 0 2_ 3 4 5 6 7

_ 8

_ 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Uee Multiplier & Dilution Factor with ISTDs
Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL] ------- I ------ I --- I ---------- I ---------- -- 3.067 BB 947.18060 1.52456e-2 14.44030 Fluoride 4.051 BB 631.19910 2.36659e-2 14.93788 Chloride

Totals : 29.37819

_______ 

# ___ *** End of Report ***

Eli Ellis 2/20/2012 9:51:16 AM Eli Ellis FA# 0212-68 Page 86 of 122 page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\105-6901.D Sample Name: hp1c67pg006 #5

Aaq. Opere.tor ---------- - -------

------------------------------------------------------- : EDE Seq. Line : 69 Acq. Instrument : Mr_Burns Location Injection Date : 2/18/2012 2:30:19 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Laet Changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5

. Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity



### us/cm 

# . ~ ADC1 A. ADC1 CHANNFL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\105-6901.D) ~

'7. 90 ~ ~ o ° 80 70 ~1~ o 60 v

50 I ~

~ ~

-~_ I ~ 40 ~ 1

7 20 ~ 30 o N ~ N ~
10 I I \

.._.. _ i~

........ l. .~,..... T- _..... ~/ \ •~ ✓ \~._..i ~1 ~~. i..L/_

.... m 0 - 7—^—~—~~r"-,-TT'~"-~--~ 2 3

_ 4 5 6 - 7 8

_ 9

_ min

External Standard Report

Sorted By

. Signal

. Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s7 [ug/mL] 

# ------- I ------ I---------- I-------

- -- I ---------- 1--I------------------ 3.074 BB 948.24554 1.52456e-2 14.45656 Fluoride 4.028 BB 636.29553 2.36653e-2 15.05816 Chloride

Totals : 29.51471

*** End of Report ***

Eli Ellis 2/20/2012 10:13:45 AM Eli E11isEA#0212-68 Page87of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\105

- 6902.D Sample Name: hp1c67pg006 #5 

### °°°°°°°°=°°°°°°_°°-------°°°°°°°' Acq. Operator 

### ---------------------- ----- : EDE Seq. Line : 69 Acq" Instrument : Mr_Burns Location Injection Date : 2/18/2012 2:44:27 AM Inj : 2 ACq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006

- 2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADCt CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\105-6902.D) 

## ~ S/cm 

# ~ F , °' ~ go- 3



## U ` r I 80 - U v 

### 70 N

R r



### o II I 

## ~ I I 

## ~ p 60 

## ~
50
40' i 

### 30

29 r 

## ~ A \ r 

## ~ i 

## f

_ ~~ - 10 

# mi -m 3 4 5 6 7 8 9 n
°°°°°°°°°_____________ ------- -----------------

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs
Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# - - I------ I ----------I---------- I ---------- --1- 3.075 BB 948.53693 1.52456e-2 14.46101 Fluoride 4.027 BB 636.33136 2.36653e-2 15.05900 Chloride

Totals : 29.52001



### ______ ----------------- 

### __________________________ *** End of Report ***

Eli Ellie 2/20/2012 10:13:54 AM Eli E11ieEA# 0212-68 Page 88 oP 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\006-3201.D Sample Name: hp1c67pg006 #SS

ACq. Operator °°°°°°°°°°°°°°°°°°°°°------------- --------------------------

: EDE Seq. Line : 32 Acq. Instru.ment : Mr_Burns Location Injection Date : 2/17/2012 9:10:25 AM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analyeie Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

## ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\006-3201.D)

- ~ 

## uS/cm
90 

### ~

80 

## I I I 

## 70 7 I

60
50 i

40 m

a °- 0 0

~ r 30 

## m ~ 

## 20 ~ 10

2


## _ 3 4 6 - - - - ---- - - T - ~~ 6 7 8 

## 9_, min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

### [min] [u8/cm*s7 [ug/mL7 

# ------- I ------ I ----------I I -I ------ 3.041 BB 67.73171 1.50082e-2 1.01653 Fluoride 4.053 BB 80.28986 2.41229e-2 1.93682 Chloride

Totals : 2.95336



## ____ _ __ _ ____ ___-- --- ----- ------- - - - ----- - ---- *** End of Report ***

Eli Ellis 2/20/2012 9:51:36 AM Eli Ellis EA#0212-68 Page89of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\006-3202.D Sample Name: hp1c67pg006 #SS

Acq. Operator : EDE Seq. Line 32 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 9:22:44 AM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Laet changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last ahanged : 2/20/2012 9:44:27 AM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q11MR BURNS\DATA\FEB\HPLC67PG006\006-3202.D) ~

~ uS/cm 90 

### I I I
70
6 8, 1 0 - !
50 -

~ 40 m °



### 0 0

o s 30 ~ U I 20 

### o ~

tn

~ m o I : \ 10

— m m ✓ ~ ~.L ~~ 

### .__ ~~~ 

### r._ M n

6


### - ~ ~ 

### - , _ - ~ 

### - - ~ 

### ._ _ _ - 0 .- Tr
- '

-- -r_ ..,- ~ r

. '

-- '~r

- '~^ -. i 2_ 3 4 5

_ 6 7 8 9 _ min

External 8tandard Report

Sorted By

. Signal Ca1ib. Data Modified . Monday, February 20, 2012 9:44:21 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [u9/Cm*s] [ug/mL] 

# ------- I ------I---------- I ----------I---------- --1------------------ 3.040 BB 67.71084 1.50081e-2 1.01621 Fluoride 4.053 BB 80.24788 2.41232e-2 1.93583 Chloride

Totals : 2.95205

*** End of Report ***

Eli E'11is 2/20/2012 9:51:47 AM Eli Ellis EA# 0212-68 Page 90 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\14PLC67PG006\106-5801.D Sample Name: hp1c67pg006 #SS

--------------------------------------------------------------------- Acq. Operator : EDE Seq. Line 58 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 9:21:26 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\106-5801.D) uS/cm 901 ~ I ° 

### I 80 j I 70 ~ 60 ~

~ 50
40 ~

9 m

o i i
30 - `o pu

### i 

# L
v
20

.._- N 

# ~ 10-

.. ~ ..-_ . _.— - 

# ~

.2

. 3

. 4 5

_ 6

_ 7 , 8 9 min



### _____==== _____________________________ External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ----------I----------I---------- --1------------------ 3.045 BB 68.15692 1.50098e-2 1.02302 Fluoride 4.023 BB 80.73736 2.41200e-2 1.94738 Chloride

Totals : 2.97041



# _____________ ________________________ *** End of Report ***

E.li Ellis 2/20/2012 10:14:08 AM Eli B11isEA#0212-68 Page91of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\106-5802.D Sample Name: hp1c67pg006 #SS



### --- ---------------------------------------------------------- -- Acq. Operator : EDE Seq. Line 58 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 9:35:34 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADCt A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\106-5802.D) uS/cm I 4 

### 90 

## ~

~ 

### 80

70 

## ~
60 - 

### 50 40 g 

### m i
I ~ 

### I `o 

### 30 ~

7 U 

### ~ 

### 20 0 o m N
r 

## 10 N N r



## _ ~/_~~... r

. ✓ 

## ~ ,. 

## ~

....... i_

. ,—,. —.....,. m , . _ ._ _ 0 2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADCl CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [u5/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- 1--I------------------ 3.045 BB 68.29653 1.50103e-2 1.02515 Fluoride 4.024 BB 80.74358 2.41199e-2 1.94753 Chloride

Totals . 2.97268

----------- - - - - - - - - - --- -- ----- - -- ---------------- -- - — -- - *** End of Report ***

Eli Ellis 2/20/2012 10:14:19 AM Eli E11isEA#0212-68 Page92of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\037-4401.D Sample Name: hp1c67pg006 #3 

# ------------

____________________________ _________________ 

# _________ Acq. Operator : EDE Seq. Line : 44 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 2:50:55 PM Inj : 1 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

# ADC1 A, ADC1 CHANNEL A(H:\HP1C2012Q1\MR BURNSIDATAIFEB\HPLC67PGOOG\037-4401.D) ~
~ uS/cm 901
I 80 

# ~ 70 ~ a

60 ~ 

# i

a LL ~ II I 50- ~ o

d L o U 401 ai i I 30 v 20 ~L~ I ! \~

~ ~ ~ 0 ~ ~ 10
I 2 3 4 5 6 ,. 7 ,. 8 -_ 9 ,min

External Standard Report

Sorted By Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL] ------- I ------ I ---------- I ---------- I ---------- 1--i--

- --------------- 3.049 BB 352.30151 1.52147e-2 5.36016 Fluoride 4.005 BB 209.57336 2.37999e-2 4.98782 Chloride

Totals : 10.34798

*** End of Report ***

Eli Ellis 2/20/2012 9:57:07 AM Eli Ellis EA#0212-68 Page93of122 page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\037-4402.D Sample Name: hp1c67pg006 43

Acq. Operator _______________ ___________ : EDE Seq. Line 44 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 3:05:02 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 9:55:01 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\037-4402.D)

— ~ uS/cm ~ 90 ° ~

70 ~ 80

g i 60 LL N a 50 0

' o
40
30
20 ~ v

~ I ~ \ ~ ~ ~ 10 _-_

1 2 3

. 4 5 6 7 8 9 min

___________________________________________________ External Standard Report

Sorted By

. . Signal Calib. Data Modified . 2/20/2012 9:53:31 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------I---------- I ---------- I ---------- --1------------------ 3.050 BB 351.99515 1.52147e-2 5.35549 Fluoride 4.005 BB 209.48251 2.38000e-2 4.98568 Chloride

Totale : 10.34116



# _____ _____________________ *** End of Report ***

&li E11is 2/20/2012 9:57:17 AM Eli Ellis EA#0212-68 Page94of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\1)ATA\FEB\HPLC67PG006\104-5701.D Sample Name: hp1c67pg006 #4

- - - - - - - — - - - - - - - - - - - - - - - - — - - - - — - - - - - -- - - - - - - - - - - - - - - — - - - - - - — - - - - Acq. Operator : EDE Seq. Line : 57 Acq. Instrument : Mr_Burns Location Injection Date : 2/17/2012 6:53:10 PM Inj : 1 Aaq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method ; C:\CHEM32\1\METHODS\HPLC67PG006-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

C ADC1 A, ADCi CHANNELA (H:AHPLC2012Q1AMR BURNSVDATAAFEBAHPLC67PG006A1045701.D) ~ uS/cm 0 90 

# ~ ~ i
BO = LL
~ 70 M t 

### v I 60 

# v i 40 i i ? 30 I I 

## ~ I 

# N n I

i 20 lD n I I 

# I 0 ...

~ T 

## min 6 9

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CAANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------I----------I----------I---------- --1------------------ 3.064 BB 668.90594 1.52380e-2 10.19276 Fluoride 4.021 BB 426.33371 2.36979e-2 10.10321 Chloride

Totals : 20.29597

*** End of Report ***

E1i Ellie 2/20/2012 10:13:03 AM Eli E11isEA#0212-68 Pege95of122 Pe.ge 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\104-5702,D Sample Name: hp1c67pg0o6 #4



# --- --- ------ ---- ---- ----- --------------------- -- ------- --- ---- ------- --------------------------------------------------------------------- Acq. Operator : EDE Seq. Line : 57 Acq. Inetrument : Mr_Burns Location Injection Date : 2/17/2012 9:07:19 PM Inj : 2 Acq. Method : C:\HPLC2011Q4\MR BURNS\METHODS\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PGOO6-2.M Last changed : 2/20/2012 10:04:43 AM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min 9uppressed Ion Conductivity

' ADC1 A, ADCt CHANNELA(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG006\104-5702.D) -- u5lcm 

## ~ ~ 

# 90 a ~ 

# = I 

## u 

# 80 , I v d

, 70

601 50 0 ~



### l V ~ 40 1 I 

## ~ [
30 

## ~

~ l 20 ~ N h (O 

### N

~ ~ I

i 10

~ 0 '

- ~T~ —,-- ~~ --- ~~ —, ~T~L

— ~^T

- T~T -- ~~ — ~ - 1 2_ 3 4 , 5 6 7 8

__ . 9 min



### = ==== ______________________________

External Standard Report

Sorted By

. Signal Calib. Data Modified . 2/20/2012 10:05:18 AM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTiine Type Area Amt/Area Amount Grp Name 

### [min]


# - - ------ [uS/cm*s] [ug/mL]


# ------------------ 3.064 BB 

# I ----------I----------

668.55640 1.52379e-2 

# I ---------- 10.18743 Fluoride 4.022 BB 425.94293 2.36980e-2 10.09399 Chloride

Totals : 20.28141

*** End of Report ***

Eli Ellis 2/20/2012 10:13:11 AM Eli El1isEA#0212-68 Page96of122 Page 1 of 1Method C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M



## _________________— —=--_____-



# ____________ ___________________________ Calibration Table

Calib. Data Modified .

Rel. Reference Window : Abs. Reference Window : Rel. Non-ref. Window . Abs. Non-ref. Window . Uncalibrated Peaks

. Partial Calibration

. Correct All Ret. Times:
Curve Type Origin Weight Recalibration Settings: Average Response
. Average Retention Time: 

## 2/21/2012 5:07:06 PM

5.000 % 0.100 min 5.000 a 0.100 min not reported Yes, identified peaks are recalibrated No, only for identified peaks

Linear 

## Connected Linear (Amnt)

Average all calibrations Floating Average New 75%
Calibration Report Options : Printout of recalibrations within a sequence: Calibration Table after Recalibration Normal Report after Recalibration If the sequence is done with bracketing: Results of first cycle (ending previous bracket)
Signal 1: ADC1 A, ADCl CHANNEL A
RetTime Lvl Amount [min] Sig [ug/mL]



## ------- -- I

-- I --- 4.150 1 1 2.000OOe-1

2 1.00000 3 5.00000 4 10.00000 5 15.00000 Area Amt/Area Ref Grp Name



# --------- I --- -------- 5.1B789 3.85513e-2 Chloride 29.09858 3.43659e-2 162.72301 3.07271e-2 328.98008 3.03970e-2 494.33885 3.03436e-2

_ 

# ________ ________________ Peak Sum Table

***No Entries in table***

--------- - Calibration Curves



### Area 

# ~ /5 / 

### 400- i 

# ~

A~ 300 Z 4



### i 200= 3 i

~

~ 1001

0 2 ~ 

### 1 ,r /
0 10

Amou n t(ug/mLl Chloride at exp. RT: 4.150 ADC1 A, ADC1 CHANNEL A 

### Correlation: 0.99991 Residual Std. Dev.: 1.52772 Formula: y = mx + b 

### m: 32.99302 b:-1.81077 x: Amount y: Area Calibration Level Weights: Level 1 : 1 Level 2 : 0.2 Level 3 : 0.04 i Level 4 : 0.02
Eli E11is 2/21/2012 5:09:07 PM Eli Ellis EA#0212-68 Page97of122 Page 1 of 2Method C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M

Level 5 : 0.013333

EA# 0212-68 Page 98 of 122 Eli Ellis 2/21/2012 5:09:07 PM Eli Ellis Page 2 of 2Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\001-0201.D Sample Name: hp1c67pg008 #1

---------------- Aaq. Operator : --- -- ------------------------------------------- EDE Seq. Line 2 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 3:02:55 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008(CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method In£o : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
Additional Info : Peak(s) manuallv i ntearated

ADCIA,ADC1 CHANNELA(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\001-0201.D) us/cm 90 I 80 ~ 70

f 60

50 

# ~

40-~ ~ ~ 30 `o

, t 0 20,
10

2 3 4 5 6_ 7 8 ., 9 min



# ____ _________________________________ External Standard Report

Sorted By Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADCl CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

### [min] [u5/cm*sl [ug/mLl 

# ------ I ---------- I ---------- I ---------- --1----------------- 4.028 MM 5.36339 4.05424e-2 2.17445e-1 Chloride 

## Manuallnt."II"(EDE)

Totals : 2.17445e-1



# ___ ________________________ *** End of Report ***

Eli Ellis 2/21/2012 4:51:41 PM Eli Ellis EA#0212-68 Page99of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FE3\HPLC67PG00B\HPLC67PG0082\001-0202.D Sample Name: hp1c67p9008 #1



### ------------- ----------------------------------------------------- Acq. Operator : EDE Seq. Line 2 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 3:17:03 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
Ar3ditional Trfo : Peak(s) manuallv intearated

ADC1 A, ADCi CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\001-0202.D) .

Fm 901 

# ~ I 

### 80 I 

### i 70 ~ 

### 60 50 ~ 

### 40 72 i 

# 30 `o 

# ~
20 ~ o0'L 

### r A U K ~ 

### I

,

N 

### 10 mPm ° P e a

. 

### .... ,.,._... ..___ ..-.

. 

### ._.,.-, ~ T ._~ I 0

4

_ 5

. . 6


### . 7



### _ 8


### ... 9



### _ min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDS Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [minj [uS/cm*e] [ug/mL]


# ------- -- ---- ---I- --------- ---------- -------- — — ----- 4.026 MM 5.33777 4.05915e-2 2.16668e-1 Chloride 

## Mnnuallnt."II"(EDE

Totals : 2.16668e-1

----------------------------------- *** End of Report ***

Eli Ellis 2/21/2012 4:51:51 PM Eli Ellis EA#0212-68 PageS00of122 Page 1 of 1Data File H:\HPLC2012Q1\MR EURNS\DATA\FEB\HPLC67PG008\HPLC67PG0083\001-2301.D Sample Name: hp1c67pg008 #1

--------------------------------------------------------- --- - -------- ------- Acq. Operator : EDE Seq. Line 23 ACq. Instrument : Mr_Surns Location Injection Date : 2/21/2012 10:32:00 AM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0083\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity Additional Info : Peak(s) manually integrated

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0083\001-2301.D) us/em 

# I d i

~ 90 80 i 70

60
50 

# ~

40 ~ - m 0 30

L 20 

# I 10 J a'Q

~ ° 

### ... °P

e

...... ,

..... ~ L.....



### ..... --T 0 

### -------- r ",- —`

~~ - ~T~ -

3 4 5 fi 7 8 9 min



### ---------------------------------- --- External Standard Re 

### p ort

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADCl A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amou.nt Grp Name 

### [min] [u5/cm*s] [ug/mL]

4.023 I NIM I 5.01746 I 4.12479e-2 I 2.06960e-1 1 IChloride 

### ManualInt."II"(EDE

Totals : 

### 2.06960e-1

_ 

# _____ _______________________________ *** End of Report ***

Eli Ellie 2/21/2012 4:52:02 PM Eli Ellis EA#0212-68 Page101Of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0083\001-2302.D Sample Name: hp1c67pg008 #1

--- -- _ _ ___---__- ---- ---- ---- — ---- ------ - --- - - - ---- ---- - Acq. Operator : EDE Seq. Line 23 Acq. Instrument : Mr_Burns Location Injection Date : 2/21/2012 10:46:06 AM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0083\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellie Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
Additional Info : Peak(s) manually intearated

ADC1 A, ADC1 CHANNELA(H \HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0083\001-2302.D 

# ~ uS/cm ~ o 90 ° 80- 70 ~ I i 60 ... I
50 - i 40- 0 30 ~ `o I 20 h,8'1h U o~,y0 I 1
10
6 -~-,T~.._.. ...... . —._ _—_._. .. .._ /..... ..._ ~ ...
I

. _ 2 3 4 5 6 7 8 9 min



# _______ ________________________

External Standard Report

Sorted By Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal l: ADCl A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ----------I---------- --1----------------- 4.021 MM 5.03293 4.12143e-2 2.07429e-1 Chloride 

## Manuallnt."II"(EDE

Totals 

# 2.07429e-1 ____°°°____-- -- --------------------------- *** End of Report ***

Eli Ellis 2/21/2012 4:52:11 PM Eli Ellie EA#0212-68 Page102of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\002-0301.D Sample Name: hp1c67pg008 #2

-------------------- Aaq. Operator -- -------- ------------------ ------------------- : EDE Seq. Line : 3 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 3:31:11 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellie Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3

. Flow Rate: 0.70mL/min Suppressed Ion Conductivity

ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNSIDATA\FEB\HPLC67PG008\HPLC07PG0082\002-0301.D) uS/cm c[ 

# ~

v, 

### 90 1 i
80 - 

### 70 I


### 60 I 50 i 

### 40 ~ ~ 30 s ° U 

### 20 0

O h 10 ~ N

.. ~~ .~ ... ~ ._..

. 2 3_ 4 5 9 ~ ~ -r 6 7 8 min

_______ External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal l: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------ I ---------- I ---------- I ---------- 1--I--

- - ---- ---- - - ---- 4.021 BB 30.05250 3.21357e-2 9.65758e-1 Chloride

Totals : 9.65758e-1



# -------------------- _____ ----- _________________ *** End of Report ***

Eli Ellis 2/21/2012 4:52:29 PM Eli Ellis EA#0212-68 Page103of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\002

- 0302.D Sample Name: hp1c67pg008 #2

Acq. Operator : EDE Seq. Line 3 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 3:45:19 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG008 2 \METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008(CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

### CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPL7PG008\HPLC67PG0082\002-0302.D)

F. A, ADCt C uS/cm 1 ~ 90 ° I 80 I 70 - 60 i I 50 i I ~ 40 m ~ o I 30 ° L I U 20 ~

o ~ ~

a d 10 0 - 2 3 4 5 6 7 8 9 min



## ______—______ _____________ External Standard Report

Sorted By Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDe Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- -I --- --1- 4.016 BB 29.67925 3.21587e-2 9.54445e-1 Chloride

Totals . 

## 9.54445e-1

°°°------------------------------- *** End of Report ***

Eli Ellis 2/21/2012 4:52:38 PM Eli Ellis EA# 0212-68 Page 104 Of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\002-1801.D Sample Name: hp1c67pg008 #2

_____________________ ____________ Acq. Operator : EDE Seq. Line 18 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 11:31:41 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CEEM32\1\METHODS\HPLC67PG008 (CL).M Last ahanged : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/imM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

AD01 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\002-1801,D) us/cm 90 - 

# ~

80 - 70- 

# ~ 60 1 50

40 ° I 30 `a U ~


# ~ 20 

### M 10 /

m a 

# ~ 2

6 

### I 2 3 4 5 6

_ 7 - 8 , 9 _min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, P.DCl CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I---------- I------

-- -- I ---------- 1--I----

---- --- -- - ---- 4.005 BB 28.34095 3.22460e-2 9.13882e-1 Chloride

Totals . 9.13882e-1

*** End of Report ***

Eli Ellis 2/21/2012 4:52:46 PM Eli Ellis EA# 0212-68 Page 105 Of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\002

- 1802.D Sample Name: hp1c67pg008 #2

--------- --------------------------------------------------------- Acq. Operator : EDE Seq. Line 18 ACq. Instrument : Mr Burns Location Injection Date : 2/20/2012 11:45:49 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysie Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

____--- - — _— - - ----- - ----- --- -- - - — ----------- - ---- External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal l: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s1 [ug/mL7 

## ------- I ------ I ---------- I ---------- I ---------- --1------------------ 4.005 BB 28.32162 3.22473e-2 9.13296e-1 Chloride

Totals : 9.13296e-1

- - -- -- - -- -- - — -- --- ----- - - ------- ---- ---- - - -- *** En.d of Report ***

Eli Ellis 2/21/2012 4:52:54 PM Eli Ellis EA# 0212-68 Page 106 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\003-0401.1) Sample Name: hp1c67pg008 #3



# -------------------------------------------------------------- -------- 

# -- - Acq. Operator : EDE Seq. Line 4 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 3:59:28 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG00B2\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/lmM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

F -- uS/cm ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNSIDATA\FEB\HPLC67PG008\HPLC67PG0082\003-0401.D 

### ~

~ 90 

### ~

- °) I 

# I

~ 80 -
70 -


### ~ 60 

### ~ 7 I l i 

# 50 °

a i i
401 `o U 

# v I 30
20 

### ~] 

# m 10 ~ ~ u'

~~ 

# m

~ (° J 

### ~ ~ ~
_ " - . 

### ~ ._...___, 

### ~
_ . ✓

_ 

### 5 4

~ — 

### - r

6 \ I 0 3 _._ 

### 7 8 9

~ r 

### mi n

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# - - I------ I ---------- I ---------- I ---------- I--i ------------------ 4.009 BB 166.42377 3.06392e-2 5.09909 Chloride

Totals : 5.09909



# -------------

____________ 

# ____.__-_____________-_______ *** End of Report ***

Eli Ellis 2/21/2012 4:53 :04 PM Eli Ellie EA# 0212-68 Page 107 oP 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\003-0402.D Sample Name: hp1c67pg008 #3

_______________ __ __________ _ Acq. Operator : EDE Seq. Line 4 Acq. Inetrument : Mr_Burns Location Injection Date : 2/20/2012 4:13:35 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Laet changed : 12/1/2011 6:52:23 PM by SJE Analysi5 Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column; Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

~ .-.. ADC1 A, ADC1 CHANNELA (H;\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\003-0402 D uS/cm H ~ 0

80 901 ~ 

### II I 70 I ' i

60 

# ~

50 a ' I 40 

### o
U i l 30, N



### ~ 20 M O



### V

~ 10

- i ,n m

_. .:.. , ~
_ .... ~.~ ~ . .... .
2 3 4 5 6 7 8 9 m in

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 use Multiplier & Dilution Bactor with ISTDs Signal 1: ADC1 A, ADCl CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL]


# - - I ---------- I ---------- I ---------- 1--i----

-- ----- ------ - 4.009 BB 165.83575 3.06404e-2 5.08127 Chloride

Totals : 5.08127

*** End of Report ***

Eli Ellis 2/21/2012 4:53 : 12 PM Eli Ellis EA# 0212-68 Page 108 Of 122 page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\003

- 19 01 .D Sample Name: hp1c67p9008 #3 

## °°°°°°°°°°°°°°°°°°°°°°°°° --- ________--------------------- Acq. Operator : EDE Seq. Line 19 ACq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 11:59:57 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 . Mobile Phase: 3.2mM.Na2CO3/1mM NaHCO3 F1ow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\003-1901,D 

# ~ I

uSlcm 

# ~ 90- i 

## 80-

70 -'
60 

# ~ 50
`o 

## 40 = U r 

### 30 0 0

M o 20 ~ \ C~ \

6 .-- —r~T-
. ~T 2 3 4 5 fi 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*sl [ug/mL] 

# ------- I ------ I ---------- I - I ---------- --1------------------ 4.004 BB 159.37566 3.06538e-2 4.88547 Chloride

Totals . 

## 4.88547

*** End of Report ***

Eli Ellis 2/21/2012 4:53 :22 PM Eli Ellis EA# 0212-68 Page 109 Of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\003-1902.D Sample Name: hp1c67pg008 #3

------------------ --------------- ------------------------------- Acq. Operator : EDE Seq. Line 19 Acq. Instrument : Mr_Burns Location Injection Date : 2/21/2012 12:14:05 AM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phaee: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\003-1902.D)

90 I 80 

# ~

70

- il

~ 60
50 40 - `o V

~ 30 r ~

0 0 M o 20 ~ M

I 0 2_ 3 ._ 4 5 6 7

_ 8 9

_ min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I---------- I ---------- I ---------- 1--1-------

- --------- - 4.004 BB 159.25688 3.06541e-2 4.88187 Chloride

Totals : 4.88187

--------------------------------------------------------------------- *** End of Report ***

Eli Ellis 2/21/2012 4:53 :33 PM Eli Ellis EA# 0212-68 Page 110 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\004-0501.D Sample Name: hp1c67pg008 #4

-------------------------------------------------------- Acq. Operator : EDE Seq. Line 5 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 4:27:43 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG00B\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analyeis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

°°°°°_°°°'°°°---- —
---------------- ---- ---------------- External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution: 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area. Amount Grp Name [min] [us/cm*s] [ug/mL] 

## ------- I ------ I ---------- I---------- I ---------- 1--i---------------

-- - 4.007 BB 335.45944 3.04730e-2 10.22247 Chloride

Totals : 10.22247

*** End of Report ***

Eli Ellie 2/21/2012 4:53:46 PM E1i Ellis EA# 0212-68 Page 111 Of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR 13URNS\DATA\FEB\HPLC67PG008\HPLC67PG008\004-0502.D Sample Name: hp1c67pg008 #4 

# ____--------------- -------------------------- ---------------- Acq. Operator : EDE Seq. Line 5 Acq. Inetrument : Mr_Burns Location Injection Date : 2/20/2012 4:41:51 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 5:07:12 PM by Eli Ellis (modified after loading) Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1A, ADCt CHANNEL A(H'.\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0081004-0502.D1 I 

### uS/cm ' P, , I 90~ 0
80

~ 70 - m o I II 60 `o ~ L 50 ~ m N ~ 40 M N ~ 30 20 - 1 h N (O O

I

_
16 V ~l °q

~.[ ~- _~l ` J ~ i_-~ ✓ ~~.,— ✓ ~--71 -. I 0. ,

2_ 3 4 -, 5 6 7 8

_ 9 min



# __________________________________

External Standard Report

8orted By

. Signal Calib. Data Modified . 2/21/2012 5:07:06 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I---

----- -- I ---------- I--1------

-- ----- ----- 4.266 BB 333.69577 3.04739e-2 10.16902 Chloride

Totals : 10.16902

End of Re --------------------------------------- 

# p ---------------- *** ort ***

Eli Ellis 2/21/2012 5: 07:15 PM Eli Ellis EA# 0212-68 Pdge 112 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\004-2001.D Sample Name: hp1c67pg008 #4

--------------------------------------------------------------------- Acq. Operator : EDE Seq. Line 20 Acq. Instrument : Mr_Burns Location Injection Date : 2/21/2012 12:28:13 AM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Qi\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\004-2001D. 

### uS/cm ~ 90 - ~ 80 ;
Il i



### 60 d 0 70 l



### a I L

40 M 30 i 20
n r 10

..._. 1 0 2 3_~ 4 5 6 7 8 9 Tin

External Standard Report

Sorted By

. Signal Ca1ib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Di].ution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/Cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- I--1- ----------------- 4.005 BB 323.20383 3.04793e-2 9.85101 Chloride

Totals : 9.85101

°°°°°°°°°°°°°°°--
- --- -- - - - - --- -- ------ ------- - --- *** End of Report ***

E1i Ellis 2/21/2012 4:54:05 PM Eli Ellis EA# 0212-68 Page 113 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\004

- 20 02 .D Sample Name: hp1c67pg008 #4 

# °°°°°°°°°°°______________°°°°°------------------- Acq. Operator : EDE Seq. Line : 20 Acq. Instrument : Mr_Burns .

~ Location Injection Date : 2/21/2012 12:42:21 AM Inj : 2 ACq. Method : C:\HPLC2012Q1\DATA\FE212\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analyeis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

90 

## ~ 

# 80 uS/cm ADC1 A, ADCi CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FE8\HPLC67PG008\HPLC67PG0082\004-2002.D 

## ~

I

~ 70 

## ~ m a 60 

# ~ o
50 V

m M i
O ~ O 40 _; 

# n v 30

, 20

.. 

## ~ ~~ ~ ~I , ~ ° 

# rn ~

0 10 

## ~

... ~ 

## ~D

~

._. 2

_ 3

_ 4

_ 5 6

_ 7 8 9 ,.min

External Standard Report

Sorted By Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilu.tion:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs
Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

# [min] [uS/cm*s] [ug/mL] 

# ------ I ---------- I ---------- I-------- -- 1--1---- -------------- 4.005 BB 323.56128.3.04791e-2 9.86184 Chloride

Totals : 

# 9.86184 _______°_°°°____°------------------------------------ *** End of Report ***

Eli Ellis 2/21/2012 4:54:14 PM Eli Ellis EA# 0212-68 Page 114 Of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PGOOS\HPLC67PG0082\005

- 0601.D Sample Name: hp1c67pg008 45

Acq. Operator °------------------------------------------------------------------ : EDE Seq. Line 6 Acq. Inetrument : Mr_Burn3 Location Injection Date : 2/20/2012 4:55:59 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SSE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008(CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM Na.HCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\005-0601.D) uS/cm 90 i 80 

# ~ a I o 

# ~ 70 7 V
60" 

# ~ 50 

# ~ I
40
30 

# ~
o a 20

~ 10 

### ~ N ~ V 0 2 3 ,_. 4 5 6 7 8 9

_ min

---------------------- External Standard Report -----------------------

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier;

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- 1--i--

------ - --------- 4.009 BB 502.16272 3.04187e-2 15.27515 Chloride

Totals : 15.27515

*** End of Report ***

Eli Ellis 2/21/2012 4:54:23 PM Eli Ellis EA# 0212-68 Page 115 Of 122 Pa.ge 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\005-0602.D Sample Name: hp1c67pg008 #5

Acq. Operator ------------------------------------------------------- : EDE Seq. Line 6 Acq. Instrument : Mr_Burne Location Injection Date : 2/20/2012 5:10:06 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysie Method : C:\CHEM32\1\METHODS\HPLC67PG008(CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\005-0602.0) us/cm w

80 a

_ 70 0 s 1
U I i 60 II

o 0 I 

# ~

i 40

30 

# ~

. 20.. O N
10 r 0 2 3 4 5 6 7 ., 8

_ 9

_ m in

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [u5/cm*s] [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- 1--i------------------ 4.007 BB 501.26697 3.04189e-2 15.24800 Chloride

Totals : 15.24800

--- - - ---- — ---- ------ - ---------- --- --- - - ---- *** End of Report ***

Eli Ellis 2/21/2012 4:54:32 PM Eli Ellis EA# 0212-68 Page 116 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\005-2101.D Sample Name: hp1c67pg008 #5

________________ ___ ---------------------- - Acq. Operator : EDE Seq. Line 21 Acq. Instrument : Mr_Burns Location Injection Date : 2/21/2012 12:56:28 AM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODB\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNELA (H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\005-2101.D) uS/cm 90 80 ~ o` I 70 U 60 ' m o ~

o ° 1 50 /~ a

401 ~ I i l I 

### y i I 30 w v

~ ~° i 20 6 o o r

~ 2. 10 ~ /~
_._ ~~ _,. 1 .._ ~ . ✓ ~~~ \..-_ ~ .....-/ ~ L1

. ~

~ 0l-__^

~~ -TTi

~ ri-T

2 3 4 5 6

- , 7

_ 8 9 mid

_____________________ _ ===
_ External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDe Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- i ------I---------- I ----------I---------- --1------------------ 4.006 BB 487.03375 3.04221e-2 14.81660 Chloride

Totals : 14.81660

*** End of RepOrt ***

Eli ElliS 2/21/2012 4:54:42 PM Eli E11is EA#0212-68 Page117of122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\005-2102.D Sample Name: hp1c67pg008 #5

--------------------------------------------------------------------- Acq. Operator : EDE Seq. Line 21 Acq. Instrument : Mr_Burns Location Injection Date :.2/21/2012 1:10:38 AM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008 (CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity
ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\005-2102.D1 

### ~ uS/cm 4 90 

### ~ ° i

` o 80 70 v

° o i 60 50

i~ 40
30 

### ~ ~I m n 

### ~

~ 

### 20

I 

### I ✓ ._.. , T , r

— —... J L _.,._,, _ ....:.
.. ~ .J_

. —. 

### 0
~ 2 3 4 5

_ 6 7 8 9 min

__________________ _______________ External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51;04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s1 [ug/mL] 

# ------- I ------ I ---------- I ---------- I ---------- --1------------------ 4.006 BB 486.89197 3.04222e-2 14.81231 Chloride

Totals : 14.81231

*** End of Report ***

Eli Ellis 2/21/2012 4:54:51 PM Eli Ellis EA# 0212-68 Page 118 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\00 6-0701 .D Sample Name: hp1c67pg008 #SS 

### °°°°°°°°°°°°°°°°°°_________ Acq. Operator 

### -------- 

### ----------------------------- : EDE Seq. Line 7 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 5:24:15 PM Inj : 1 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE

. Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008(CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

### ADC1 A, ADCi CHANNEL A(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\006-0701.D) uS/cm 

## ~ 7 ~ 90 80 70 1
, 

## ~ 60 i I 50
~ 

### 40 a 

### o i
30 ; U 

### 20 

### i 10 

### 0 2 3 

### 4 5 6 7 8 9 

### mir

----------------- =



# _______ _________________________________ _ External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier: 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDs
Signal 1: ADC1 A, ADC1 CHANNEL A
RetTime Type Area Amt/Area Amount Grp Name 

### [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ---------- i ----------I - ---- 4.007 BB 62.15482 3.11925e-2 1.93876 Chloride

Totals 

### 1.93876



### ___________________-- -------------------- *** End of Report ***

Eli Ellis 2/21/2012 4:55:12 PM Eli Ellis EA# 0212-68 Page 119 of 122 Page 1 of 1Data File H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\006-0702.D Sample Name: hp1c67pg008 #SS

Acq. Operator 

### --------------------------------------------- -----

: EDE Seq. Line 7 Acq. Instrument : Mr_Burns Location Injection Date : 2/20/2012 5:36:22 PM Inj : 2 Acq. Method : C:\HPLC2012Q1\DATA\FEB12\HPLC67PG008\HPLC67PG0082\METROHM.M Last changed : 12/1/2011 6:52:23 PM by SJE Analysis Method : C:\CHEM32\1\METHODS\HPLC67PG008(CL).M Last changed : 2/21/2012 4:51:31 PM by Eli Ellis Method Info : Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity 

### ADC1 A, ADC1 CHANNEL A(H:\HPLC2012Q1\MR BURNSIDATA\FEB\HPLC67PG008\HPLC67PG0082\006-0702.D) uS/cm 

### 90 a! 80 1 I l i I 70 , 

### I

~ 

### I 60 l i 50 - 40 ° I 

### 30

~ U 

### 20 , m 10
.r ✓ _.. 

### 0 ",-' ~~-I~~ -,—ITr'

~ „-,- ~~ -r' ~~ T
2 3 4 5 6 7 8 9 min

External Standard Report

Sorted By

. Signal Calib. Data Modified . Tuesday, February 21, 2012 4:51:04 PM Multiplier:

. 1.0000 Dilution:

. 1.0000 Use Multiplier & Dilution Factor with ISTDS
Signal 1: ADC1 A, ADC1 CHANNEL A RetTime Type Area Amt/Area Amount Grp Name [min] [uS/cm*s] [ug/mL] 

# ------- I ------ I ----------I----------I---------- I--i ------------------ 4.007 BB 62.25212 3.11911e-2 1.94171 Chloride

Totals : 

### 1.94171

__ ___ _ __ ______ _ _— - - - -__ --- - ----- - - -- — - - ----- - --------- ------ *** End of Report ***

Eli Ellis 2/21/2012 4:55:23 PM Eli Ellis EA# 0212-68 Page 120 of 122 Page 1 of 1method: C:\HPLC2011Q1\MR BURNS\METHODS\METROHM.M Modified on: 4/1/2010 at 4:15:36 PM

Method Information Method: C:\HPLC2011Q1\MR BURNS\METHODS\METROHM.M Modi£ied: 4/1/2010 at 9:15:36 PM
Column: Metrosep A Supp 5 Mobile Phase: 3.2mM Na2CO3/1mM NaHCO3 Flow Rate: 0.70mL/min Suppressed Ion Conductivity

--------- -- ANALOG DIGITAL CONVERTER

- 

# I

------------------------------- Signal l ------

--------------------- Description: ADCl CHANNEL A Source: Signal Unit: uS/cm Units/volt: 1.00.000 Peakwidth (Data Rate): 0.027 Min (10.00 Hz) Stop Time: No Limit Data Storage: A11 Start Signal Source: External Device Will Start 35900

Timed Event Table: <no events>

Mr Burns 4/22/2011 10:55:13 AM KHB EA# 0212-68 Page 121 of 122 Page 1 of 1

# This Is The Last Page

Of This Report.



# ~

EA# 0212-68 Page 122 of 122YourProject# 141.11-210N

~ Your Project Name: General Shale Sample'rypeo Liquid Collectiou Date: 02/02/12 Collected By: Client Receipt Date: 02/02/12 12:00 

# - CERTIFICATE OF ANALYSIS -

Report Date: 10-Fe6-12

Client ID: WILCOX ENV2

Wilcox Environmental Eng. 5757 West 74th Street Indianapolis, Indiana 46278 Attn: Joe Kinder

Our Lab # 12001353-001

' Your Project # 141.1 L210N : Ymir Project Name: General Shale SampleType: Liquid Phone: (317)472-0999 FAX: (317) 472-0993 Your Sample ID: Blank KMN04

Callection Date: 02/02/12 CollectedBy: Client Recelpt Date: 02/02/12 12:00

Mercury in etnissions, CVAA 

### AnaTVfiical Method Prep Method Prep Date II 

### ~ Method 29 Method 29 2/9/2012 ]mcleary Quant, Analysis Parameter Result Units Qual Limit CAS # Date By Mercury, Hg < 150 ug 2.50 7439-97-6 2/912012 Imoleary

Our Lab # 12001353-002 Your Sample ID: Blank Nitric 

### ~

GFAA P6 emissions 

### Analvtical Method Prep Method Prep Date By Method 29 Method 29 218/2012 lmcleary

D

•• • ug i• • •

Lab# 12001353-002 Sample ID: Blank Nitric Page / of 7 

# ESC Laboratories
5927 WEST 71 ST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA 46278 FAX (317) 290-1670Our Lab # 12001353-003 Your Sample ID: Run I KMN04

YourProject# 141.11-210N Collection Date: 02/02/12 Your Project Name: General Shale Colleeted By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

Mercury in emissions, CVAA 

### Analvtical Method Prep Method Pren Date Bv Method 29 Method 29 219/2012 lmoleary
! : Qual Limit CAS # 1

r 0

- 

### h am.=-

~ 

### o' ,

Our Lab # 12001353-004 Your Sample ID: Run 2 KNIlVO4
Your Project # 141.11-210N Collection Date: 02/02/12 i Your Project Name: General SBale Collected By: Client

: Sample Type: Giquid Reeeipt Date: 02/02/12 12:00

Mercury in emissions, CVAA 

### AnalVtical Method Pren Method Prep Date By 

### Method 29 Method 29 2/9/2012 Imcleary Quant, Analysis Parameter Result Units Qual Limit CAS # Date By Mercury, Hg 10.3 ug 2.50 7439-97-6 2/9/2012 Imcleary

OurLab# 12001353-005 Your Sample ID: Run 3 KMN04
Your Project # 141.11-210N Coliection Date: 02/02/ 12 Your Projecf Name: General Sbale Collected By: Client

, Sample Type: Liquid Receipt Datet 02/02/12 12:00

Mercury in emissions, CVAA 

### Analvtical Method Prea Method Prep Date Dy, 

### Method 29 Method 29 2/9/2012 Imcleary



### ! ! 

### L imit CAS ff D.
7. 05 ug 2.50 0

Lab # 12001353-005 Sample ID: Run 3 KMN04 PaSe Z of 7 

# ESG Laboratories

5927 WEST 71 ST STREET PHONE (317) 290-1471

... _ . INDIANAPOCIS,INDIANA 46278

......... ......... .._...... ~ ._.. - ..._ ._ . ... . .... .. ... .... .... ... - FAX(317)

- 290-1870.

.Our Lab # 12001353-006 Your Sample ID: Run 1 Nitric C4

YourProject# 141.11-210N Collection Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

GFAA Pb emissions 

### Analvt'ical Method Prep Method, PreD Date By Method 29 Method 29 2/8/2012 Imcleary

• 

### Qual Limit CAS # l.

0 0
z ~

OurLab# 12001353-007 Your Sample ID: Run 2 Nitric C4A
Your Project # 141.1 1-210N Callection Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sampte Typee Liquid Receipt Date: 02102/12 12:00

GFAA Pb emissions 

### Analvtical Method Prep Method PreQ Date By Method 29 Method 29 2/8/2012 lmcleary Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Lead, Pb t 1.65 ug 1.65 7439-92-1 2/912012 Imcleary

Our Lab # 12001353-009 Your Sample ID: Run 3 Nitric C4A ~
YourProject# 141.11-210N Collection Date: 02102/12

~ Your Project Name: General Shale Cullected By: Client '. Sample Type: Liquid 

### Receipt Date: 02/02/12 12:00

GFAA Pb emissions 

### Analvtical Method Prep Method Prep Date Bv 

### Method 29 Method 29 2/8/2012 lmcleary

• Qual Limit CAS # D
0

Lab # 12001353-008 Sample ID: Run 3 Nitric C4A Page 3 of l 

# ESG Laboratories

5927 W EST 71 ST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46276 FAX (317) 290•1670Our Lab # 12001353-009 Your Smnple ID: Run I Nitric Probe

YourProject# 141.11-210N Collection Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:OD

GFAA Pb emissions 

### Ana]Ytical Method Prep Method Prep Date Bv Method 29 Method 29 2/8/2012 ]mcleary

• Qual Limit CAS t• 0

. 180 r 

# xc - A s..y-a, a s. , .>"r<. ✓ .v ~,~', ~~~ r F ~.~e~ -?='

~ '3

~ _ , ~ .. ~ . , v.

~ a „,iE ~ ~ 2, ~ f„ : i e ~'~ ,::'.
Our Lab # 12001353-010 Your Sample ID: Run 2 Nitric Probe
YourProject# 141.11-210N Collection Date: 02/02/ 12 Your Project Name: General Shale Colleeted By: Cllant

. SampleTypec Liquid Reeeipt Date: 02/02/12 12:00

GFAA Pb emissions 

### Analytical Method Prel) Method Preu Date Bv Method 29 Method 29 2/8/2012 lmcleary



### • Qual Limit CAS # 1: 0

. 946 ug 0

, 220 t



### ~

~ OurLabq 12001353-011 Yonr Sample ID: Run 3 N itrlc Probe
YmrrProject# 141.11-210N Collection Date: 02/02/12 Yonr Project Name: General Shate Colteeted By: Cllent SampleType: Liquid Recelpt Date: 02102/I2 12:00

GFAA Pb emissions 

### Analvtical Method Prep Method Prep Date BY Method 29 Method 29 2/8/2012 lmcleary

• Qual Limit CAS V D. 0

, 697 Lig

. •

Lab # 12001353-011 Sample ID: Run 3 Nitric Probe Page ® of 7 

# ESG Laboratories
5927 W EST 71 ST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46278 FAX (317) 290-1670Our Lab # 12001353-012 Your Sample ID: Run l Nitric CSA

Your Project # 141.1 I-210N Collection Date: 02/02/12 !. Your Pruject Name: General Shale Collected By: Client

, SampleType: Liquid Recefpt Date: 02/02/12 12:00

GFAA Pb ernissions Analvtical Method Pren Method Pren Date By Method 29 Method 29 2/8/2012 Imcleary Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Lead, Pb 0.552 ug 0.0850 7439-92-1 2/9/2012 Imcleary

, Our Lab # 12001353-013 Your Sample ID: Run 2 Nitric C5A

YourProject# 141.11-210N Col7ection Date: 02/02/12 Yonr Projeet Name: General Shale Collected By: Client SampleType: Liquid Receipt Date: 02/02/ 12 12:00

GFAA Pb emissions Analytical Method P,rep Method Prep Date ay Method 29 Method 29 2/812012 Imeleary

• Qual Limit CAS # 1
t 0

. 120 0



## . ., . .S

. :. 4^

~ 

## " 3

~ 

## •, f ,,. . J

_
Our Lab # 12001353-014 Your Sample IDe Run 3 Nitrie C5A
Ymv Projeet # 141.11-210N Colleotion Date: 02/02/12 Your Project Name: General Shale Coneeted By: Ctient Sample Type: Liquid Receipt Date: 02/02/12 12:00

GFAA Pb emissions Analytical Method Prea Method Pren Date By Method 29 Method 29 2/912012 Imcleary Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Lead, Ph < 0.0650 ug 0.0650 7439-92-1 219/2012 Imcleary

Lab # I2001353-014 Sample ID: Run 3 Nitric C5A Page 5of7 

# ESG Laboratories

5927WEST7ISTSTREET - PHONE (317) 290-1471 INDIANA°OLlS, INDIANA46275 FAX (317) 290-1670Our Lab # 12001353-01 S Your Sample ID: Run 1 Nitric CSC

YuurProject# 141.11-210N Collection Date: 02102/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12r00

GFAA Pb emissions 

### Analvtical Method Prep Method Prep Date By Method 29 Method 29 2/9/2012 lmcteary Q . Qual Limit CAS # 1 0,145 ug 0 0

OurLab# 12001353-016 Your Sample @: Run 2 Nitric C5C
YourProject# 141.11-210N Collectton Date: 02/02/12 Your Project Name: General Shale Collected Byr Client Sample Type: Liquid Receipt Date: 02102/12 12:00

GFAA Pb emissions 

### Analytical Method Prep Method Prep Date By Method 29 Method 29 2/9/2012 Imcleary Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Lead, Pb 0.261 ug 0.165 7439-92-1 2/1012012 Imcleary

OurLab# 12001353-017 Your Sample ID; Run 3 Nitric CSC
YourProject# 141.11-210N Collection Dater 02/02/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

GFAA Pb emissions 

### Analvtical Method Prep Method Prep Date By Method 29 Method 29 2/9/2012 Imeleary Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Lead, Pb < 0.165 ug 0.165 7439-92-1 2I1012012 4ncleary

Lab # 12001353-017 Sample ID: Run 3 Nhric C5C Page 6 of 7 

# ESG Laboratories
5927 WEST7ISTSTREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA 46278 FAX (317) 290-1670OurLab# 12001353-01$ Your Sample ID: Run 2 Nitric C4B

' Your Project # 141.11-210N Collection Date: 02/02/12 ! Your Project Name: General Sbale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

GFAA Pb emissions 

### Analvtical Metbod Prep Method Pren Date Bv Method 29 Method 29 2/9/2012 Imcleary

• Qual Limit CAS it 1 0

. 120 0

. 120 0

_

Our Lab # 12001353-019 Your Sample ID: Run 3 Nitric C4B
Your Projeet # 141.1 1-210N Collection Date: 02/02/12 YourProjectName: General5hale Collected By: Client SampleType: Liquid Receipt Date: 02/02/12 12:00

GFAA Pb emissions 

### Analvtical Method Pren Method Prep Date B Method 29 Method 29 2/9/2012 lmcleary Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Lead, Pb < 0.115 ug 0.115 7439-92-1 2/9/2012 Imcleary

Lab Man 

# ~ 2/10/2012
Date

Lab # 12001353-019 Sample ID: Run 3 Nitric C4B Page 7 of 7 

# ESG Laboratories

5927 W EST 71 ST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46278 FAX (317) 290-1670

# O Z:



### R o

6 6



# z zzz;zzzz .........

ro O Z~ b

O



# IE y

PA7E O



# O

>0 

# O

z 0-I

ff



# Cl 

# d D 0

41 

## p

1 

## <

Q

zzzzzzz

rA rA

## - CERTIFICATE OF ANALYSIS -

Report Date: 

### 02-Mar-I2

Client ID: WILCOX ENV2

Wiloox Envuonmental Eng. 5757 West 74th Street Indianapolis, Indiana 46278 Phone: (317) 472-0999 Attn; Mack Overton FAX: (317) 472-0993

i Our I,ab i! 12001772-001 - Your Sample ID: Blank Nitric

I , Your Project M 141.11-210N Collectian Date: 02/02/I2 Your Project Name: Geaeral Shale Collected By: Client SampleType: Liquid ReceiptDate: 02/02/12 12:00

Antimony, ICP-AES Analyt' ical Method Prep Method Preu Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS #t Date By Antimony, Sb < 19.4 ug 19.4 7440

- 36

- 0 312/2012 kfoltz

Beryllium, ICP-AES Analvtical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Beryllium, Be < 0.776 ug 0.776 7440-41-7 312/2012 kfoltz

Arsenic, ICP-AES Analvtical Method Preu Method Pren Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz
Quant. Analysis Parameter Result Units Qual Limit ---,—___..---...---..

~ _,— CAS # Date By

---- — Arsenic, As < 1.94 ug 1.94 7440-38-2 3/212012 kfoltz

Selenium, ICP-AES Analvtical Method Prea Method Preo Date By SW8466010B SW8463010A. 2/21/2012 kfoltz

. Quant. Analysis Parameter Result Units Qual L irn it CAS # Date By Selenium, Se "---T

~ — < 1.94 ug 1.94 7782-49-2 3/2/2012 J

~ kfoltz

~
Lab it 12001772-001 Sample ID: Blank Nitric Page 1 af30 

# ESG Laboratories

5927 WEST 71ST STREET PRONE (317) 290-1471 INDIANAPOLIS, INDIANA46278 FAX (317) 290-1670Cobalt, ICP-AES Analvtical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/21Y2012 kPoltz Quant. Analysis Parameter Result Units 

### ------_-----------

Qual Limit CAS # Date By 

### -----'— Cobalt, Co < 3.88 ug 3.88

_ ~ 7440-48-4 3/2/2012 kfoltz



### Cadminm,ICP-AES Analvtical Method Prep Method Prep Date 

### By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Pararneter - Result Units Qual Limit CAS # Date By Cadmium, Cd < 194 ug 1.94 7440-43-9 3/2/2012 kfoltz

Chromium, ICP-AES Analytical Method Preu Method Prep Date 13V SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Quaf Limit CAS # Date By Chromium, Cr < 3.88 ug 3.88 7440

- 47

- 3 312/2012 kfoltz

Manganese, ICP-AES Analvtical Method Prep Method Pren Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn < 1.94 ug 1.94 7439-96•5 3/2/2012 kfoltz

Nickel, ICP-AES Analytical Method Preo Method Prep llate By SW8466010B SW8463030A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Nickel, Ni < 3.88 ug 3.88 7440-02-0 312/2012 kfoltz

Lab # 12001772-001 

# ESG Laboratories
5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 Sample ID: Blank Nitric Page 2 oJ j 30

PHONE (317) 290-1471 FAX (317) 290-1670Our Lab # 12001772-005 Your Sample ID: Run 1 Nitric Probe


# ~ I ~ Your Project # 141.11-210N Collection Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02102/12 12:00

Antimony, ICP-AES Analvtical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb < 18.0 ug 18.0 7440-36-0 3/2/2012 kfoltz

Beryllium, ICP-AES Analvtieal Method Prep Method Prep Date BV SW846 6010B SW846 3010A 2/21/2012 1<foltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Beryllium,Be <0.720 ug 0.720 7440-41-7 3/2/2012. kfoltz

Arsenic, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Arsenic, As < 1.80 ug 1.80 7440-38-2 302012 kfoltz

Selenium, ICP-AES Analvtical Method Prep Method PrepDate By SW846601OB SW8463010A 2/21/2012 kfoltz

. Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Selenium, Se < 1.80 ug 1.80 7782-49-2 312/2012 kfoltz

Cobalt, ICP-AES Analvtical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cobalt, Co < 3.60 ug 3,60 7440-48-4 3/2/2012 kfoltz

Cadmitun, ICP-AES Analytical Method Prep Method Pren Date BY

- SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual L im it CAS # D ate By
Cadmium,Cd ...._..—..—_._-.._<._,. —_...... 1,80 ug

. 1.80 7440-43-9 312/2012 kfoltz
Lab q 12001772-005 Sample ID: Run 1 Nitric Probe Page 9 of30 

# ESG Laboratories

5927 WEST7IST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46278

. FAX (317) 290-1670Lab # 12001772-005 Sample ID: Ran 1 Nitric Probe 

# ESG Laboratories

5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 PHONE (317) 290-1471 FAX (317) 290-1670 Puge 10 of 30 Chromium, ICP-AES

. Analytical Method Pren Method Pren Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Unfts Qual Lim9t CAS # Date By
Chromium,Cr <3.60 ug 3.60 744047-3 3/2/2012 kfoltz

Manganese, ICP-AES Analytical Method Prep Method Prep Date BySW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qnal Limit CAS # Date By Manganese, Mn < 1.80 ug 1.80 7439-96-5 312/2012 kfoltz



### r. Prep Method Prep 1 . 61 . 301 OA 2/21J2012

.



### !
. ! 1

~ ' ex a !

~ ,v

~ , ,,, z .: i t ~'r~~ -.2.. L.

~ Bh.'cnt..

~~ r.,.- v 60 ug

r ~ .e 1 rc

. exr
~ . S G. 'K' ~~ ~ r tim

~ .tt,
. ~ 5:. t,uf4a`^,'M1 3.60 d t

~ 4 x

~ . .,,.'2mu s

~d~ ?8a,

~ + ':

~ .-? 440 0 0

'

- I~ , - ~ k

,, ; .,.M,k 0Our Lab # 12001772-008 Your Sample ID: Run 1 Nitric C5A

YourProjectq 141.11-210N Collection Date: 02/02/12 Your Project Name: GeneraEShale Coflected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

Antimony, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb < 17.0 ug 17.0 7440-36-0 3/2/2012 kfoitz

Beryllium, ICP-AES , Analvtical Method Prep Method Prep Date Bv SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit. CAS # Date By Berylllum,Be <0.680 ug 0.680 7440-41-7 3/2/2012 kfoltz

Arsenic, ICP-AES Analvtical Method Pren Method Pren Date Ry SW846 6010B SW846 3010A 2/2112012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Arsenic, As ` W < 1.70 ug 1.70 7440-38•2 3/212012 ^T kfoltz

Selenium, ICP-AES Analytical Method Prep Methnd Prep Date ~ SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Paranreter Result Units Qual Limit CAS # Date By

--- .........___ Selenium, Se < 1.70 ug 1.70 ----.._—...__....___ 7782-49-2 3/2/2012 kfoitz

Cobalt, ICP-AES Analvtical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz

. Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cobalt, Ca < 3.40 ug 3.40 7440-48-4 31212012 kfoltz

Cadmium, ICP-AES Analvtical Method Prep Method Preu Date By SW8466010B SW8463010A 2/21/2012 kfoltz

. Quant. Analysis Parameter Result Unita Qual Limit CAS# Date ByLab N 12001772-008 Sample ID: Run 1 Nitric C5A 

# ESG Laboratories
5927 WEST 71 ST STREET INDIANAPOI.IS , INDIANA4627$ PHONE (317) 290-1471 FAX (317) 290-1670 Poge 76 oj30 Chromium, ICP-AES Analvtical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfolt7 Qnant. Analysis Parameter Result Units Qual Limit CAS # Date By
Chromium, Cr < 3.40 ug 3.40 7440-47•3 312/2012 kfoltz

Manganese, ICP-AES Analytical Method Prep Method Prel) Date By SW8466010B SW8463010A 2/21/2012 kfoltz

Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn 1.70 ug 1.70 7439-96-5 31212012

~ kfoltz

r Prei) Metliod Pret) 1

: ..1 1' SW846 3010A 2/21/2012 kfo ltz



### , Q 

# Nm3

~~ 

# tw ~% uin l~a~ 4



# h,-,.

~ 

# ' .°-7 j u l"

, 40 ug 3A0 440 0 0 0Our Lab # 12001772-011 Your Sample ID: Run 1 Nitric C5C

Your Project # 141.11-210N Collection Date: 02/02/12 Your Project Name: General Shale Collected Byc Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

Antimony, ICP-AES Analvtical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant, Analysis Parameter Result Units Qual Limit CAS # Date By

i Antimony,Sb mammsmsmm <29.0 ug 29.0 7440-36-0 3/2/2012 kfoltz

Beryllium, 1CP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result IInits Qual Limit CAS # Date By Beryllium, Be

~ ^ 

### mmnm ^ < 1.16 ug 1.16 7440-41-7 31212012 kfoliz

Arsenic, ICP-AES Analytical Method Prep Method Prep Date By SW846 6010B SWS46 3010A 2/21/2012 kfoltz Quant, Analysis Parameter Result Units Qual Limit CAS # Date By

m- Arsenic, As < 2,90 ug 2.90 7440-38-2 302012

~ kfoltz

Selenium, ICP-AES Anal t y ical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By

--- Selenium, Se somm - ------..._.,_.___

. 26.7 ug 2.90 -----'--__.--------

7782-49-2 3/2/2012 kfoltz

Cobalt,lCP-AES Analvtical Method Prep NIethod Prep Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cobalt, Co < 5.80 ug 5.80 7440-48-4 3/2/2012 kfoltz

Cadmium, ICP-AES Analvtical Method Preu Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cadmlum,Cd

. <2.90 ug 2.90 7440-43-9 3/212012 kfoltz

Lab # 12001772-011 Sample ID: Run 1 Nitric C5C Page-21 of30 

# ESG Laboratories

5927 WEST 71ST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46278 FAX (317) 290-1670Lab # 12001772-021 Sample IDn Run 1 Nitric C5C 

# ESG Laboratories
5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 PHONE (317) 290-1471 FAX (317) 290-1670 Page 22 of30 Chromium, ICP-AES Analytical Method Prep Method Prep Date By

. SW9466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Chromium, Cr < 5.80 ug 5.80 7440-0.7-3 312/2012 kfoltz

Manganese, ICP-AES Analytical Method Prep Method Prep Date By

. SW8466010B SW8463010A 2/2l/2012 kfaltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn 52600 ug 290 7439-96-5 3/2/2012 kfoftz

Nicl<el, ICP-AES Analytical Method Prep Method Pren Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
` Nickel, Ni < 5.80 ug 5.80 7440-02-0 312/2012 kfoltzOur Lab # 12001772-002 Your Sample ID: Run 1 Nitric C4

Your Project # 141.11-210N Collection Date: 02/02/12 Your Projeet Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

Anrimony, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A 2/2112012 kfoltz Qnant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb < 28.0 ug 28.0 7440-36-0 31212012 kfoltz

Berylliiim, ICP-AES Analvtical Method Prep Method Pren Date BY SW8466010B SW8463010A 2/21/2012 kfoltz Quant: Analysis Parameter Result Units Qual Limit CAS# Date By Beryllium, Be < 1.12 ug 1.12 7440-41-7 312l2012 kfoitz

Arsenic, ICP-AES Analvtical Method Prep Method Prep Date 1I ~ SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Arsenic, As < 2.80 ug 2,80 7440-38-2 312/2012 kfoitz

Selenium, ICP-AES Analvtical Method Preu Method Prep Date By SW8466019B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Selenium, Se < 2.80 ug 2.80 7782-49-2 3/212012 kfoltz

Cobalt, ICP-AES Analytical Method Prep Method Prep Date BV SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS# Date By Cobalt, Co

~ < 5.60 ug 5.60 7440-48-4 3/212012 kfoltz

Cadmium, ICP-AES Analvtical Method Prep Method Preu Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter

_.. Result Units

...,_. ~ .__--.._.._... Qnal Limit CAS # Date By Cadmium, Cd < 2.80 ug 2.80 7440-43-9 31212012 kfoltz

Lab # 12001772-002 Sample ID: Run 1 Nitrie C4 Page 3 of 30 

# ESG La.boratories
5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 PHONE (317) 290-1471 FAX (317) 290-1670Lab # 12001772-002 Sampfe 1D: Run 1 Nitric C4 

# ESG Laboratories

5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 PHONE (317) 290-1471 FAX (317) 290-1670 Page 4 of 30 Chromium, ICP-AES Analytical Method Preu Method Pren Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Chromium, Cr < 5.60 ug 5.60 7440-47-3 3/212012 kfoltr

Manganese, ICP-AES Analytical Method Preo Method Preo Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn 8.76 ug 2.80 7439-96-5 3/2/2012 kfoltz

.d ) Metho ) ! 601 1' SW846 JOIOA ! kfoltz

, ! Limit CAS # 1.
0 ug 5.60 ! 0 0 !Our Lab # 12001772-012 Your Sample ID: Run 2 Nitric C5C

Your Project # 141.11-210N Collection Date: 02/02/12 Your Project Name: GeneralShale Collected By: Client SampieType: Liquid Receipt Date: 02/02/12 12:00

Antimony, ICP-AES AnalVtical Method Preu Method Preu Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb < 33.0 ug T 33.0 7440-36-0 3/2/2012 kfoltz

Beryllium, ICP-AES Analvtical Method Preu Method Pren Date By SW8466010B SW8463010A 2/21/2012 kfoltz

Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Beryllium, Be ^ < 1.32 ug 1.32 7440-41-7 3/212012 T kfoltz

Arsenic, ICP-AES Analytical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Psrameter Result Units Qual Limit CAS # Date By
Arsenic, As 3.30 ug 3.30 7440-38-2 31212012 

### onszmmmmmom kfoltz

Selen' rum, ICP-AES Analytical Method Prea Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant, Analysis Parameter Result Units Qnal Limit CAS # Date By
Selenium, Se 32.9 ug 130 7782-49-2 3/2/2012 ^ kfaltz

Cobalt, ICP-AES Analvtical Method Preu Method Prep Date Ey SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS #

. Date By
Cobalt, Co

~ ~ ^ < 6.60 ug 6.60

_ 7440-48-4 312/2012 kfoltz

Cadmium, ICP-AES Analytical Method Pren Method Preu Date Bv_ SW846 6010B SW846 3010A 2121/2012 kfoltz Quant. Analysis Parameter Result Units Quai Limit CAS# Date ByLab M 12001772-012 Sample ID; Run 2 Nitric C5C 

# ESG Laboratories

5927 WEST 71ST STPEET INDIANAPOLIS, INDIANA46278 PHONE (317) 290-1471 FAX (317) 290-1670 Page 24 oj30 Chromium, ICP-AES Analvtical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Chromium, Cr < 6.60 ug 6.60 7440-47-3 3/2/2012 kfolfz

Manganese, ICP-AES Analytical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese,Mn 63400 ug 330 7439-96-5 312/2012 kfoltz



### o PrepMethod Prep 1 SW8 46 61 1' SW846 3010A 2/21/2012 kfo ltz

, 

### Q u

„c..Ke.: s".rw ;! Ho ffi.p 60 ug 6.60 0 Q

b $
. ~ . . t 0

.2. m

~ -- . ,- nOur Lab # 12001772-014 Your Sample ID: Run 2 Nitric C4B

YourProject# 141.11-210N Coilection Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02112 12:00

Antimony, ICP-AES Analytical Method Preo Method Pren Dato 

## B SW846 6010B SW846 3010A 2/21/2012 kfoltz

. Quant. Analysis Parameter ftesult Units Qo al Lim it CA S # Date By Antimony, Sb < 12.0 ug 12.0 7440-36-0 3/2/2012 kfoltz

Beryllium, ICP-AES Analytical Method Prep Method Prep Date 

## Bv SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter R e sult Units Qual Limi t CAS # Date By Beryllium, Be < 0.480 ug 0.480 7440-41-7 312/2012 kfaltz

Arsenic, ICP-AES Analytical Method Prep Method Prep Date By

. SW8466010B SW8463010A 2/21/2012 kfoltz

. Quant. Analysis Parameter R e sult Units Q ual Litnit CAS # Date By Arsenic, As < 1.20 ug 1.20 7440-38-2 3/2/2012 kfoltz

Selenium, ICP-AES

Parameter Analvtical Method SW8466010B

Result Units Prep Method SW8463010A Quant. Q u a l Limit Prep Date

2/21/2012

CAS # 

## B

kfoltz Analysis D ate By Selenium, Se

. < 1.20 ug 1.20 7782-49-2 3/2/2012 kfoltz

Cobalt, ICP-AES Analytical Method PreD Method Pren Date Rv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Q ua l Li mit CAS # Date By Cobalt, Co < 2.40 ug 2.40 7440-48-4 31212012 kfoRz

Cadmium, ICP-AES Analvtical Method Prep Method Prep Date BY SW846 601OB SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Liinit CAS # Dat e ByLab # 12901772-014 Sample iD: Run 2 ilitric C413 

# ESG Laboratorres

5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA 46278 PHONE (317) 290-1471 FAX (317) 290-1670 Page 28 oj30 Chromium, ICP-AES Anatvtical Method Preo Method Prep Date By SW846 6010B SW846 3010A 2/2I/2012 kfoltz

. Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Chromium, Cr < 2.40 ug 2.40 7440-47-3 31212012 kfoltz

Manganese, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B

. SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn < 1.20 ug
~ 1.20 7439-96-5 3/2/2012 kfolfz

Nickel, ICP-AES Analvtical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz

. Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Nickel,Ni <2.4D ug 2.40 7440-02-0 3/2/2012 kfoltzOur Lab # 12001772-003 Your Sample ID: Rim 2 Nitric C4A

Your Projeet # 10.1.11-210N Collection Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sampie Type: Liquid Receipt Date: 02/02/12 12:00

AntimOny, ICP-AES Analvtical Method Prep Method Prep Date Bv SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant, Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb

~ < 33.0 ug 33.0 7440-36-0 3/212012

~ kfoltz

Beryllium, ICP-AES Analvtical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/20I2 kfoltz Quant. Analysis Parameter

. Result Units Qual Limit CAS # Date By Beryllium,Be <1,32 ug 1.32 7440-41-7 3/2/2012 kfoltz

Arsenic, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 lcfoltz Quant. Anatysis Parameter Result Units Qual Limit CAS# Date By
Arsenic, As < 3.30 ug 130 7440-38-2 31212012 kfoltz

Selenium, ICP-AES Analytical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfaltz Quant. Analysis Parameter Result llnits Qual Limit CAS # Date By
Selenium, Se < 3.30 ug 3.30 7782-49-2 3l212012 kfoltz

Cobalt, ICP-AES Artalvtieal Mettiod Prep Mettiod Prep Date py SW846 6010B SW846 3010A 2/21/2012 kfoltz

- Quant. Analysis Parameter - Result . Units Qual Lirnit CAS # Date By
Cobalt, Co < 6.60 ug 6.60 7440-48-4 3/212012 kfoltz

Cadmium, ICP-AES Anaiyt' rcal Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cadmium, Cd < 3.30 ug 3.30 7440-43-9 312/2012 kfoltz

Lab # 12001772-003 Sample ID: Run 2 Nitric C4A Page 9 oj30 

# ESG Laboratories

5927 WEST7ISTSTREET INDIANAPOLIS, INDIANA 46278 PHONE (317) 290-1471 FAX (317) 290-1670Lab tS 12001772-003 ' Sample ID: Run 2 Nitrlc C4A 

# ESG Laboratories
5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 PHONE (317) 290-1471 FAX (317) 290-1670 Page 6 of 30 Chromium, ICP-AES AnaIVtical Method Prep Method Prep Date By SW8466010B SW8469010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS N Date By Chromium, Cr EM < 6.60 ug 6.60 7440-47-3 3/2/1012 kPaltz

Manganesc, ICP-AES Analvtical Method Prep Method Prep Date By, SW8466010B SW8463010A 2/2112012 kfoltz Quant. Aualysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn - 13.1 ug 3.30 7439-96-5 3/212012 kfoltz

Nickel, ICP-AES Analytical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz

_ Quant, Anaiysis Parameter ResuIt Units Qual Limit CAS ti Date By Nlokel, Ni < 6.60 ug 6.60 7440-02-0 31212012 kfoltzOur Lab # 12001772-006 Your Sanrple ID: Run 2 Nitric Probe

Your Project # 141.11-210N Collection Date: 02/02/12 Your Project Name: GenernlShale Collected By: Client Sample Type: Liquid Beceipt Date: 02/02/12 12,00

Antimony, ICP-AES Analvtical Method Preu Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz

- Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb < 22.0 ug 22.0 7440-36-0 3/2/2012 kfoltz

Beryllium,lCP-AES Analvtical Method Prep Method Pren Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS# Date By Beryllium, Be < 0.880 ug 0.880 7440-41-7 3/212012 kfoltz

Arsen'rc, ICP-AES Analyticai Method Prep Method Prep Date 11 ~ SW846 6010B SW846 3010A 2/21/2012 kfoltz
Quant, Analysis Parameter Result Units Qual Lirnit
-...._.__..-- CAS # Date By

-- Arsenic, As ---- --- < 2.20 ug 2.20 7440-38-2 3l2/2012 kfoltz

Selenium, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Selenium,Se <2.20 ug 2.20 7782-49-2 3/2/2012 kfoltz

Cobalt, ICP-AES Analvtical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS# Date By
Cobalt, Co < 4.40 ug 4.40 7440-48-4 3/212012 kfoltz

Cadmium, ICP-AES Anaivtical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS# Date By
Cadmium, Cd ME < 2.20 ug 2.20 7440-43-9 3/2/2012 kfoltz

Lab # 12001772-006 Sample ID: Run 2 Nftric Probe Page 11 of 30 

# ESG Laboratories

5927 W EST 71 ST STREET PHONE (317) 290•1471 INDIANAPOLIS, INDIANA 46278 FAX (317) 290-1670Lab # 12001772-006 Sample ID: Rua 2 Nitric Probe 

# ESG Laboratories

5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA 46278 PNONE (317) 290-1471 FAX (317) 290-1670 Page 12 of30 Chromium, ICP-AES Analvtical Method Prep Method Preu Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result IInits Qual Limit CAS # Date By
Chromium, CI - -------_— --_- <4.40 - ug --^
~_~— 4.40 7440•47-3 3/2/2012 kfoltz

Manganese, ICP-AES Analvtical Method Prep Method Pren Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn T < 120 ug 2.20 7439-96-5 3/212012 ktoltz

Nickel, ICP-AES Analvtical Method Pren Method Prea Date Bv , SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Nickel, Ni <4.40 ug 4.40 7440-02-0 3/2/2012 kfo@zOur Lab k 12001.772-009 Your Sample ID: Run 2 Nitric C5A

Yaur Projeet tl 141.11-210N Collection Date: 02/02/12 YourProjectName: GeneralShale Colleeted By: Client Sample Type: Liquid Reeeipt Date: 02/02/12 12:00

Antimony, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A. 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Q ual Limit CAS # Da te By Antimony, Sb m < 12.0 ug 12.0 7440-36-0 3/2/2012 kfoltz

Beryllium, ICP-AES Analytical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/21l2012 kfoltz Quant. Analysis Parameter Result Units Quai Limit CAS # Da te By Beryllium,Be <0.480 ug 0.480 7440-41-7 3/2/2012 kfoltz

Arsenic, ICP-ABS Analytical Method Preu Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Arsenic, As < 1.20 ug 1.20 7440-38-2 3/2/2012 kfoftz

Seleninm, ICP-AES Analvtical Method Prep Method Prep Date 

### Ey SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter R es ul t Uni ts Qual Limit C AS # Da te By Selenium, Se J < 1.20 ug 1.20 7782-49-2 31212012 kfoltz

Cobalt, ICP-AES Analvtical Method Preo Metltod PreD Date 

### EY SW8466010B SW8463010A 2/21/2012 kfoltz

- Quant. Analysis Par a meter Result Units Qual Limit CAS # Date By Cobalt, Co < 2.40 ug 2.40 7440-48-4 3/2/2012 kfoltz

Cadmium, ICP-AES Analvtical Method Prep Method Pren Date 

### 1!1 SW8466010B SW8463610A 2/21/2012 kfoltz

# I
g . r ~ ~ L Chromium, ICP-AES Analytical Methud Prep_Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz ~ Quant. a~
. Analysis Parameter Result Units Qual Limit CAS i# Date By
Chromium, Cr < 2.40 ug 2.40 7440-473 312/2012 kfoltz

Manganese, ICP-AES Analytical Method Preo NIethod Prep Date py SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn < 1,20 ug 1.20 7439-96-5 3/212012 kfoltz

Nickel, ICP-AES Analytical Method Prep 111ethod Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Nickel, Ni < 2.40 ug 2.40 7440 02-0 3/2/2012 kfoltz

Lab # 12001772-009

. 

# ESG LaboratoriPs

5927 WEST 71ST STREET INDIANAPOLIS, INDIANA 46278 Sampie ID: Run 2 Nitric C5A Page 18 oJ30

PHONE (317) 290-1471 

# ~ ,! !: FAX (317) 290-1670Our Lab # 12001772-004 Your Sample ID: Run 3 Nilrio C4A

YourProjeot# 141.11-210N Coileetion Date: 02102112 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

Antimotty, ICP-AES Analytical Method Prep Method Prep Date By - SW846 6010B SW846 3010A 2/21/20I2 kfoltz Quant. - Analysis Parameter Result Units Qual Limit CAS #

. Date By Antimony, Sb < 32.7 ug 32.7 7440-36-0 312I2012 kfoltz

Beryllium, ICP-AES Analvtical Method Prep Method Prep Date Bl; SW8466010B SW8463010A 20-1/2012 kfoltz

Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Beryllium, Be < 1.31 ug 1.31 7440-41-7 312/2012 kfoltz

Arsenic, ICP-AES Analytical Method Prep Method Prep Date BX SW8466010B SW8463010A 2/21/2012 kfoltz QuanL Analysis Parameter Result Units Qual Limit CAS # Date By

____._--- ------------- Arsenic, As < 3.27 ug $.27 7440-38-2 312/2012 kfoltz

Selenium, ICP-AES Anal tic

~ al

~ Method Prep Method Prep Date By SW8466010B SW84630t0A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units

.-_._.--- ----'--"-'-- Qual Limit CAS #
-------- -____ Date By
Selenium, Se < 3.27 ug 3.27 7782-49-2 3/2/2012 kfoltz

Cobalt, ICP-AES Analvtical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz

. Quant. Analys' rs Parameter Result Units Qaal Limit CAS # Date By
Cobalt, Co

. < 6.54 ug 6.54 7440-48-4. 3/2/2012 kfoltz

Cadmitun, ICP-AES Analytical Method Prep Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cadmium, Cd .< 3.27 ug 3.27 ^ 7440-43-9 312/2012 kfoltz

Lab # 12001772-004 Sample ID: Run 3 Nitrlc C4A Page 7 of30 

# ESG Laboratories

5927 WEST7IST STREET PHONE (317) 290-1471 INOIANAPOLIS, INDIANA46278 FAX (317) 290-1670Lab #! 12001772-004 Sample ID: Run 3 Nitdc C4A 

# ESG Laboratories
5927 WEST 71 ST STREET INDIANAPOLIS, INDIANA46276 - PHONE (317) 290-1471 FAX (317) 290-1670 Page 8 of 30 Chromium, ICP-AES Analvtical Method Prep Method Prep Date iiy SW8466010B SW8463010A 2/21/2012 kfoltz

, Quant. Analysis Parameter Result Units Qua l Limit CAS # Da t e By Chromium, Cr < 6.54 ug 6.54 7440-47-3 3/212012 kfoltz

Manganese, ICP-AES Analgtical Method Prep Method Pren Date ,By SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Q ual Limit CAS # Date By Manganese, Mn W 5.59 ug 3.27 7439-96-5 312/2012 kfolk

Nickel, ICP-A&S Analvtical Method Prep Method Prep Date By

. SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Nickel, Ni < 6.54 ug 6.54 7440-02.0 3/2/2012 kfoitzOur Lab # 12001772-007 Your Sample ID: Run 3 Nitric Probe

YourProject# 141.11-2I0N Collection Date: 02/02112 Your Project Name; GeneralShaie Collected By: Client SampleType: Liquid Reccipt Date: 02/02/12 12:00

Antimony, ICP-AES Analytical Method Prep Method Prep Date 11 ~ SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS# Date By Antimony, Sb < 34.5 ug 34.5 W 7440-36-0 312/2012 kfoltz

Beryllium, ICP-AES Analytical Method Preu Method Prep Date Il ~ SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Beryllium, Be 

### magemmmmmgm < 138 ug 1.38 7440-41-7 312/2012 kfaltz

Arsenic, ICP-AES Analytical Method Prep Method Preu Date By SW8466010B SW8463010A 2/21/2012 kfoltz

Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Arsenic,As <3.45 ug 3.45 7440-38-2 312/2012 kfoltz

Selenium, 1CP-AES Analvtieal Method Preo Method Prep Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Selenium, Se < 3.45 ug 3.45 7782-49-2 312/2012 kfoltz

Cobalt, ICP-AES Analvtical Method Preu Method Prep Datc 1l ~ SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cobalt, Co < 6'.90 ug 6.90 7440-48-4 3/212012 kfoltz

Cadmium, ICP-AES Analvtical Method Prerp Method Prep Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz

, Quant. Analysis Parameter Result Units Qual L imit CAS # Date By
Cadmium, Cd < 3,45, ug 3.45 7440-43-9 3/2/2012 kfoltz

Lab # 12001772-007 Sample ID: Run 3 Nitric Probe Page 13 af30 

# ESG Laboratories

5927 W EST 71 ST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46278 FAX (317) 290-1670I t 

### ~

~ Chromium, ICP-AES Analytical Method Prep Method Prep Date By 

# ~ SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter ' Result Units Qual 

# Li mit CAS # Date By 

# ~ Chromium, Cr < 6.90 ug 6.90 7440-47-3 3/2/2012 kfoltz L 

# r Manganese, ICP-AES Analvtical Method Prep Method Prep Date Ily SW846 6010B SW846 3010A 2/21/2012 kfoltz 

# ~
Quant. Analysis 

### ~ Parameter Result Units ._._ _ _ _. Qnal Limit # , _CAS Date By_ Manganese,Mn <3.45 ug 3.45 7439-96-5 302012 kfoltz

Nickel, ICP-AES Analvtical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Nickel, Ni < 6.90 ug 6.90 7440-02-0 3/2/2012 kfo{tz

Lab # 1 2001 7 72-007 Sample ID: Run 3 Nitric Probe Page 14 oj30 

# ESG Laboratories
5927 WEST 71ST STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46278 FAX (317) 290-1670Our Lab # 12001772-010 Your Sample ID: Run 3 Nitrio C5A

Your Praject # 141.11-210N Collectiou Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Pate: 02/02/12 12:00

Antimony, ICP-AES Analytical Method Prep Method Prep Date Ily SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb < 13.0 ug 13.0 7440-36-0 3/212012 kfoltz

Beryllium, ICP-AES Analdtical Method Prep Method Pren Date By, SW846 6010B SW846 3010A 2/21/2012 kPoftz Quant. Analysis Parameter Result Units Qual Limit CAS# Date By Beryllium, Be < 0.520 ug 0.520 7440-41-7 3/2/2012 kfoltz

Arsenic, ICP-AES AnalvtYcal Method Prep Method Prep Date By SW346601oB - SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Arsenic, As

~ fawam < 1.30 ug 1.30 7440-38-2 3/2/2012 kfoltz

Selenium, ICP-AES Analvtical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2121/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Selenium, Se

. < 1.30 ug 1.30 7782-49-2 3/2/2012 kfoltz

Cobalt, ICP-AES Analytical Method Pren Method Prep Date By SW846601EB SW8463010A 2/21/2012 kfoltz

. Quant. Analysis Parameter Result Units Qual Limit CAS # Date By
Cobalt, Co < 2.60 ug 2.60 744048-4 312/2012 kfoltz

Cadmium, ICP-AES Analvtical Method Preo Method Pr

..
_ - ,ep Date By SW8466070B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Resutt Units Qual Limit CAS # Date By
Cadmium, Cd < 1.30 ug 1.30 7440-43-9 3/212012 kfoltz

Lab # 12001772-010 Sample ID: Rnn 3 Nitric CSA Page 19 of 30 

# ESG Laboratories

5927 WEST7ISTSTREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA 46278 FAX ($17) 290-1670Lab # 12001772-010 Sample IDa Run 3 NitriC C5A 

# ESG Laboratories

5927 W EST 71 ST STREEI' INDIANAPOLIS, INDIANA46276 PHONE (317) 290-1471 FAX (317) 290-1670 Pnge 20 of 30 Chromiun , ICP-AES Analvtical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/2112012 

### kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Chmmium, Cr < 2.60 ug 2,60 7440-47-3 31212012 kfoltz

Manganese, ICP-AES Analytical Method Prep Method Prep Date BI SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn

. < 1.30 ug 1.30 7439-96-5 3/212012 kfoltz

Nickel, ICP-AES Analvtical Method Prep Mefhod Prep Date B}y SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Nickel, Ni < 2.60 ug 2.60 7440-02-0 3/2/2012 T kfoltzOur Lab # 12001772-013 Your Sample ID: Run 3 Nitric C5C

YourProject# 141.11-210N Collection Date: 02/02/12 Your Project Name: General Shale Collected By: Client Sample Type: Liquid Receipt Date: 02/02/12 12:00

Antimony, TCP-AES Analvtical Method Prep Method Prep Date By SW84660IOB SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb < 33.0 ug 33.0 7440-36-0 312/2012 kfoltz

Beryllium, ICP-AES Analytical Method Prep Method Prep Date Rv SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Beryllium, Be < 1.32 ug 1.32 7440-41-7 31212012 kfoltz

Arsenic, ICP-AES Analvtical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz

, Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Arsenic, As .< 3.30 ug 3.30 7440-38-2 3/2/2012 kfoltz

Selenium, ICP-AES Analytical Methad Prep Method Prep Date 

### Ey SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Selenium, Se 46.0 ug 3.30 7782-49-2 3/212012 kfoltz

Cobalt, ICP-AES Analytical Method Prep iVlethod Pren Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Cobalt, Co < 6.60 ug 6.60 7440-4B-4 3/2/2012 kfoltz

Cadmium, ICP-AES Analytical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 kfoltz

. Quant. Analysis Parameter Result Units Qual Limit CAS # Date By

. Cadmium, Cd < 3.30 ug ,3.30 7440-43-9 312/2012 kfoltz

Lah # 12001772-013 Sample 1D: Run 3 Nitric C5C Puge 25 of30 

# ESG Laboratories

5927 WEST 715T STREET PHONE (317) 290-1471 INDIANAPOLIS, INDIANA46278 FAX (317) 290-1670Chromium, ICP-AES Analvtical Method Prep Method Prep Date 13 1 SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qaal Limit CAS # Date By
Chromium,Cr <6.fi0 ug 6.60 744047-3 3/212012 kfoltz

Manganese, ICP-AHS Analvtical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/20I2 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By

00 ug 330 0 

### nti.A~+wF i

.......... ........... 4 ri..

. u,M1.Ek.~~.vA, .„,42 ,mM,r •dr. ~~ x,Y. e, ., ~i s- ~-- ~','^~ PrepMethod prep . 61 1' SW846 3 01 1 • 2/21/2012 kfoltz

•
. Qual Limit CAS # 1.

li'n ~`+ .H_ 0 ug 6.60 0 • • 0 3l-i~ Y5d94.~.y

Lab # 12001772-013 Sample ID: Run 3 Nitric C5C 

# ESG Laboratories

5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 Page 26 af 30

PHONE (317) 290-1471 FAX (317) 290-1670Our Lab # 12001772-015 Your Sample ID: Rum 3 Nitric C4B

Your Pruject k 141.11-210N Collection Date: 02/02/12 : Your Project Name: General Sbale Coilected By: Client SampleType: Liquid ReceiptDate: 02/02/12 12:00

Antimony, ICP-AES Analytical Method Prep Method Prep Date By SW846 6010B SW846 3010A 2/21/2012 lcfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Antimony, Sb `< 11.5 ug 11.5 7440-36-0 3/212012 kfoltz

Beryllium, ICP-AES Analvtical Method Prep Method Prep Date Il ~ SW846 6010B SW846 3010A 2/2l/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Beryllium, Be <0.460 ug 0,460 7440-41-7 ........._._._— 3/2/2012 kfoltz

Arsenic, ICP-AES Analytical Method Prep Method Prep Date B SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Arsenic, As < 1.15 ug m 1.15 7440-38-2 312l2012 kfoltz

Selenium, ICP-AES Analvtical Method Prep Method Pr

~ Date Bv SW846 6010B SW846 3010A 2/21/2012 kfoltz Quant.

. Analysis Parameter Result Units Qua1 Limit CAS # Date By Selenlum, Se < 1.15 ug 1.15 7782-49-2 312I2012 kfoltz

Cobalt, ICP-AES Analvtical Method Prep Method Pren Date B SW8466010B SW8463010A 2/21/2012 kfoltz Quant.

. Analysis Parameter Result Units Qual Limit CAS # Date By Cobait, Co < 2.30 ug 2.30 7440-48-4 3/2/2012 kfoltz

Cadmium, ICP-AES Analytical Method Prep Method Prep Date Bv SW846 6010B SW846 3010A 2/21/2012 kfoltz

. Quant. Analysis Parameter Resutt Units Qua1 Limit CAS# Date By Cadrrlium, Cd < 1.15 ug 1.15 7440-43-9 3/212012 kfoltz

Lab # 12001772-015 Sample ID: Rum 3 Nitric C4B

. Page 29 of30 

# ESG Laboratories

5927 WEST71ST STFEET PHONE (317) 290-1471 INDIANAPOLIS, IN L11ANA 46278 FAX (317) 290- 1670Lab # 1 2001 772-0 1 5 Sample ID: Rum 3 Nitric C4B 

# ESG Laboratories
5927 W EST 71 ST STREET INDIANAPOLIS, INDIANA46278 PHONE (317) 290-1471 FAX (317) 290-1670 I Pnge 30 of30 Cluomium, ICP-AES Analvtical Method Prep Method Preo Date By SW8466010B SW8463010A 2/21/2012 kfoltz Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Chromium, Cr < 2.30 ug 2.30 7440-47-3 3/212012 kfoltz

Manganese, ICP-AES Analvtical Method Prep Method Prep Date Bv SW8466010B SW8463010A 2/2I/2012 kfoltz

Quant. Analysis Parameter Result Units Qual Limit CAS # Date By Manganese, Mn < 1.15 ug 1.15 7439-96-5 312/2012 kfoltz

. . Method 1 •' SW846 3010A 1 kfoltz

, Q Limit CAS N 1

• ug 230 •• • • •

3/2/2012 Lab Manager Date

### General Shale Brick, Inc Proj ect Number: 141.11



## APPENDIX VI

SUBMITTED PROTOCOL

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### General Shale Brick, Inc Project Number: 141.11



## APPENDIX VII

PROD UCTION DATA

Wilcox Environmental Engineering, Inc. Air Analysis DivisionIU blMfl OI ! IciL 5737 t4,

~ 9 740 Sueel
I htitlolis.lNVt228 

# WI L,COX .

GNVIRONMENTAL ENGINEERING

General Shale Brick: ICR stack testing

Production Data: 19.5 tons/hr
Date: 2/1/12 phnee319.472.tl999
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