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 

COZ 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 

O2 Oxygen (dry volume %) 17.3 17.3 17.3 17.3 

COz 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)(PY,) 

Where: 

Vi, 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~XPma' a" XYa) j

.O

e 

(4 60 

23.L 

+7 ) 

Where: 

Py„, barometric pressure (in Hg) 

Tm 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') 

Yd gas meter correction factor (dimensionless) 

DH average pressure drop across meter box orifice (in IizO) 

17.64 conversion factor (°R/in Hg) 

13.6 conversion Factor (in Hz0/irt FIg) 

460 °Fto °Rconversionconstant 

3. Samplc gas pressure (in Hg) 

pf P P 

t

136 ) 

VJhere: 

i'y,,, - barometric pressure (in Hg) 

Ps sample gas static pressure (in H ~O) 

P, absolute sample gas pressure (in HZO) 

13.6 conversion factor (in H zO/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, 

Ps 

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) 

CO2 proportion of carbon dioxide in the gas stream by volume (%) 

0= proport'roa of oxygen in the gas stream by volume (%) 

CO +N2 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,x17.64x1—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 

Vm„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 r ) u

V,a Volume Standard conditions 

2.2046e-9 conversion factor, pounds per microgram 

60 conversion factor, minutes per hour 
VIA - 

Figore 26&~1^ Saopliog %raio 
1527 

'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 

0 ~ O 

6 A 

—J E m~ 

W 

m 

Z 4 

= a 

— _—J n ` w o m ~ C7 d 

=J En 

do a1 0 

d ~ v _ 

` No N m ~ 

V

N 

, W 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 Division 
STACK 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 53.708 
COMPANY 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 toi 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 

3 I Cal 1.049 ].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 

anaaat = 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 O66 
PoIIWnlMassEmisslonRale,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 abaaar = 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 6,821 

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 0 
31ack 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 

qama 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' ~6SuareDelpP ~ '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 86 
PalluhnlMass 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 0 
COMPANVNAME: 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 

pa 

PEnnUea Hpl 29500 

mma ? a2 B 

Vmisltll 58442 

Molelme CSnlent cl9tack Gas Bwo 

Bwo 141 10 

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 0.176 

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 94 

HNOyH2 

H2GOdIKm 

Total U 366 1.94 

UG 1 8591 5323 
PollursntMessEmisslonftar6 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 51.684 
FIELOOATA 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]4 100.7386 
COMPANY 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 1.2762 
COMPANY 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 LID 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 00 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 Division 
10 

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" 
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General Shale Brick, Inc 

Project Number: 141.11 

APPENDIX IV 

CALIBRATIoN DATA 

Wilcox Environmental Engineering, Inc. 

Air Analysis Division 
CP InxATIGn6HECn 

IPaeITeaIIPer EMTIGGUItltllnaG0 ~ 26 

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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 

1/8tn" 

W cm 0.0 

W is less than 0.08cm 

1/32ndn 

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 DateJanuary 7th , 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 

1/8th, 

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 74th Street 

Indianapolis, IN 46278 

General Shale 

Client # 141.11 

Analytical Report 

(0212-68) 

EPA Method 2" (NaOH Matrir) 

Chloride 

EPA Method 2" (H2SO4 Matrix) 

Hydrogen chloride, Hydrogen fluoride 

Enthalpy Analytical, Inc. 

Phone: (919) 850 - 4392 / Fax: (919) 850 - 9012 / www.enthalpy.com m 800-1 Capitola Drive Durham, NC 27713-4385 
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 MOU 

EA# 0212-68 Page 2 of 122 
Summary of Results 

F' 

7~OA 

EA# 0212-68 Page 3 of 122 
Company 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 122 
Company 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 

Y)0~1- 

EA# 0212-68 Page 6 of 122 
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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 H2SO4 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' 157ArOdAd 

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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Sample 

Chromatograms 

~ 

EA# 0212-68 Page 23 of 122 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 

30 o ~

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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\MRBURNS\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 

~.~_~_ i —~i..... S.,_ .._....— —._.._— ......... ,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 1 
Data 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\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MRBURNS\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:\HPLC2012Q1\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 

2 3 4 5 6 r . 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBIIRNS\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\MRBURNS\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 1 
Data 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 

70 J 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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\MRBURNS\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 1 
Data 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 1 
Data 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,—~rTn 

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MR13URNS\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\MRBURNS\DATA\PEB\HPLC67PG006\060-4301.D) 

uS/cm 

90 

80 . 

70 

60 I 

a 

I 

50 d ~ 

40 LL~ 2

 ~o 

30 V a L I~ 

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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\MRBURNS\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 1 
Data 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\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 

c6 U 

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 i 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 il \ 

.

. 

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 2 
Data 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 ! II 

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 2 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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\MRBURNS \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 2 
Data 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 

FUSIcm 

 _ 90 4 ° 

80 . 

~ 701 ~ ~I 

60 i 

50 li 

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 2 
Data File H:\HPLC2012Q1\MRBURNS\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 

I1 

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

3.047 MM 339.93423 1.52129e-2 5.17139 Fluoride Manua[Int."II"(EDEI 

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- 

0 v 

60 '.. 

JJJ 

50 -~ ~ rn g I 

40 1 

] 

n 

4 

t 

U I I 

30 

~ 

N 

20 

N N 

10 ~ r 

0 - -. --- Tr 

, 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 1 
Data Fi1e H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 ~ 

il 80 , I 1 ~ 

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 1 
Data 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\MRBURNS\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 

~ m 6 i 

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 1 
Data 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 .- 

00 ~ 

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 1 
Data 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 1 
Data 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 80 I 

70 

I I 

60 

m 

50 

L ~ 40 U I 

N 30 - 

20 

1 10^]{ 

O 

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 

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 1 
Data 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 1 
Data 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 

Mj 

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 1 
Data 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 

" 

FUS/cz 

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 ~ ._ rJ _ . ~ ~ _:.: _ 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 cx 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 1 
Data 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 1 
Data 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 

rusic: 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 1 
Data 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\MRBURNS\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 00y tLj bq°'~ I \ 20 ~ ,h°' ~ ~M 

..._..._.._.__'. 

10 

n ~ , 

~~

e 

,. 2 .,.,N 

0 ~- T-6~~ 8-" 

- 

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 

li 

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 2 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 

~ 

il ~ 

60 

50 - 

ii 

i 

, Ii 

40 ~ 

30- 

~ 20 

~ i 

10 N 

._.. .-..-- .._.. 

0 .- .-_----- —r r-_ 

2 3 4 5 6 r 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 2 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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~ i A 

' 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 2 
Data 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 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, 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 2 
Data 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 

~ a v III 

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 1 
Data 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\MRBURNS\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 1 
Data 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 1 
Data 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\MRBURNS\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 \ 

,.~. , . ~ ✓ ...._ T .... __.~-_.. ~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------------------ 

3.963 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 122 
Method 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 2 
Method 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"J1I 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 

 _Amountfug/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 2 
Data 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 ~he 

o 

U 

{1 

20 

ry 

~ ^ 

ea o ea. 

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 

20 ~ra ' 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 II 

70 

II 

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 1 
Data 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;nnalT.,fn -peak(S) manuallvintearate d 

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

uS/cm μ 

90 - 

~ 

° 

80 - 

70 -_ II ~ 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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\MRBURNS\DATA\FEB\HPLC67PG006\102-6601.D) 

us/cm ~s ~ 

90 - 

80 

j °} I 

~ 

70 

60 l 

i 

50 

40 - 

~ 

a m 

30 20 , 

L0 M O h N M 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 

60 4 

50 

40 O o I 

~ 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 

50 LL ~ 

O L 

40 oi U i 

30 ~ °o 

v li 

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 

0.— ~/— ~. —~/__ .~—.— .~~+ — 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 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 1 
Data 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 

I 0 ..2_ . 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 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 1 
Data 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 ^ 

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

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 1 
Dflta 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 li i a 0 

40 

30 

20 

10 

r 

0~.....~~T. 4~T-~T 6 7 r 8 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, 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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\MRBURNS\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 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/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 1 
Data 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 - 

60 ~ v ~ I ~ 

56 I ON li a ~il 40 - 

j 

30 

I 

20 i I i 6 

10 

\ J ... ~ ~.~_..._ , ~ T ..—...~. 

4 !O-_,a ~ n\,_ 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 1 
Data 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 i 
Data 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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~ ........ l. .~,..... 

I I 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 1 
Data 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 

~I ~p I III 60 ~ 

50 

40' 

i 

30 

29 r 

A ~ 

\ 

r 

i ~ 

f 

_ ~~ 

- 

10 

3 4 5 6 7 8 9 mi-m 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 1 
Data 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\MRBURNS\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 III 

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 1 
Data 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 ~ ~.L ~~ 

 6 

.__ ~~~m r._ - ~ ~M - , _ n -~ - - ~

._ _ _ - 

i 0 .-Tr-'---r_..,-~r. '--'~r-'~^-. 

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\DATA\FEB\HPLC67PG006\106-5801.D) 

uS/cm 

901 

~ 

I ° 

I 

80 

j 

I 

70 ~ 

60 ~ ~ 50 

40 

~ 

9 

m 

o ii 

30 - 

`o p 

ui 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 1 
Data 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MRBURNS\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\MRBURNS\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 ~ 

BO = 

LL 

~i 

~ 

70 

M t 

v 

I 60 

v i 

40 ii 

? 

30 I 

I ~ I N n I 

i 20 lD n I I 

I

0 

...

6 9 ~Tmin 

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 1 
Data 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\MRBURNS\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 , v d I , 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 1 
Method 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 

Amount(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 2 
Method 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 2 
Data File H:\HPLC2012Q1\MRBURNS\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 intearated 

ADCIA,ADC1 CHANNELA(H:\HPLC2012Q1\MR BURNS\DATA\FEB\HPLC67PG008\HPLC67PG0082\001-0201.D) 

us/cm 

90 

I 

80 ~ 

70 

60 f 

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 1 
Data 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 °Pea 

. .... ,.,._... 

..___ 

..-. I 0 ._.,.-, ~T._~ . 

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 1 
Data File H:\HPLC2012Q1\MREURNS\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

di ~ 90 

80 i 

70 

60 

50 ~ 

40 ~ 

- m 0 

30 

20 L I 

10 J a'Q~° ... °Pe ...... 

, 

..... ..... ~L..... 

0 --T -------- 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 1 
Data 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 34 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 1 
Data 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 

50 I 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 1 
Data 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 1 
Data 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 

I 6 

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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 1 
Data 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 

li 

50 a ° i i 

401 

`o 

U 

v I 30 

20 ~] m 

10 ~ ~ u' 

~~ 

m 

~ 

(° 

._...___, ~ ~ ~_ _ .✓ " _ J ~ - .~ 

I 0 3 _._ 4 ~— 5 6 \ - r 7 8 9~rmi 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 1 
Data 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 

~ III 70 I ' i 

60 ~ 

50 a ' I 

40 

o 

U il 

30, 

N 

~ 20 

M O V 

~ 10 

- 

i ,n m 

_. .:.. ,~ _ .... ~.~ ~ . .... . 

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 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 1 
Data 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 1 
Data 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 ; 

Ili 

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 1 
Data 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 m V 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 1 
Data 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 

I 

~ o 0 

i 

40 

. 3020.. ~ O N 

10 r 

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] [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 1 
Data 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 ~ 

Ii 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 1 
Data File H:\HPLC2012Q1\MRBURNS\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 1 
Data 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 1 
Data 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 li 

I 

70 , 

I ~I 

60 li 

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 1 
method: C:\HPLC2011Q1\MRBURNS\METHODS\METROHM.M 

Modified on: 4/1/2010 at 4:15:36 PM 

Method Information 

Method: C:\HPLC2011Q1\MRBURNS\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 122 
YourProject# 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 DateBy 

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) 290-1670 
Our 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 DateBv 

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 DateDy, 

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 DateBy 

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 DateBv 

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•1670 
Our 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 DateBv 

Method 29 Method 29 2/8/2012 ]mcleary 

• 

Qual Limit CAS t• 

0 . 180 r 

xc- As..y-a,as.,.>"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 DateBv 

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) 290-1670 
Our 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) 290-1670 
Our 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 DateBy 

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) 290-1670 
OurLab# 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 DateBv 

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: 

o R 

6 6 

z 

zzz;zzzz ......... 

ro 

O 

Z~b 

O 

IE 

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PA 
7E 

O 

O 

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O 

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ff 

Cl d 

D 0 

p 41 

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 Lirnit 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) 290-1670 
Cobalt, 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 oJj 30 

PHONE (317) 290-1471 

FAX (317) 290-1670 
Our 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 Limit CAS # Date 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) 290-1670 
Lab # 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~ . SG. 'K'~~ ~ r tim ~.tt, . ~5:. t,uf4a`^,'M1 

3.60 

d t~4 

x ~. .,,.'2mu ~d~ s ?8a,~':+ ~ .-? 

440 0 0 

' - I~-, ~k 

,, ; .,.M,k 

0 
Our 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 kfoltz ^T 

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 By 
Lab 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 kfoltz 

Q , 

Nm3 ~~tw~% uin l~a~ 4h,-,. '~.°-7 jul"

, 

40 ug 3A0 440 0 0 0 
Our 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 ty 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) 290-1670 
Lab # 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 kfoltz 
Our 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) 290-1670 
Lab # 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 33.0 T 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 kfoltz T 

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 By 
Lab 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 

SW846 61 1' SW846 3010A 2/21/2012 kfoltz 

Q , u 

„c..Ke.: s".rw ;! Hoffi.p 

60 ug 6.60 0 Q 

b$.~ ..t 

0 

 .2.m ~ -- . ,-n 
Our 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 QoalLimit CAS# 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 Result Units QualLimit 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 Result Units Qual 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. 

Qual Limit 

Prep Date 

2/21/2012 

CAS # 

B 

kfoltz 

Analysis 

Date 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 Qual Limit 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 # Date By 
Lab # 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 kfoltz 
Our 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) 290-1670 
Lab 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 kfoltz 
Our 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) 290-1670 
Lab # 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 < 120 ug T 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@z 
Our 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 QualLimit CAS # Date 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 # Date 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 Result Units Qual Limit CAS # 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 

Parameter Result Units QualLimit 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) 290-1670 
Our 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) 290-1670 
Lab #! 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 Qual Limit CAS # Date 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 QualLimit 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 kfoitz 
Our 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 W7440-36-0 312/2012 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) 290-1670 
I 

t 

~ 

~ 

Chromium, 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 ~ 

Chromium, Cr < 6.90 ug 6.90 7440-47-3 3/2/2012 kfoltz L 

Manganese, ICP-AES Analvtical Method Prep Method Prep Date Ily r 

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) 290-1670 
Our 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) 290-1670 
Lab # 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 kfoltz 
Our 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) 290-1670 
Chromium, ICP-AES Analvtical Method Prep Method Prep Date 131 

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) 290-1670 
Our 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- 1670 
Lab # 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 

Wilcox Enviromnental Engineering, Inc. 

Air Analysis Division 
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General Shale Brick, Inc 

Project Number: 141.11 

APPENDIX VII 

PROD UCTION DATA 

Wilcox Environmental Engineering, Inc. 

Air Analysis Division 
IU 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 

l~ li AI>.15' 0993 

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