grays harbor energy, llc 401 keys road

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October 12, 2015 Analytical Report for Service Request No: K1509368 Peter Valinske Grays Harbor Energy, LLC 401 Keys Road Elma, WA 98541 Analyses were performed according to our laboratory’s NELAP-approved quality assurance program. The test results meet requirements of the current NELAP standards, where applicable, and except as noted in the laboratory case narrative provided. For a specific list of NELAP-accredited analytes, refer to the certifications section at www.alsglobal.com. All results are intended to be considered in their entirety, and ALS Group USA Corp. dba ALS Environmental (ALS) is not responsible for use of less than the complete report. Results apply only to the items submitted to the laboratory for analysis and individual items (samples) analyzed, as listed in the report. For your reference, these analyses have been assigned our service request number Enclosed are the results of the sample(s) submitted to our laboratory August 26, 2015 RE: GHEC NPDES Dear Peter, K1509368. Please contact me if you have any questions. My extension is 3275. You may also contact me via email at [email protected]. Respectfully submitted, ALS Group USA, Corp. dba ALS Environmental Chris Leaf Project Manager ALS Group USA, Corp 1317 South 13th Avenue Kelso, WA 98626 +1 360 577 7222 +1 360 636 1068 T : F : ALS Environmental www.alsglobal.com RIGHT SOLUTIONS | RIGHT PARTNER for Page 1 of 196

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Page 1: Grays Harbor Energy, LLC 401 Keys Road

October 12, 2015 Analytical Report for Service Request No: K1509368

Peter ValinskeGrays Harbor Energy, LLC401 Keys RoadElma, WA 98541

Analyses were performed according to our laboratory’s NELAP-approved quality assurance program. The test results meet requirements of the current NELAP standards, where applicable, and except as noted in the laboratory case narrative provided. For a specific list of NELAP-accredited analytes, refer to the certifications section at www.alsglobal.com. All results are intended to be considered in their entirety, and ALS Group USA Corp. dba ALS Environmental (ALS) is not responsible for use of less than the complete report. Results apply only to the items submitted to the laboratory for analysis and individual items (samples) analyzed, as listed in the report.

For your reference, these analyses have been assigned our service request numberEnclosed are the results of the sample(s) submitted to our laboratory August 26, 2015

RE: GHEC NPDES

Dear Peter,

K1509368.

Please contact me if you have any questions. My extension is 3275. You may also contact me via email at [email protected].

Respectfully submitted,

ALS Group USA, Corp. dba ALS Environmental

Chris LeafProject Manager

ALS Group USA, Corp1317 South 13th AvenueKelso, WA 98626

+1 360 577 7222+1 360 636 1068

T :F :

ALS Environmental

www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

for

Page 1 of 196

Gregory.Salata
Salata signature
Page 2: Grays Harbor Energy, LLC 401 Keys Road

www.alsglobal.com

ALS Environmental

F :T :

+1 360 636 1068+1 360 577 7222

Kelso, WA 986261317 South 13th AvenueALS Group USA, Corp

Table of Contents

RIGHT SOLUTIONS | RIGHT PARTNER

Acronyms

Qualifiers

State Certifications, Accreditations, And Licenses

Case Narrative

Chain of Custody

General Chemistry

Metals

Organochlorine Pesticides and Polychlorinated Biphenyls

Volatile Organic Compounds

Semi-Volatile Organic Compounds by GCMS

Subcontract Lab Results

Page 2 of 196

Page 3: Grays Harbor Energy, LLC 401 Keys Road

ASTM American Society for Testing and Materials

A2LA American Association for Laboratory Accreditation

CARB California Air Resources Board

CAS Number Chemical Abstract Service registry Number

CFC Chlorofluorocarbon

CFU Colony-Forming Unit

DEC Department of Environmental Conservation

DEQ Department of Environmental Quality

DHS Department of Health Services

DOE Department of Ecology

DOH Department of Health

EPA U. S. Environmental Protection Agency

ELAP Environmental Laboratory Accreditation Program

GC Gas Chromatography

GC/MS Gas Chromatography/Mass Spectrometry

LOD Limit of Detection

LOQ Limit of Quantitation

LUFT Leaking Underground Fuel Tank

M ModifiedMCL Maximum Contaminant Level is the highest permissible concentration of a substance

allowed in drinking water as established by the USEPA.

MDL Method Detection Limit

MPN Most Probable Number

MRL Method Reporting Limit

NA Not Applicable

NC Not Calculated

NCASI National Council of the Paper Industry for Air and Stream Improvement

ND Not Detected

NIOSH National Institute for Occupational Safety and Health

PQL Practical Quantitation Limit

RCRA Resource Conservation and Recovery Act

SIM Selected Ion Monitoring

TPH Total Petroleum Hydrocarbonstr Trace level is the concentration of an analyte that is less than the PQL but greater than or

equal to the MDL.

Acronyms

Page 3 of 196

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Inorganic Data Qualifiers

* The result is an outlier. See case narrative.

# The control limit criteria is not applicable. See case narrative.

B The analyte was found in the associated method blank at a level that is significant relative to the sample result as defined by the DOD or NELAC standards.

E The result is an estimate amount because the value exceeded the instrument calibration range.

J The result is an estimated value.

U The analyte was analyzed for, but was not detected ("Non-detect") at or above the MRL/MDL. DOD-QSM 4.2 definition : Analyte was not detected and is reported as less than the LOD or as defined by the project. The detection limit is adjusted for dilution.

i The MRL/MDL or LOQ/LOD is elevated due to a matrix interference.

X See case narrative.

Q See case narrative. One or more quality control criteria was outside the limits.

H The holding time for this test is immediately following sample collection. The samples were analyzed as soon as possible afterreceipt by the laboratory.

Metals Data Qualifiers

# The control limit criteria is not applicable. See case narrative.

J The result is an estimated value.

E The percent difference for the serial dilution was greater than 10%, indicating a possible matrix interference in the sample.

M The duplicate injection precision was not met.

N The Matrix Spike sample recovery is not within control limits. See case narrative.

S The reported value was determined by the Method of Standard Additions (MSA).

U The analyte was analyzed for, but was not detected ("Non-detect") at or above the MRL/MDL. DOD-QSM 4.2 definition : Analyte was not detected and is reported as less than the LOD or as defined by the project. The detection limit is adjusted for dilution.

W The post-digestion spike for furnace AA analysis is out of control limits, while sample absorbance is less than 50% of spike absorbance.

i The MRL/MDL or LOQ/LOD is elevated due to a matrix interference.

X See case narrative.

+ The correlation coefficient for the MSA is less than 0.995.

Q See case narrative. One or more quality control criteria was outside the limits.

Organic Data Qualifiers

* The result is an outlier. See case narrative.

# The control limit criteria is not applicable. See case narrative.

A A tentatively identified compound, a suspected aldol-condensation product.

B The analyte was found in the associated method blank at a level that is significant relative to the sample result as defined by the DOD or NELAC standards.

C The analyte was qualitatively confirmed using GC/MS techniques, pattern recognition, or by comparing to historical data.

D The reported result is from a dilution.

E The result is an estimated value.

J The result is an estimated value.

N The result is presumptive. The analyte was tentatively identified, but a confirmation analysis was not performed.

PThe GC or HPLC confirmation criteria was exceeded. The relative percent difference is greater than 40% between the two analytical results.

U The analyte was analyzed for, but was not detected ("Non-detect") at or above the MRL/MDL. DOD-QSM 4.2 definition : Analyte was not detected and is reported as less than the LOD or as defined by the project. The detection limit is adjusted for dilution.

i The MRL/MDL or LOQ/LOD is elevated due to a chromatographic interference.

X See case narrative.

Q See case narrative. One or more quality control criteria was outside the limits.

Additional Petroleum Hydrocarbon Specific Qualifiers

F The chromatographic fingerprint of the sample matches the elution pattern of the calibration standard.

L The chromatographic fingerprint of the sample resembles a petroleum product, but the elution pattern indicates the presence of a greater amount of lighter molecular weight constituents than the calibration standard.

H The chromatographic fingerprint of the sample resembles a petroleum product, but the elution pattern indicates the presence of a greater amount of heavier molecular weight constituents than the calibration standard.

O The chromatographic fingerprint of the sample resembles an oil, but does not match the calibration standard.

Y The chromatographic fingerprint of the sample resembles a petroleum product eluting in approximately the correct carbon range, but the elution pattern does not match the calibration standard.

Z The chromatographic fingerprint does not resemble a petroleum product.

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Agency Web Site Number

Alaska DEC UST http://dec.alaska.gov/applications/eh/ehllabreports/USTLabs.aspx UST-040

Arizona DHS http://www.azdhs.gov/lab/license/env.htm AZ0339

Arkansas - DEQ http://www.adeq.state.ar.us/techsvs/labcert.htm 88-0637

California DHS (ELAP) http://www.cdph.ca.gov/certlic/labs/Pages/ELAP.aspx 2795

DOD ELAP http://www.denix.osd.mil/edqw/Accreditation/AccreditedLabs.cfm L14-51

Florida DOH http://www.doh.state.fl.us/lab/EnvLabCert/WaterCert.htm E87412

Hawaii DOH Not available -

Idaho DHWhttp://www.healthandwelfare.idaho.gov/Health/Labs/CertificationDrinkingWaterLabs/tabid/1833/Default.aspx -

ISO 17025 http://www.pjlabs.com/ L14-50

Louisiana DEQhttp://www.deq.louisiana.gov/portal/DIVISIONS/PublicParticipationandPermitSupport/LouisianaLaboratoryAccreditationProgram.aspx 03016

Maine DHS Not available WA01276

Michigan DEQ http://www.michigan.gov/deq/0,1607,7-135-3307_4131_4156---,00.html 9949

Minnesota DOH http://www.health.state.mn.us/accreditation 053-999-457

Montana DPHHS http://www.dphhs.mt.gov/publichealth/ CERT0047

Nevada DEP http://ndep.nv.gov/bsdw/labservice.htm WA01276

New Jersey DEP http://www.nj.gov/dep/oqa/ WA005

North Carolina DWQ http://www.dwqlab.org/ 605

Oklahoma DEQ http://www.deq.state.ok.us/CSDnew/labcert.htm 9801

Oregon – DEQ (NELAP)http://public.health.oregon.gov/LaboratoryServices/EnvironmentalLaboratoryAccreditation/Pages/index.aspx WA100010

South Carolina DHEC http://www.scdhec.gov/environment/envserv/ 61002

Texas CEQ http://www.tceq.texas.gov/field/qa/env_lab_accreditation.html T104704427

Washington DOE http://www.ecy.wa.gov/programs/eap/labs/lab-accreditation.html C544

Wisconsin DNR http://dnr.wi.gov/ 998386840

Wyoming (EPA Region 8) http://www.epa.gov/region8/water/dwhome/wyomingdi.html -

Kelso Laboratory Website www.alsglobal.com NA

ALS Group USA Corp. dba ALS Environmental (ALS) - KelsoState Certifications, Accreditations, and Licenses

Analyses were performed according to our laboratory’s NELAP-approved quality assurance program. A complete listing of specific NELAP-certified analytes, can be found in the certification section at www.ALSGlobal.com or at the accreditation bodies web site.Please refer to the certification and/or accreditation body's web site if samples are submitted for compliance purposes. The states highlighted above, require the analysis be listed on the state certification if used for compliance purposes and if the method/anlayte is offered by that state.

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Case Narrative

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

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Approved by______________________________________________

ALS ENVIRONMENTAL Client: Grays Harbor Energy, LLC Service Request No.: K1509368 Project: GHEC NPDES Date Received: 08/26/15 Sample Matrix: Water

Case Narrative All analyses were performed consistent with the quality assurance program of ALS Environmental. This report contains analytical results for samples designated for Tier II data deliverables. When appropriate to the method, method blank results have been reported with each analytical test. Surrogate recoveries have been reported for all applicable organic analyses. Additional quality control analyses reported herein include: Laboratory Duplicate (DUP), Matrix Spike (MS), Matrix/Duplicate Matrix Spike (MS/DMS), Laboratory Control Sample (LCS), and Laboratory/Duplicate Laboratory Control Sample (LCS/DLCS). Sample Receipt One water sample was received for analysis at ALS Environmental on 08/26/15. The sample was received in good condition and consistent with the accompanying chain of custody form. The sample was stored in a refrigerator at 4ºC upon receipt at the laboratory. General Chemistry Parameters Orthophosphate as Phosphorus by Method 365.3: The control criteria for matrix spike recovery for sample PP were not applicable. The analyte concentration in the sample was significantly higher than the added spike concentration, preventing accurate evaluation of the spike recovery. Chlorine, Total Residual by Method SM 4500-Cl G: The matrix spike recovery for sample PP was outside control criteria. Recovery in the Laboratory Control Sample (LCS) was acceptable, which indicated the analytical batch was in control. The matrix spike outlier suggested a potential low bias in this matrix. No further corrective action was appropriate. No other anomalies associated with the analysis of these samples were observed. Total Metals No anomalies associated with the analysis of these samples were observed. Organochlorine Pesticides and PCBs by EPA Method 608 Calibration Verification Exceptions: The analysis of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) by EPA 608 requires the use of dual column confirmation. When the Continuing Calibration Verification (CCV) criteria is met for both columns, the higher of the two sample results is generally reported. The primary evaluation criteria were not met on the confirmation column for 4,4’-DDT, 4,4’-DDE and Endrin Aldehyde. The results are reported from the column with an acceptable CCV. The data quality is not affected. No further corrective action was necessary. No other anomalies associated with the analysis of these samples were observed.

Page 7 of 196

Gregory.Salata
Salata signature
Page 8: Grays Harbor Energy, LLC 401 Keys Road

Approved by______________________________________________

Volatile Organic Compounds by EPA Method 624 No anomalies associated with the analysis of these samples were observed. Semivolatile Organic Compounds by EPA Method 625 Lab Control Sample Exceptions: The advisory criterion was exceeded for Benzidine and 3,3’-Dichlorobenzidine in the replicate Laboratory Control Samples (LCS/DLCS) KWG1508140-3 and KWG1508140-4. As per the ALS/Kelso Standard Operating Procedure (SOP) for this method, these compounds are not included in the subset of analytes used to control the analysis. The recovery information reported for these analytes is for advisory purposes only (i.e. to provide additional detail related to the performance of each individual compound). No further corrective action was required. The upper control criterion was exceeded for Pyrene in Laboratory Control Sample (LCS) KWG1508140-3. The analyte in question was not detected in the associated field sample. The error associated with elevated recovery indicated a high bias. The sample data was not significantly affected. No further corrective action was appropriate. Elevated Detection Limits: The detection limit was elevated for Bis(2-chloroethyl) Ether, N-Nitrosodi-n-propylamine, Nitrobenzene, 2,6-Dinitrotoluene, 2,4-Dinitrotoluene, and Di-n-octyl Phthalate for all analyses due to insufficient instrument sensitivity necessary to detect the compound at the standard Method Reporting Limit (MRL) at time of calibration. No further corrective action was taken. The detection limits were elevated for sample PP due to less than optimal sample volume extracted for analysis. Sample Notes and Discussion: The target analyte list for EPA Method 625 does not include Perylene, 3-Methylcholanthrene, Dibenzo(a,i)pyrene, Dibenzo(a,e)pyrene, Dibenz(a,h)acridine, Dibenz(a,h)pyrene, Dibenz(a,h)acridine. The analytes were searched for and quantitated as a Tentatively Identified Compound (TIC). Quantitative standards were not analyzed for the listed analytes. No other anomalies associated with the analysis of these samples were observed. Dioxins and Furans by EPA Method 1613B The analysis for Dioxins and Furans was performed at ALS Environmental in Houston, Texas. The data for this analysis is included in the corresponding section of this report.

Page 8 of 196

Gregory.Salata
Salata signature
Page 9: Grays Harbor Energy, LLC 401 Keys Road

Chain of Custody

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

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Page 10 of 196

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General Chemistry

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 13 of 196

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Oil and Grease, Total (HEM)

Basis:Units: mg/L

NA1664AMethodPrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 09/15/15 22:40 9/15/1510.85.4 UNDK1509368-001Method Blank 09/15/15 22:40 9/15/1510.85.0 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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QA/QC Report

mg/LK1509635-001 Basis:Lab Code:

Units:Sample Name: Batch QC

Oil and Grease, Total (HEM)Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/15/15N/A

Date Collected: N/A

Method1664A

Prep Method:Analysis Method:

Analyte Name ResultSample Result Spike Amount % Rec

Matrix SpikeK1509635-001MS

% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

09/15/15Date Extracted:

Oil and Grease, Total (HEM) ND U 52.0 57.1 91 78-114

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Duplicate Lab Control SampleK1509368-DLCS3

Lab Control SampleK1509368-LCS3

Analyte Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Duplicate Lab Control Sample SummaryGeneral Chemistry Parameters

Analysis Method:Prep Method:

1664AMethod NA

mg/LBasis:Units:

Analysis Lot: 462405

09/15/15

Spike AmountResult % Rec % RecResult

Spike Amount

% Rec Limits RPD

RPD Limit

09/15/15Date Extracted:

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

56.0 60.0Oil and Grease, Total (HEM) 207 78-11487 60.052.3 93

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Page 16 of 196

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Bromide

Basis:Units: mg/L

NA300.0MethodPrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 08/26/15 15:15 8/26/1520.0080.20 UNDK1509368-001Method Blank 08/26/15 09:42 8/26/1510.0040.10 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

Printed 9/17/2015 9:21:02 AM 15-0000344261 rev 00Superset Reference:

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

08/26/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC mg/LBasis:Units:

KQ1509534-03 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

KQ1509534-03DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Bromide NC 0.20 0.008 ND U ND U NC 20300.0

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LKQ1509534-03 Basis:Lab Code:

Units:Sample Name: Batch QC

BromideDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeKQ1509534-03MS KQ1509534-03DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Bromide ND U 9.63 10.0 96 9.59 10.0 96 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryBromide

Analysis Method:Prep Method:

300.0Method NA

mg/LBasis:Units:

Analysis Lot: 459716

08/26/15

Spike AmountResult % Rec

% Rec Limits

08/26/15Date Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 90-11096 2.502.41K1509368-LCS1

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ALS Group USA, Corp.

Bromide

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: 300.0 mg/LUnits:

dba ALS Environmental

90-110962.40459716 2.5008/26/15 08:59KQ1509535-01CCV190-110962.41459716 2.5008/26/15 11:52KQ1509535-02CCV290-110962.39459716 2.5008/26/15 14:45KQ1509535-03CCV390-110962.41459716 2.5008/26/15 18:26KQ1509535-04CCV4

15-0000344261 rev 00Printed 9/17/2015 9:21:03 AM Superset Reference:

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ALS Group USA, Corp.

300.0

Bromide

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509535-05 08/26/15 09:14 0.10459716 0.004 UNDCCB2 KQ1509535-06 08/26/15 12:07 0.10459716 0.004 UNDCCB3 KQ1509535-07 08/26/15 15:00 0.10459716 0.004 UNDCCB4 KQ1509535-08 08/26/15 18:41 0.10459716 0.004 UND

15-0000344261 rev 00Printed 9/17/2015 9:21:03 AM Superset Reference:

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Fluoride

Basis:Units: mg/L

NA300.0MethodPrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 08/26/15 15:15 8/26/1520.0060.20 J0.08K1509368-001Method Blank 08/26/15 09:42 8/26/1510.0030.10 J0.01K1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.dba ALS Environmental

QA/QC Report

Client:ProjectSample Matrix:

Prep Method:Analysis Method:

Grays Harbor Energy, LLCGHEC NPDESWater

300.0Method

Service Request:Date Collected:Date Received:

Basis:Units:

K1509368NANA

mg/LNA

Replicate Sample SummaryFluoride

Sample Name: Lab Code:Date

AnalyzedRPDLimitMRL MDL RPD

DuplicateResult Average

SampleResult

<1 0.20 0.006 0.86 0.86 0.859 20Batch QC K1509300-001DUP 08/26/15NC 0.20 0.006 ND U ND U NC 20Batch QC KQ1509534-03DUP 08/26/15

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

Printed 9/17/2015 9:21:03 AM 15-0000344261 rev 00Superset Reference:

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QA/QC Report

mg/LK1509300-001 Basis:Lab Code:

Units:Sample Name: Batch QC

FluorideDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509300-001MS K1509300-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Fluoride 0.86 11.2 10.0 103 11.0 10.0 101 90-110 2 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

Printed 9/17/2015 9:21:03 AM 15-0000344261 rev 00Superset Reference:

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QA/QC Report

mg/LKQ1509534-03 Basis:Lab Code:

Units:Sample Name: Batch QC

FluorideDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeKQ1509534-03MS KQ1509534-03DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Fluoride ND U 10.1 10.0 101 10.1 10.0 101 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryFluoride

Analysis Method:Prep Method:

300.0Method NA

mg/LBasis:Units:

Analysis Lot: 459716

08/26/15

Spike AmountResult % Rec

% Rec Limits

08/26/15Date Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 90-11095 5.004.76K1509368-LCS1

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ALS Group USA, Corp.

Fluoride

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: 300.0 mg/LUnits:

dba ALS Environmental

90-110954.77459716 5.0008/26/15 08:59KQ1509535-01CCV190-110954.77459716 5.0008/26/15 11:52KQ1509535-02CCV290-110954.73459716 5.0008/26/15 14:45KQ1509535-03CCV390-110964.80459716 5.0008/26/15 18:26KQ1509535-04CCV4

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ALS Group USA, Corp.

300.0

Fluoride

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509535-05 08/26/15 09:14 0.10459716 0.003 UNDCCB2 KQ1509535-06 08/26/15 12:07 0.10459716 0.003 J0.02CCB3 KQ1509535-07 08/26/15 15:00 0.10459716 0.003 J0.02CCB4 KQ1509535-08 08/26/15 18:41 0.10459716 0.003 UND

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Nitrite as Nitrogen

Basis:Units: mg/L

NA300.0MethodPrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 08/26/15 15:15 8/26/1520.0040.10 UNDK1509368-001Method Blank 08/26/15 09:42 8/26/1510.0020.050 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

08/26/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC mg/LBasis:Units:

K1509300-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509300-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Nitrite as Nitrogen NC 0.10 0.004 ND U ND U NC 20300.0

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509300-001 Basis:Lab Code:

Units:Sample Name: Batch QC

Nitrite as NitrogenDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509300-001MS K1509300-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Nitrite as Nitrogen ND U 10.1 10.0 101 10.0 10.0 100 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryNitrite as Nitrogen

Analysis Method:Prep Method:

300.0Method NA

mg/LBasis:Units:

Analysis Lot: 459716

08/26/15

Spike AmountResult % Rec

% Rec Limits

08/26/15Date Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 90-110102 2.502.55K1509368-LCS1

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Page 33 of 196

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ALS Group USA, Corp.

Nitrite as Nitrogen

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: 300.0 mg/LUnits:

dba ALS Environmental

90-1101022.55459716 2.5008/26/15 08:59KQ1509535-01CCV190-1101032.57459716 2.5008/26/15 11:52KQ1509535-02CCV290-1101022.56459716 2.5008/26/15 14:45KQ1509535-03CCV390-1101032.57459716 2.5008/26/15 18:26KQ1509535-04CCV4

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ALS Group USA, Corp.

300.0

Nitrite as Nitrogen

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509535-05 08/26/15 09:14 0.050459716 0.002 UNDCCB2 KQ1509535-06 08/26/15 12:07 0.050459716 0.002 UNDCCB3 KQ1509535-07 08/26/15 15:00 0.050459716 0.002 UNDCCB4 KQ1509535-08 08/26/15 18:41 0.050459716 0.002 UND

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Nitrate as Nitrogen

Basis:Units: mg/L

NA300.0MethodPrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 08/26/15 15:15 8/26/1520.010.106.65K1509368-001Method Blank 08/26/15 09:42 8/26/1510.0050.050 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.dba ALS Environmental

QA/QC Report

Client:ProjectSample Matrix:

Prep Method:Analysis Method:

Grays Harbor Energy, LLCGHEC NPDESWater

300.0Method

Service Request:Date Collected:Date Received:

Basis:Units:

K1509368NANA

mg/LNA

Replicate Sample SummaryNitrate as Nitrogen

Sample Name: Lab Code:Date

AnalyzedRPDLimitMRL MDL RPD

DuplicateResult Average

SampleResult

1 0.10 0.01 0.88 0.87 0.880 20Batch QC K1509287-001DUP 08/26/15<1 0.10 0.01 0.12 0.11 0.114 20Batch QC K1509300-001DUP 08/26/15

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509287-001 Basis:Lab Code:

Units:Sample Name: Batch QC

Nitrate as NitrogenDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509287-001MS K1509287-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Nitrate as Nitrogen 0.88 10.3 10.0 95 10.3 10.0 94 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509300-001 Basis:Lab Code:

Units:Sample Name: Batch QC

Nitrate as NitrogenDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509300-001MS K1509300-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Nitrate as Nitrogen 0.12 9.73 10.0 96 9.64 10.0 95 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryNitrate as Nitrogen

Analysis Method:Prep Method:

300.0Method NA

mg/LBasis:Units:

Analysis Lot: 459716

08/26/15

Spike AmountResult % Rec

% Rec Limits

08/26/15Date Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 90-11093 2.502.33K1509368-LCS1

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Page 40 of 196

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ALS Group USA, Corp.

Nitrate as Nitrogen

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: 300.0 mg/LUnits:

dba ALS Environmental

90-110932.34459716 2.5008/26/15 08:59KQ1509535-01CCV190-110932.33459716 2.5008/26/15 11:52KQ1509535-02CCV290-110932.32459716 2.5008/26/15 14:45KQ1509535-03CCV390-110932.33459716 2.5008/26/15 18:26KQ1509535-04CCV4

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ALS Group USA, Corp.

300.0

Nitrate as Nitrogen

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509535-05 08/26/15 09:14 0.050459716 0.005 UNDCCB2 KQ1509535-06 08/26/15 12:07 0.050459716 0.005 UNDCCB3 KQ1509535-07 08/26/15 15:00 0.050459716 0.005 UNDCCB4 KQ1509535-08 08/26/15 18:41 0.050459716 0.005 UND

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Sulfate

Basis:Units: mg/L

NA300.0MethodPrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 08/26/15 17:14 8/26/15100110495K1509368-001Method Blank 08/26/15 09:42 8/26/1510.010.10 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.dba ALS Environmental

QA/QC Report

Client:ProjectSample Matrix:

Prep Method:Analysis Method:

Grays Harbor Energy, LLCGHEC NPDESWater

300.0Method

Service Request:Date Collected:Date Received:

Basis:Units:

K1509368NANA

mg/LNA

Replicate Sample SummarySulfate

Sample Name: Lab Code:Date

AnalyzedRPDLimitMRL MDL RPD

DuplicateResult Average

SampleResult

<1 0.20 0.02 7.03 7.06 7.04 20Batch QC K1509300-001DUP 08/26/15<1 0.20 0.02 0.49 0.49 0.487 20Batch QC KQ1509534-03DUP 08/26/15

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509300-001 Basis:Lab Code:

Units:Sample Name: Batch QC

SulfateDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509300-001MS K1509300-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Sulfate 7.03 16.6 10.0 95 16.6 10.0 96 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LKQ1509534-03 Basis:Lab Code:

Units:Sample Name: Batch QC

SulfateDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/15N/A

Date Collected: N/A

Method300.0

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeKQ1509534-03MS KQ1509534-03DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/26/15Date Extracted:

Sulfate 0.49 9.77 10.0 93 9.72 10.0 92 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummarySulfate

Analysis Method:Prep Method:

300.0Method NA

mg/LBasis:Units:

Analysis Lot: 459716

08/26/15

Spike AmountResult % Rec

% Rec Limits

08/26/15Date Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 90-11093 5.004.66K1509368-LCS1

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Page 47 of 196

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ALS Group USA, Corp.

Sulfate

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: 300.0 mg/LUnits:

dba ALS Environmental

90-110944.70459716 5.0008/26/15 08:59KQ1509535-01CCV190-110944.69459716 5.0008/26/15 11:52KQ1509535-02CCV290-110954.74459716 5.0008/26/15 14:45KQ1509535-03CCV390-110944.70459716 5.0008/26/15 18:26KQ1509535-04CCV4

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ALS Group USA, Corp.

300.0

Sulfate

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509535-05 08/26/15 09:14 0.10459716 0.01 UNDCCB2 KQ1509535-06 08/26/15 12:07 0.10459716 0.01 UNDCCB3 KQ1509535-07 08/26/15 15:00 0.10459716 0.01 UNDCCB4 KQ1509535-08 08/26/15 18:41 0.10459716 0.01 UND

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Cyanide, Total

Basis:Units: mg/L

NA335.4MethodPrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 09/02/15 11:59 9/1/1510.00090.010 J0.003K1509368-001Method Blank 09/02/15 11:59 9/1/1510.00090.010 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

09/02/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC mg/LBasis:Units:

KQ1509769-10 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

KQ1509769-10DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Cyanide, Total NC 0.010 0.0009 ND U ND U NC 20335.4

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LKQ1509769-10 Basis:Lab Code:

Units:Sample Name: Batch QC

Cyanide, TotalDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/2/15N/A

Date Collected: N/A

Method335.4

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeKQ1509769-10MS KQ1509769-10DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

09/1/15Date Extracted:

Cyanide, Total ND U 0.108 0.100 108 0.108 0.100 108 90-110 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryCyanide, Total

Analysis Method:Prep Method:

335.4Method NA

mg/LBasis:Units:

Analysis Lot: 460676

09/02/15

Spike AmountResult % Rec

% Rec Limits

09/01/15Date Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 90-110107 0.1500.161K1509368-LCS1

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Page 53 of 196

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ALS Group USA, Corp.

Cyanide, Total

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: 335.4 ug/LUnits:

dba ALS Environmental

90-110103103460676 10009/02/15 11:59KQ1509829-17CCV190-110103103460676 10009/02/15 11:59KQ1509829-18CCV290-110103103460676 10009/02/15 11:59KQ1509829-19CCV390-110104104460676 10009/02/15 11:59KQ1509829-20CCV490-110104104460676 10009/02/15 11:59KQ1509829-21CCV590-110104104460676 10009/02/15 11:59KQ1509829-22CCV690-110103103460676 10009/02/15 11:59KQ1509829-23CCV7

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ALS Group USA, Corp.

335.4

Cyanide, Total

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509829-10 09/02/15 11:59 0.010460676 0.0009 UNDCCB2 KQ1509829-11 09/02/15 11:59 0.010460676 0.0009 UNDCCB3 KQ1509829-12 09/02/15 11:59 0.010460676 0.0009 UNDCCB4 KQ1509829-13 09/02/15 11:59 0.010460676 0.0009 UNDCCB5 KQ1509829-14 09/02/15 11:59 0.010460676 0.0009 UNDCCB6 KQ1509829-15 09/02/15 11:59 0.010460676 0.0009 UNDCCB7 KQ1509829-16 09/02/15 11:59 0.010460676 0.0009 UND

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K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Orthophosphate as Phosphorus

Basis:Units: mg/L

NA365.3NonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 15:3350.0200.0502.09K1509368-001Method Blank 08/26/15 15:3310.0040.010 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

08/26/15Date Collected:Date Received: 08/26/15

08/26/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

PP mg/LBasis:Units:

K1509368-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509368-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Orthophosphate as Phosphorus 2 0.050 0.020 2.09 2.06 2.07 20365.3

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509368-001 Basis:Lab Code:

Units:Sample Name: PP

Orthophosphate as PhosphorusDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/1508/26/15

Date Collected: 08/26/15

None365.3

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509368-001MS K1509368-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

NADate Extracted:

Orthophosphate as Phosphorus 2.09 2.41 0.400 79 #2.46 0.400 90 # 60-130 13 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryOrthophosphate as Phosphorus

Analysis Method:Prep Method:

365.3None NA

mg/LBasis:Units:

Analysis Lot: 459599

08/26/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 85-11591 2.542.31K1509368-LCS1

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Orthophosphate as Phosphorus

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: 365.3 mg/LUnits:

dba ALS Environmental

90-110940.472459599 0.50008/26/15 15:33KQ1509502-01CCV190-110940.472459599 0.50008/26/15 15:33KQ1509502-02CCV290-110950.476459599 0.50008/26/15 15:33KQ1509502-03CCV390-110950.475459599 0.50008/26/15 15:33KQ1509502-04CCV4

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ALS Group USA, Corp.

365.3

Orthophosphate as Phosphorus

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509502-05 08/26/15 15:33 0.010459599 0.004 UNDCCB2 KQ1509502-06 08/26/15 15:33 0.010459599 0.004 UNDCCB3 KQ1509502-07 08/26/15 15:33 0.010459599 0.004 UNDCCB4 KQ1509502-08 08/26/15 15:33 0.010459599 0.004 UND

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K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Nitrogen, Total Kjeldahl (TKN)

Basis:Units: mg/L

NAASTM D1426-08BASTM D3590-02(2006)(A)Prep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDate

ExtractedDil.MDLMRLResult Q

PP 09/09/15 10:30 9/8/1520.080.401.67K1509368-001Method Blank 09/09/15 10:30 9/8/1520.080.40 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

09/09/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC mg/LBasis:Units:

K1509407-002 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509407-002DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Nitrogen, Total Kjeldahl (TKN) 2 0.40 0.08 0.48 0.47 0.472 20ASTM D1426-08B

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509407-002 Basis:Lab Code:

Units:Sample Name: Batch QC

Nitrogen, Total Kjeldahl (TKN)Duplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/9/15N/A

Date Collected: N/A

ASTM D3590-02(2006)(A)ASTM D1426-08B

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509407-002MS K1509407-002DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

09/8/15Date Extracted:

Nitrogen, Total Kjeldahl (TKN) 0.48 18.9 20.0 92 17.3 20.0 84 53-160 9 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryNitrogen, Total Kjeldahl (TKN)

Analysis Method:Prep Method:

ASTM D1426-08BASTM D3590-02(2006)(A) NA

mg/LBasis:Units:

Analysis Lot: 461172

09/09/15

Spike AmountResult % Rec

% Rec Limits

09/08/15Date Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 72-12996 6.456.20K1509368-LCS1

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Nitrogen, Total Kjeldahl (TKN)

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: ASTM D1426-08B mg/LUnits:

dba ALS Environmental

90-11010310.3461172 10.009/09/15 10:30KQ1510041-05CCV190-11010510.5461172 10.009/09/15 10:30KQ1510041-06CCV290-11010410.4461172 10.009/09/15 10:30KQ1510041-07CCV390-11010510.5461172 10.009/09/15 10:30KQ1510041-08CCV4

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ASTM D1426-08B

Nitrogen, Total Kjeldahl (TKN)

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1510041-01 09/09/15 10:30 0.20461172 0.04 UNDCCB2 KQ1510041-02 09/09/15 10:30 0.20461172 0.04 J0.05CCB3 KQ1510041-03 09/09/15 10:30 0.20461172 0.04 UNDCCB4 KQ1510041-04 09/09/15 10:30 0.20461172 0.04 UND

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Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Nitrate+Nitrite as Nitrogen

Basis:Units: mg/L

NACalculationNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 15:1510.010.206.65K1509368-001

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Nitrogen, Total Organic as Nitrogen

Basis:Units: mg/L

NACalculationNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 09/09/15 10:3010.070.351.56K1509368-001

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Color

Basis:Units: ColorUnits

NASM 2120 BNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 15:381-5.0 UNDK1509368-001Method Blank 08/26/15 10:201-5.0 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

08/26/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC ColorUnitsBasis:Units:

K1509300-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509300-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Color NC 5.0 - ND U ND U NC 20SM 2120 B

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryColor

Analysis Method:Prep Method:

SM 2120 BNone NA

ColorUnitsBasis:Units:

Analysis Lot: 459595

08/26/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 85-115100 50.050.0K1509368-LCS1

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Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Solids, Total Dissolved

Basis:Units: mg/L

NASM 2540 CNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 09/01/15 16:311-131030K1509368-001Method Blank 09/01/15 16:311-10 UNDK1509368-MB1Method Blank 09/01/15 16:311-10 UNDK1509368-MB2

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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QA/QC Report

Client:ProjectSample Matrix:

Prep Method:Analysis Method:

Grays Harbor Energy, LLCGHEC NPDESWater

SM 2540 CNone

Service Request:Date Collected:Date Received:

Basis:Units:

K1509368NANA

mg/LNA

Replicate Sample SummarySolids, Total Dissolved

Sample Name: Lab Code:Date

AnalyzedRPDLimitMRL MDL RPD

DuplicateResult Average

SampleResult

9 10 - 122 134 128 10Batch QC K1509407-002DUP 09/01/15<1 10 - 324 325 325 10Batch QC K1509459-014DUP 09/01/15

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummarySolids, Total Dissolved

Analysis Method:Prep Method:

SM 2540 CNone NA

mg/LBasis:Units:

Analysis Lot: 460473

09/01/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 85-11598 897882K1509368-LCS1

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K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Solids, Total Suspended (TSS)

Basis:Units: mg/L

NASM 2540 DNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/27/15 14:061-5.0 UNDK1509368-001Method Blank 08/27/15 14:061-5.0 UNDK1509368-MB1Method Blank 08/27/15 14:061-5.0 UNDK1509368-MB2

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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QA/QC Report

Client:ProjectSample Matrix:

Prep Method:Analysis Method:

Grays Harbor Energy, LLCGHEC NPDESWater

SM 2540 DNone

Service Request:Date Collected:Date Received:

Basis:Units:

K1509368NANA

mg/LNA

Replicate Sample SummarySolids, Total Suspended (TSS)

Sample Name: Lab Code:Date

AnalyzedRPDLimitMRL MDL RPD

DuplicateResult Average

SampleResult

NC 5.0 - ND U ND U NC 10Batch QC K1509239-001DUP 08/27/15NC 5.0 - ND U ND U NC 10Batch QC K1509355-001DUP 08/27/15

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummarySolids, Total Suspended (TSS)

Analysis Method:Prep Method:

SM 2540 DNone NA

mg/LBasis:Units:

Analysis Lot: 459832

08/27/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 85-11597 191186K1509368-LCS1

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Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Chlorine, Total Residual

Basis:Units: mg/L

NASM 4500-Cl GNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 15:0010.0090.050 UND HK1509368-001Method Blank 08/26/15 15:0010.0090.050 UNDK1509368-MB1Method Blank 08/26/15 15:0010.0090.050 UNDK1509368-MB2

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

08/26/15Date Collected:Date Received: 08/26/15

08/26/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

PP mg/LBasis:Units:

K1509368-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509368-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Chlorine, Total Residual NC 0.050 0.009 ND U ND U NC 20SM 4500-Cl G

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509368-001 Basis:Lab Code:

Units:Sample Name: PP

Chlorine, Total ResidualDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/26/1508/26/15

Date Collected: 08/26/15

NoneSM 4500-Cl G

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509368-001MS K1509368-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

NADate Extracted:

Chlorine, Total Residual ND U ND 1.00 0 *ND 1.00 0 * 21-141 NC 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryChlorine, Total Residual

Analysis Method:Prep Method:

SM 4500-Cl GNone NA

mg/LBasis:Units:

Analysis Lot: 459600

08/26/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 78-116106 1.001.06K1509368-LCS1Lab Control Sample 78-116106 1.001.06K1509368-LCS2

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Client:

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K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Ammonia as Nitrogen

Basis:Units: mg/L

NASM 4500-NH3 ENonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 09/02/15 08:0010.0090.0500.117K1509368-001Method Blank 09/02/15 08:0010.0090.050 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

09/02/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC mg/LBasis:Units:

K1509359-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509359-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Ammonia as Nitrogen 5 2.5 0.5 144 137 140 20SM 4500-NH3 E

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509359-001 Basis:Lab Code:

Units:Sample Name: Batch QC

Ammonia as NitrogenMatrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/2/15N/A

Date Collected: N/A

NoneSM 4500-NH3 E

Prep Method:Analysis Method:

Analyte Name ResultSample Result Spike Amount % Rec

Matrix SpikeK1509359-001MS

% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

NADate Extracted:

Ammonia as Nitrogen 144 625 500 96 80-115

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryAmmonia as Nitrogen

Analysis Method:Prep Method:

SM 4500-NH3 ENone NA

mg/LBasis:Units:

Analysis Lot: 460672

09/02/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 80-115100 5.365.35K1509368-LCS1

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ALS Group USA, Corp.

Ammonia as Nitrogen

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: SM 4500-NH3 E mg/LUnits:

dba ALS Environmental

90-110979.68460672 10.009/02/15 08:00KQ1509836-09CCV190-110999.88460672 10.009/02/15 08:00KQ1509836-10CCV290-1101009.96460672 10.009/02/15 08:00KQ1509836-11CCV390-11010210.2460672 10.009/02/15 08:00KQ1509836-12CCV4

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ALS Group USA, Corp.

SM 4500-NH3 E

Ammonia as Nitrogen

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509836-05 09/02/15 08:00 0.050460672 0.009 UNDCCB2 KQ1509836-06 09/02/15 08:00 0.050460672 0.009 J0.018CCB3 KQ1509836-07 09/02/15 08:00 0.050460672 0.009 J0.023CCB4 KQ1509836-08 09/02/15 08:00 0.050460672 0.009 J0.019

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Oxygen, Dissolved

Basis:Units: mg/L

NASM 4500-O GNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 14:201-1.07.3 HK1509368-001

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Total Sulfide

Basis:Units: mg/L

NASM 4500-S2- DNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 09/02/15 23:3710.0200.050 UNDK1509368-001Method Blank 09/02/15 23:3710.0200.050 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

08/26/15Date Collected:Date Received: 08/26/15

09/02/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

PP mg/LBasis:Units:

K1509368-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509368-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Total Sulfide NC 0.050 0.020 ND U ND U NC 20SM 4500-S2- D

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509368-001 Basis:Lab Code:

Units:Sample Name: PP

Total SulfideDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/2/1508/26/15

Date Collected: 08/26/15

NoneSM 4500-S2- D

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509368-001MS K1509368-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

NADate Extracted:

Total Sulfide ND U 1.74 1.88 93 1.74 1.88 92 69-123 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryTotal Sulfide

Analysis Method:Prep Method:

SM 4500-S2- DNone NA

mg/LBasis:Units:

Analysis Lot: 460705

09/02/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 85-10692 1.881.73K1509368-LCS1

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ALS Group USA, Corp.

Total Sulfide

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: SM 4500-S2- D mg/LUnits:

dba ALS Environmental

90-1101011.89460705 1.8809/02/15 23:37KQ1509874-06CCV190-1101011.89460705 1.8809/02/15 23:37KQ1509874-07CCV2

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ALS Group USA, Corp.

SM 4500-S2- D

Total Sulfide

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509874-08 09/02/15 23:37 0.050460705 0.020 UNDCCB2 KQ1509874-09 09/02/15 23:37 0.050460705 0.020 UND

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Sulfite

Basis:Units: mg/L

NASM 4500-SO32- BNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 18:2310.32.06.6 HK1509368-001Method Blank 08/26/15 18:2310.32.0 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

08/26/15Date Collected:Date Received: 08/26/15

08/26/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

PP mg/LBasis:Units:

K1509368-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509368-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Sulfite 2 2.0 0.3 6.6 6.5 6.55 20SM 4500-SO32- B

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Biochemical Oxygen Demand (BOD)

Basis:Units: mg/L

NASM 5210 BNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/27/15 15:1522.04.0 UNDK1509368-001

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

08/27/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC mg/LBasis:Units:

K1508360-038 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1508360-038DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Biochemical Oxygen Demand (BOD) 2 30 15 92 90 90.9 20SM 5210 B

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryBiochemical Oxygen Demand (BOD)

Analysis Method:Prep Method:

SM 5210 BNone NA

mg/LBasis:Units:

Analysis Lot: 460349

08/27/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 85-11594 198187K1509368-LCS1

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Chemical Oxygen Demand (COD)

Basis:Units: mg/L

NASM 5220 CNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 09/01/15 15:0513.05.016.1K1509368-001Method Blank 09/01/15 15:0513.05.0 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

NADate Collected:Date Received: NA

09/01/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

Batch QC mg/LBasis:Units:

K1509524-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509524-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Chemical Oxygen Demand (COD) 4 5.0 3.0 12.0 11.5 11.7 20SM 5220 C

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509524-001 Basis:Lab Code:

Units:Sample Name: Batch QC

Chemical Oxygen Demand (COD)Duplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/1/15N/A

Date Collected: N/A

NoneSM 5220 C

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509524-001MS K1509524-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

NADate Extracted:

Chemical Oxygen Demand (COD) 12.0 116 100 104 115 100 103 80-128 <1 20

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryChemical Oxygen Demand (COD)

Analysis Method:Prep Method:

SM 5220 CNone NA

mg/LBasis:Units:

Analysis Lot: 460443

09/01/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 83-117101 91.592.1K1509368-LCS1

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Carbon, Total Organic

Basis:Units: mg/L

NASM 5310 CNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 09/03/15 19:3610.070.506.49K1509368-001Method Blank 09/03/15 19:3610.070.50 J0.11K1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

08/26/15Date Collected:Date Received: 08/26/15

09/03/15Date Analyzed:

Replicate Sample SummaryGeneral Chemistry Parameters

PP mg/LBasis:Units:

K1509368-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

K1509368-001DUP Result Average

SampleResultAnalyte Name

dba ALS Environmental

Carbon, Total Organic 2 0.50 0.07 6.49 6.35 6.42 10SM 5310 C

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509368-001 Basis:Lab Code:

Units:Sample Name: PP

Carbon, Total OrganicMatrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/3/1508/26/15

Date Collected: 08/26/15

NoneSM 5310 C

Prep Method:Analysis Method:

Analyte Name ResultSample Result Spike Amount % Rec

Matrix SpikeK1509368-001MS

% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

NADate Extracted:

Carbon, Total Organic 6.49 33.1 25.0 106 83-117

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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QA/QC Report

mg/LK1509379-001 Basis:Lab Code:

Units:Sample Name: Batch QC

Carbon, Total OrganicDuplicate Matrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/3/15N/A

Date Collected: N/A

NoneSM 5310 C

Prep Method:Analysis Method:

Analyte NameRPD LimitRPDResult

Sample Result

Spike Amount % Rec

Matrix SpikeK1509379-001MS K1509379-001DMS

Duplicate Matrix Spike

% RecSpike

AmountResult% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

NADate Extracted:

Carbon, Total Organic 5.5 51.8 50.0 93 51.8 50.0 93 83-117 <1 10

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

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Sample Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryCarbon, Total Organic

Analysis Method:Prep Method:

SM 5310 CNone NA

mg/LBasis:Units:

Analysis Lot: 460883

09/03/15

Spike AmountResult % Rec

% Rec Limits

NADate Extracted:

Lab Code

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Lab Control Sample 83-11799 19.819.7K1509368-LCS1

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ALS Group USA, Corp.

Carbon, Total Organic

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: SM 5310 C mg/LUnits:

dba ALS Environmental

90-1109824.5460883 25.009/03/15 19:36KQ1509940-30CCV190-1109924.8460883 25.009/03/15 19:36KQ1509940-31CCV290-1109924.8460883 25.009/03/15 19:36KQ1509940-32CCV390-1109724.1460883 25.009/03/15 19:36KQ1509940-33CCV490-1109523.7460883 25.009/03/15 19:36KQ1509940-38CCV5

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ALS Group USA, Corp.

SM 5310 C

Carbon, Total Organic

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509940-34 09/03/15 19:36 0.50460883 0.07 UNDCCB2 KQ1509940-35 09/03/15 19:36 0.50460883 0.07 J0.13CCB3 KQ1509940-36 09/03/15 19:36 0.50460883 0.07 J0.12CCB4 KQ1509940-37 09/03/15 19:36 0.50460883 0.07 UNDCCB5 KQ1509940-39 09/03/15 19:36 0.50460883 0.07 UND

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Methylene Blue Active Substances

Basis:Units: mg/L

NASM 5540 CNonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 12:4010.0500.050 UNDK1509368-001Method Blank 08/26/15 12:4010.0500.050 UNDK1509368-MB1

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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Duplicate Lab Control SampleK1509368-DLCS3

Lab Control SampleK1509368-LCS3

Analyte Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Duplicate Lab Control Sample SummaryGeneral Chemistry Parameters

Analysis Method:Prep Method:

SM 5540 CNone NA

mg/LBasis:Units:

Analysis Lot: 459544

08/26/15

Spike AmountResult % Rec % RecResult

Spike Amount

% Rec Limits RPD

RPD Limit

NADate Extracted:

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

0.170 0.200Methylene Blue Active Substances 203 70-13082 0.2000.165 85

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ALS Group USA, Corp.

Methylene Blue Active Substances

QA/QC Report

Continuing Calibration Verification (CCV) Summary

Analysis Lot Lab Code

Date Analyzed

True Value

Measured Value

Percent Recovery Acceptance Limits

Project:Grays Harbor Energy, LLCGHEC NPDES

Client: Service Request: K1509368

Analysis Method: SM 5540 C mg/LUnits:

dba ALS Environmental

90-110830.330459544 0.40008/26/15 12:40KQ1509479-01CCV190-110850.340459544 0.40008/26/15 12:40KQ1509479-07CCV2

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ALS Group USA, Corp.

SM 5540 C

Methylene Blue Active Substances

Client:Project:

Grays Harbor Energy, LLC Service Request:K1509368

QA/QC Report

mg/L

GHEC NPDES

Analysis Method:

Continuing Calibration Blank (CCB) Summary

Units:

Analysis Lot Lab Code

Date Analyzed MRL MDL QResult

dba ALS Environmental

CCB1 KQ1509479-02 08/26/15 12:40 0.050459544 0.050 UNDCCB2 KQ1509479-06 08/26/15 12:40 0.050459544 0.050 UND

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Client:

08/26/15

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15

Coliform, Fecal

Basis:Units: MPN/100mL

NASM 9221 ENonePrep Method:

Analysis Method:

Lab CodeSample NameDate

AnalyzedDil.MDLMRLResult Q

PP 08/26/15 14:301-1.8 UNDK1509368-001

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

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Metals

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

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ALS Group USA, Corp.dba ALS Environmental

Analytical Report

Client: Grays Harbor Energy, LLC Service Request: K1509368

Project: GHEC NPDES Date Collected: 08/26/15

Sample Matrix: Water Date Received: 08/26/15

Mercury, Total

Prep Method: METHOD Units: ng/L

Analysis Method: 1631E Basis: NA

Test Notes:

Dilution Date Date ResultSample Name Lab Code MRL MDL Factor Extracted Analyzed Result Notes

PP K1509368-001 0.5 0.06 1 08/31/15 09/08/15 44.4

Method Blank 1 K1509368-MB1 0.5 0.06 1 08/31/15 09/08/15 ND

Method Blank 2 K1509368-MB2 0.5 0.06 1 08/31/15 09/08/15 ND

Method Blank 3 K1509368-MB3 0.5 0.06 1 08/31/15 09/08/15 ND

K1509368ICP.JB1 - Sample 09/09/15 Page No.:

Page 118 of 196

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ALS Group USA, Corp.dba ALS Environmental

QA/QC Report

Client: Grays Harbor Energy, LLC Service Request: K1509368Project: GHEC NPDES Date Collected: NASample Matrix: Water Date Received: NA

Date Extracted: 08/31/15Date Analyzed: 09/08/15

Matrix Spike/Duplicate Matrix Spike Summary

Total Metals

Sample Name: Batch QC Units: ng/L

Lab Code: K1509334-001MS, K1509334-001MSD Basis: NATest Notes:

P e r c e n t R e c o v e r y

ALS RelativePrep Analysis Spike Level Sample Spike Result Acceptance Percent Result

Analyte Method Method MRL MS DMS Result MS DMS MS DMS Limits Difference Notes Mercury METHOD 1631E 0.5 50 50 2.95 53.6 52.2 101 99 71-125 3

K1509368ICP.JB1 - DMS 09/09/15 Page No.:

Page 119 of 196

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ALS Group USA, Corp.dba ALS Environmental

QA/QC Report

Client: Grays Harbor Energy, LLC Service Request: K1509368

Project: GHEC NPDES Date Collected: NALCS Matrix: Water Date Received: NA

Date Extracted: NADate Analyzed: 09/08/15

Ongoing Precision and Recovery (OPR) Sample SummaryTotal Metals

Sample Name: Ongoing Precision and Recovery (Initial) Units: ng/L

Basis: NA

Test Notes:

ALSPercent

RecoveryPrep Analysis True Percent Acceptance Result

Analyte Method Method Value Result Recovery Limits Notes

Mercury METHOD 1631E 5.00 5.92 118 77-123

K1509368ICP.JB1 - OPR (lcsw) 09/09/15 Page No.:

Page 120 of 196

Page 121: Grays Harbor Energy, LLC 401 Keys Road

ALS Group USA, Corp.dba ALS Environmental

QA/QC Report

Client: Grays Harbor Energy, LLC Service Request: K1509368

Project: GHEC NPDES Date Collected: NALCS Matrix: Water Date Received: NA

Date Extracted: NADate Analyzed: 09/08/15

Ongoing Precision and Recovery (OPR) Sample SummaryTotal Metals

Sample Name: Ongoing Precision and Recovery (Final) Units: ng/L

Basis: NA

Test Notes:

ALSPercent

RecoveryPrep Analysis True Percent Acceptance Result

Analyte Method Method Value Result Recovery Limits Notes

Mercury METHOD 1631E 5.00 5.09 102 77-123

K1509368ICP.JB1 - OPR (lcsw) (2) 09/09/15 Page No.:

Page 121 of 196

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ALS Group USA, Corp.dba ALS Environmental

QA/QC Report

Client: Grays Harbor Energy, LLC Service Request: K1509368

Project: GHEC NPDES Date Collected: NALCS Matrix: Water Date Received: NA

Date Extracted: NADate Analyzed: 09/08/15

Quality Control Sample (QCS) SummaryTotal Metals

Sample Name: Quality Control Sample Units: ng/L

Basis: NA

Test Notes:

ALSPercent

RecoveryPrep Analysis True Percent Acceptance Result

Analyte Method Method Value Result Recovery Limits Notes

Mercury METHOD 1631E 5.00 4.69 94 77-123

K1509368ICP.JB1 - QCS (icv) 09/09/15 Page No.:

Page 122 of 196

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- 1 - INORGANIC ANALYSIS DATA PACKAGE

ALS Group USA, Corp.

Metals

dba ALS Environmental

C QAnalyte

Grays Harbor Energy, LLCClient:

Project No.:

Service Request: K1509368

Matrix:

Lab Code: K1509368-001

Date Received:

Units:WATER ug/L

Project Name:

Sample Name:

Date Collected:

Basis: NA

NA

GHEC NPDES

08/26/15

08/26/15

PP

AnalysisMethod MRL

Dilution Factor

DateExtracted

DateAnalyzed ResultMDL

3.3Chromium 7195/70 2.0 1.0 08/26/15 09/01/150.6

Comments:

Form I - IN

Page 123 of 196

Page 124: Grays Harbor Energy, LLC 401 Keys Road

- 1 - INORGANIC ANALYSIS DATA PACKAGE

ALS Group USA, Corp.

Metals

dba ALS Environmental

C QAnalyte

Grays Harbor Energy, LLCClient:

Project No.:

Service Request: K1509368

Matrix:

Lab Code: KQ1509526-01

Date Received:

Units:WATER ug/L

Project Name:

Sample Name:

Date Collected:

Basis: NA

NA

GHEC NPDES

Method Blank

AnalysisMethod MRL

Dilution Factor

DateExtracted

DateAnalyzed ResultMDL

0.6Chromium U7195/70 2.0 1.0 08/26/15 09/01/150.6

Comments:

Form I - IN

Page 124 of 196

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- 5A - SPIKE SAMPLE RECOVERY

ALS Group USA, Corp.

Metals

dba ALS Environmental

Analyte Spike Result QC Method

ControlLimit %R %R

C

PPSSample Name: Lab Code: K1509368-001S

Client: Grays Harbor Energy, LLC

Project No.:

Service Request: K1509368

Matrix:

Units:

WATER

UG/L

Basis: NA

NA

GHEC NPDESProject Name:

SampleResult

SpikeAdded

3.375 - 125 12.0 10 87.0Chromium 7195/7010

Form V (PART 1) - IN

An empty field in the Control Limit column indicates the control limit is not applicable

Page 125 of 196

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- 6 -DUPLICATES

ALS Group USA, Corp.

Metals

dba ALS Environmental

Analyte Sample (S) QC MethodControlLimit RPDC Duplicate (D)

PPDSample Name: Lab Code: K1509368-001D

Client: Grays Harbor Energy, LLC

Project No.:

Service Request: K1509368

Matrix:

Units:

WATER

UG/L

Basis: NA

NA

GHEC NPDESProject Name:

3.53.3 5.9Chromium 7195/7010

Form VI - IN

An empty field in the Control Limit column indicates the control limit is not applicable.

Page 126 of 196

Page 127: Grays Harbor Energy, LLC 401 Keys Road

- 7 -LABORATORY CONTROL SAMPLE

ALS Group USA, Corp.

Metals

dba ALS Environmental

Analyte

Solid LCS Source:Aqueous LCS Source:

%R

Solid (mg/kg)

True Found %R True Found

Aqueous (ug/L)

C Limits

ALS MIXED

Client: Grays Harbor Energy, LLC

Project No.:

Project Name:

NA

GHEC NPDES

K1509368Service Request:

8.810 88.0Chromium

Form VII - IN

Page 127 of 196

Page 128: Grays Harbor Energy, LLC 401 Keys Road

Client:

08/26/15 13:30

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15 07:45

Dissolved Metals

Basis: NA

Analysis MethodAnalyte Name QDate Analyzed Date ExtractedDil.MDLMRLResult Units

Sample Name: PPLab Code: K1509368-001

Arsenic 08/31/15 07:23 08/28/1510.050.5015.9200.8 ug/L

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

Printed 09/10/15 11:15:16 AM Superset Reference:

Page 128 of 196

Page 129: Grays Harbor Energy, LLC 401 Keys Road

Client:

08/26/15 13:30

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: 08/26/15 07:45

Total Metals

Basis: NA

Analysis MethodAnalyte Name QDate Analyzed Date ExtractedDil.MDLMRLResult Units

Sample Name: PPLab Code: K1509368-001

Aluminum 08/31/15 07:06 08/28/1510.22.08.7200.8 ug/LAntimony 08/31/15 07:06 08/28/1510.0100.0500.710200.8 ug/LArsenic 08/31/15 07:06 08/28/1510.050.5016.8200.8 ug/LBarium 08/31/15 07:06 08/28/1510.0050.05014.0200.8 ug/LBeryllium 08/31/15 07:06 08/28/1510.0080.020 UND200.8 ug/LBoron 08/31/15 07:06 08/28/1510.071.049.3200.8 ug/LCadmium 08/31/15 07:06 08/28/1510.0050.020 J0.015200.8 ug/LChromium 08/31/15 07:06 08/28/1510.020.205.77200.8 ug/LCobalt 08/31/15 07:06 08/28/1510.0060.0200.027200.8 ug/LCopper 08/31/15 07:06 08/28/1510.030.102.28200.8 ug/LIron 09/04/15 02:38 09/01/15132068200.7 ug/LLead 08/31/15 07:06 08/28/1510.0020.0200.028200.8 ug/LMagnesium 09/04/15 02:38 09/01/1510.25.037600200.7 ug/LManganese 08/31/15 07:06 08/28/1510.0060.0501.12200.8 ug/LMolybdenum 08/31/15 07:06 08/28/1510.0080.0503.06200.8 ug/LNickel 08/31/15 07:06 08/28/1510.040.200.95200.8 ug/LPhosphorus 09/04/15 02:38 09/01/1516402820200.7 ug/LSelenium 08/31/15 07:06 08/28/1510.41.01.3200.8 ug/LSilver 08/31/15 07:06 08/28/1510.0050.020 UND200.8 ug/LThallium 08/31/15 07:06 08/28/1510.0020.020 UND200.8 ug/LTin 08/31/15 07:06 08/28/1510.0100.050 J0.011200.8 ug/LTitanium 09/04/15 02:38 09/01/1510.42.02.3200.7 ug/LZinc 08/31/15 07:06 08/28/1510.090.506.31200.8 ug/L

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

Printed 09/10/15 11:15:16 AM Superset Reference:

Page 129 of 196

Page 130: Grays Harbor Energy, LLC 401 Keys Road

Client:

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: NA

Total Metals

Basis: NA

Analysis MethodAnalyte Name QDate Analyzed Date ExtractedDil.MDLMRLResult Units

Sample Name: Method BlankLab Code: KQ1509714-01

Iron 09/04/15 02:32 09/01/151320 J5200.7 ug/LMagnesium 09/04/15 02:32 09/01/1510.25.0 J4.0200.7 ug/LPhosphorus 09/04/15 02:32 09/01/151640 UND200.7 ug/LTitanium 09/04/15 02:32 09/01/1510.42.0 UND200.7 ug/L

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

Printed 09/10/15 11:15:16 AM Superset Reference:

Page 130 of 196

Page 131: Grays Harbor Energy, LLC 401 Keys Road

Client:

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project: NA

Total Metals

Basis: NA

Analysis MethodAnalyte Name QDate Analyzed Date ExtractedDil.MDLMRLResult Units

Sample Name: Method BlankLab Code: KQ1509607-01

Aluminum 08/31/15 05:47 08/28/1510.22.0 J0.2200.8 ug/LAntimony 08/31/15 05:47 08/28/1510.0100.050 UND200.8 ug/LArsenic 08/31/15 05:47 08/28/1510.050.50 UND200.8 ug/LBarium 08/31/15 05:47 08/28/1510.0050.050 J0.021200.8 ug/LBeryllium 08/31/15 05:47 08/28/1510.0080.020 UND200.8 ug/LBoron 08/31/15 05:47 08/28/1510.071.0 J0.09200.8 ug/LCadmium 08/31/15 05:47 08/28/1510.0050.020 UND200.8 ug/LChromium 08/31/15 05:47 08/28/1510.020.20 UND200.8 ug/LCobalt 08/31/15 05:47 08/28/1510.0060.020 UND200.8 ug/LCopper 08/31/15 05:47 08/28/1510.030.10 UND200.8 ug/LLead 08/31/15 05:47 08/28/1510.0020.020 UND200.8 ug/LManganese 08/31/15 05:47 08/28/1510.0060.050 UND200.8 ug/LMolybdenum 08/31/15 05:47 08/28/1510.0080.050 UND200.8 ug/LNickel 08/31/15 05:47 08/28/1510.040.20 UND200.8 ug/LSelenium 08/31/15 05:47 08/28/1510.41.0 UND200.8 ug/LSilver 08/31/15 05:47 08/28/1510.0050.020 UND200.8 ug/LThallium 08/31/15 05:47 08/28/1510.0020.020 UND200.8 ug/LTin 08/31/15 05:47 08/28/1510.0100.050 UND200.8 ug/LZinc 08/31/15 05:47 08/28/1510.090.50 UND200.8 ug/L

Analytical Report

ALS Group USA, Corp. dba ALS Environmental

Printed 09/10/15 11:15:17 AM Superset Reference:

Page 131 of 196

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

08/26/15Date Collected:Date Received: 08/26/15

09/04/15Date Analyzed:

Replicate Sample SummaryTotal Metals

PP ug/LBasis:Units:

K1509368-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

KQ1509714-03 Result Average

SampleResultAnalyte Name

dba ALS Environmental

Iron 7 20 3 68 63 65 20200.7Magnesium 2 5.0 0.2 37600 36800 37200 20200.7Phosphorus 2 40 6 2820 2770 2790 20200.7Titanium 39 2.0 0.4 2.3 3.4 2.9 20200.7

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

Printed 09/10/15 11:15:17 AM Superset Reference:

Page 132 of 196

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ALS Group USA, Corp.

QA/QC Report

Client:ProjectSample Matrix: Water

GHEC NPDESGrays Harbor Energy, LLC Service Request: K1509368

08/26/15Date Collected:Date Received: 08/26/15

08/31/15Date Analyzed:

Replicate Sample SummaryTotal Metals

PP ug/LBasis:Units:

K1509368-001 NALab Code:Sample Name:

RPD LimitMRL MDLAnalysis Method RPD

Duplicate Sample

KQ1509607-03 Result Average

SampleResultAnalyte Name

dba ALS Environmental

Aluminum <1 2.0 0.2 8.7 8.6 8.6 20200.8Antimony <1 0.050 0.010 0.710 0.712 0.711 20200.8Arsenic 2 0.50 0.05 16.8 16.4 16.6 20200.8Barium 4 0.050 0.005 14.0 13.5 13.8 20200.8Beryllium - 0.020 0.008 ND U ND U ND 20200.8Boron <1 1.0 0.07 49.3 49.0 49.1 20200.8Cadmium NC 0.020 0.005 0.015 J ND U NC 20200.8Chromium 5 0.20 0.02 5.77 5.50 5.64 20200.8Cobalt 24 0.020 0.006 0.027 0.035 0.031 20200.8Copper 4 0.10 0.03 2.28 2.19 2.23 20200.8Lead 13 0.020 0.002 0.028 0.024 0.026 20200.8Manganese 4 0.050 0.006 1.12 1.08 1.10 20200.8Molybdenum 2 0.050 0.008 3.06 3.00 3.03 20200.8Nickel 4 0.20 0.04 0.95 0.91 0.93 20200.8Selenium 9 1.0 0.4 1.3 1.2 1.2 20200.8Silver - 0.020 0.005 ND U ND U ND 20200.8Thallium - 0.020 0.002 ND U ND U ND 20200.8Tin 29 0.050 0.010 0.011 J 0.015 J 0.013 20200.8Zinc 5 0.50 0.09 6.31 6.00 6.15 20200.8

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

Printed 09/10/15 11:15:17 AM Superset Reference:

Page 133 of 196

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QA/QC Report

ug/LK1509368-001 Basis:Lab Code:

Units:Sample Name: PP

Total MetalsMatrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

09/4/1508/26/15

Date Collected: 08/26/15

EPA CLP-METALS ILM04.0200.7

Prep Method:Analysis Method:

Analyte Name ResultSample Result Spike Amount % Rec

Matrix SpikeKQ1509714-04

% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

09/1/15Date Extracted:

Iron 68 1060 1000 99 70-130Magnesium 37600 46700 10000 91 70-130Phosphorus 2820 13100 10000 103 70-130Titanium 2.3 10000 10000 100 70-130

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

Printed 09/10/15 11:15:17 AM Superset Reference:

Page 134 of 196

Page 135: Grays Harbor Energy, LLC 401 Keys Road

QA/QC Report

ug/LK1509368-001 Basis:Lab Code:

Units:Sample Name: PP

Total MetalsMatrix Spike Summary

NA

Client:Project:Sample Matrix:

Grays Harbor Energy, LLCGHEC NPDESWater

Service Request:

Date Analyzed:Date Received:

K1509368

08/31/1508/26/15

Date Collected: 08/26/15

EPA CLP-METALS ILM04.0200.8

Prep Method:Analysis Method:

Analyte Name ResultSample Result Spike Amount % Rec

Matrix SpikeKQ1509607-04

% Rec Limits

ALS Group USA, Corp.dba ALS Environmental

08/28/15Date Extracted:

Aluminum 8.7 97.7 100 89 70-130Antimony 0.710 52.3 50.0 103 70-130Arsenic 16.8 66.4 50.0 99 70-130Barium 14.0 120 100 106 70-130Beryllium ND U 2.39 2.50 95 70-130Cadmium 0.015 J 23.3 25.0 93 70-130Chromium 5.77 16.1 10.0 104 70-130Cobalt 0.027 26.1 25.0 104 70-130Copper 2.28 13.4 12.5 89 70-130Lead 0.028 43.9 50.0 88 70-130Manganese 1.12 24.6 25.0 94 70-130Molybdenum 3.06 25.7 20.0 113 70-130Nickel 0.95 25.5 25.0 98 70-130Selenium 1.3 55.0 50.0 107 70-130Silver ND U 9.73 12.5 78 70-130Thallium ND U 45.7 50.0 91 70-130Zinc 6.31 27.1 25.0 83 70-130

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

Printed 09/10/15 11:15:18 AM Superset Reference:

Page 135 of 196

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Lab Control SampleKQ1509714-02

Analyte Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryTotal Metals

Analysis Method:Prep Method:

200.7EPA CLP-METALS ILM04.0 NA

ug/LBasis:Units:

Analysis Lot: 460939

09/04/15

Spike AmountResult % Rec % Rec Limits

09/01/15Date Extracted:

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Iron 85-115101 25002530Magnesium 85-115104 1250013100Phosphorus 85-115101 1000010100Titanium 85-11599 100009920

Superset Reference:Printed 09/10/15 11:15:17 AM

Page 136 of 196

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Lab Control SampleKQ1509607-02

Analyte Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Lab Control Sample SummaryTotal Metals

Analysis Method:Prep Method:

200.8EPA CLP-METALS ILM04.0 NA

ug/LBasis:Units:

Analysis Lot: 460276

08/31/15

Spike AmountResult % Rec % Rec Limits

08/28/15Date Extracted:

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

Aluminum 85-11596 10096.3Antimony 85-115103 50.051.3Arsenic 85-11599 50.049.4Barium 85-115100 100100Beryllium 85-115100 2.502.51Cadmium 85-115101 25.025.3Chromium 85-115100 10.09.98Cobalt 85-11598 25.024.6Copper 85-11598 12.512.2Lead 85-11598 50.049.2Manganese 85-11594 25.023.5Molybdenum 85-115102 20.020.3Nickel 85-11599 25.024.8Selenium 85-115108 50.054.1Silver 85-11588 12.511.0Thallium 85-115102 50.051.0Zinc 85-115100 25.025.0

Superset Reference:Printed 09/10/15 11:15:17 AM

Page 137 of 196

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Organochlorine Pesticides and Polychlorinated Biphenyls

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 138 of 196

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Analytical Results

Grays Harbor Energy, LLC K1509368

K1509368-001

ug/L

NA

PP

08/26/2015

08/26/2015

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Organochlorine Pesticides and Polychlorinated Biphenyls

Lab Code:

Level: LowExtraction Method:

Analysis Method:

EPA 3520C

608

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

0.013 08/31/151 KWG150823709/09/150.00080UNDalpha-BHC

0.013 08/31/151 KWG150823709/09/150.00097UNDbeta-BHC

0.013 08/31/151 KWG150823709/09/150.0025UNDgamma-BHC (Lindane)

0.013 08/31/151 KWG150823709/09/150.0043UNDdelta-BHC

0.013 08/31/151 KWG150823709/09/150.0013UNDHeptachlor

0.013 08/31/151 KWG150823709/09/150.0021UNDAldrin

0.013 08/31/151 KWG150823709/09/150.0013UNDHeptachlor Epoxide

0.013 08/31/151 KWG150823709/10/150.0016UNDEndosulfan I

0.013 08/31/151 KWG150823709/09/150.0011UNDDieldrin

0.013 08/31/151 KWG150823709/09/150.0014UND4,4'-DDE

0.013 08/31/151 KWG150823709/10/150.0016UNDEndrin

0.013 08/31/151 KWG150823709/09/150.0013UNDEndosulfan II

0.013 08/31/151 KWG150823709/09/150.0019UND4,4'-DDD

0.013 08/31/151 KWG150823709/09/150.0021UNDEndrin Aldehyde

0.013 08/31/151 KWG150823709/09/150.0015UNDEndosulfan Sulfate

0.013 08/31/151 KWG150823709/09/150.0022UND4,4'-DDT

0.61 08/31/151 KWG150823709/09/150.11UNDToxaphene

0.25 08/31/151 KWG150823709/09/150.026UNDChlordane

0.061 08/31/151 KWG150823709/09/150.053UNDAroclor 1016

0.13 08/31/151 KWG150823709/09/150.071UNDAroclor 1221

0.13 08/31/151 KWG150823709/09/150.060UNDAroclor 1232

0.13 08/31/151 KWG150823709/09/150.022UNDAroclor 1242

0.13 08/31/151 KWG150823709/09/150.043UNDAroclor 1248

0.13 08/31/151 KWG150823709/09/150.036UNDAroclor 1254

0.13 08/31/151 KWG150823709/09/150.065UNDAroclor 1260

Surrogate Name %Rec

Control

Limits NoteDate

Analyzed

10-134 AcceptableDecachlorobiphenyl 09/09/1576

Comments:

1of1Page15:08:0609/11/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181667u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 139 of 196

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Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508237-4

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Organochlorine Pesticides and Polychlorinated Biphenyls

Lab Code:

Level: LowExtraction Method:

Analysis Method:

EPA 3520C

608

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

0.0095 08/31/151 KWG150823709/09/150.00065UNDalpha-BHC

0.0095 08/31/151 KWG150823709/09/150.00079UNDbeta-BHC

0.0095 08/31/151 KWG150823709/09/150.0020UNDgamma-BHC (Lindane)

0.0095 08/31/151 KWG150823709/09/150.0035UNDdelta-BHC

0.0095 08/31/151 KWG150823709/09/150.0010UNDHeptachlor

0.0095 08/31/151 KWG150823709/09/150.0017UNDAldrin

0.0095 08/31/151 KWG150823709/09/150.0010UNDHeptachlor Epoxide

0.0095 08/31/151 KWG150823709/10/150.0013UNDEndosulfan I

0.0095 08/31/151 KWG150823709/09/150.00085UNDDieldrin

0.0095 08/31/151 KWG150823709/09/150.0011UND4,4'-DDE

0.0095 08/31/151 KWG150823709/10/150.0013UNDEndrin

0.0095 08/31/151 KWG150823709/09/150.0010UNDEndosulfan II

0.0095 08/31/151 KWG150823709/09/150.0015UND4,4'-DDD

0.0095 08/31/151 KWG150823709/09/150.0017UNDEndrin Aldehyde

0.0095 08/31/151 KWG150823709/09/150.0012UNDEndosulfan Sulfate

0.0095 08/31/151 KWG150823709/09/150.0018UND4,4'-DDT

0.48 08/31/151 KWG150823709/09/150.083UNDToxaphene

0.19 08/31/151 KWG150823709/09/150.021UNDChlordane

0.048 08/31/151 KWG150823709/09/150.043UNDAroclor 1016

0.095 08/31/151 KWG150823709/09/150.058UNDAroclor 1221

0.095 08/31/151 KWG150823709/09/150.049UNDAroclor 1232

0.095 08/31/151 KWG150823709/09/150.018UNDAroclor 1242

0.095 08/31/151 KWG150823709/09/150.035UNDAroclor 1248

0.095 08/31/151 KWG150823709/09/150.029UNDAroclor 1254

0.095 08/31/151 KWG150823709/09/150.053UNDAroclor 1260

Surrogate Name %Rec

Control

Limits NoteDate

Analyzed

10-134 AcceptableDecachlorobiphenyl 09/09/1552

Comments:

1of1Page15:08:1009/11/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181667u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 140 of 196

Page 141: Grays Harbor Energy, LLC 401 Keys Road

ALS Group USA, Corp. dba ALS Environmental

Extraction Method:

QA/QC Report

Surrogate Recovery Summary

Grays Harbor Energy, LLC K1509368

Low

Water

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Units:

Level:

Sample Name Lab Code

Organochlorine Pesticides and Polychlorinated Biphenyls

EPA 3520C

Analysis Method: 608

Sur1

Percent

K1509368-001PP 76

KWG1508237-4Method Blank 52

KWG1508237-1PPMS 78

KWG1508237-2PPDMS 75

KWG1508237-3Lab Control Sample 78

Form 2A - OrganicPrinted: 09/11/2015 15:08:15 1 of 1

Surrogate Recovery Control Limits (%)

10-134Decachlorobiphenyl

Results flagged with an asterisk (*) indicate values outside control criteria.

Page

Results flagged with a pound (#) indicate the control criteria is not applicable.

RR181667SuperSet Reference:

Sur1 =

u:\Stealth\Crystal.rpt\Form2.rpt

Page 141 of 196

Page 142: Grays Harbor Energy, LLC 401 Keys Road

Matrix Spike/Duplicate Matrix Spike Summary

Sample

Result %Rec

Matrix Spike

%Rec

Limits

Duplicate Matrix Spike

%Rec RPD

RPD

Limit

QA/QC Report

Grays Harbor Energy, LLC

PP

K1509368-001

608

K1509368

ug/L

NA

Organochlorine Pesticides and Polychlorinated Biphenyls

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Sample Name:

Lab Code:

Extraction Method:

Analysis Method:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result Result

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed:

08/31/2015

09/09/2015 -

09/10/2015

EPA 3520C

KWG1508237

KWG1508237-2KWG1508237-1

PPMS PPDMS

Spike

Amount

Spike

Amount

37-134ND 0.106 68alpha-BHC 0.109 70 3040.0760 0.0726

17-147ND 0.106 67beta-BHC 0.109 61 3070.0660 0.0708

32-127ND 0.106 70gamma-BHC (Lindane) 0.109 74 3070.0800 0.0744

19-140ND 0.106 68delta-BHC 0.109 72 3080.0786 0.0723

34-111ND 0.106 62Heptachlor 0.109 66 3080.0721 0.0664

42-122ND 0.106 70Aldrin 0.109 72 3060.0782 0.0739

37-142ND 0.106 70Heptachlor Epoxide 0.109 73 3060.0798 0.0749

45-153ND 0.106 63Endosulfan I 0.109 69 30120.0750 0.0668

36-146ND 0.106 80Dieldrin 0.109 83 3060.0901 0.0852

30-145ND 0.106 814,4'-DDE 0.109 84 3050.0908 0.0862

30-147ND 0.106 73Endrin 0.109 82 30130.0886 0.0778

10-202ND 0.106 72Endosulfan II 0.109 79 30120.0859 0.0765

31-141ND 0.106 844,4'-DDD 0.109 87 3050.0941 0.0894

43-125ND 0.106 78Endrin Aldehyde 0.109 89 30160.0969 0.0828

26-144ND 0.106 80Endosulfan Sulfate 0.109 86 3090.0936 0.0853

25-160ND 0.106 854,4'-DDT 0.109 93 30110.102 0.0907

Form 3A - OrganicPrinted: 09/11/2015 15:08:19 Page 1 of 1

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

RR181667SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3DMS.rpt

Page 142 of 196

Page 143: Grays Harbor Energy, LLC 401 Keys Road

Lab Control Spike Summary

%Rec

Lab Control Spike

%Rec

Limits

QA/QC Report

Grays Harbor Energy, LLC K1509368

608

ug/L

NA

Lab Control Sample

KWG1508237-3

Organochlorine Pesticides and Polychlorinated Biphenyls

KWG1508237

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result

Extraction Method:

Analysis Method:

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed: 09/09/2015 -

09/10/2015

08/31/2015

EPA 3520C

Spike

Amount

37-134alpha-BHC 0.100 730.0733

17-147beta-BHC 0.100 730.0728

32-127gamma-BHC (Lindane) 0.100 740.0743

19-140delta-BHC 0.100 740.0743

34-111Heptachlor 0.100 660.0659

42-122Aldrin 0.100 750.0755

37-142Heptachlor Epoxide 0.100 810.0810

45-153Endosulfan I 0.100 730.0730

36-146Dieldrin 0.100 900.0900

30-1454,4'-DDE 0.100 940.0938

30-147Endrin 0.100 840.0844

10-202Endosulfan II 0.100 870.0874

31-1414,4'-DDD 0.100 920.0924

43-125Endrin Aldehyde 0.100 850.0847

26-144Endosulfan Sulfate 0.100 970.0970

25-1604,4'-DDT 0.100 900.0901

Form 3C - OrganicPrinted: 09/11/2015 15:08:23 Page 1 of 1

Results flagged with an asterisk (*) indicate values outside control criteria.

RR181667SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3LCS.rpt

Page 143 of 196

Page 144: Grays Harbor Energy, LLC 401 Keys Road

Volatile Organic Compounds

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 144 of 196

Page 145: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

K1509368-001

ug/L

NA

PP

08/26/2015

08/26/2015

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Volatile Organic Compounds

Lab Code:

Level: LowExtraction Method:

Analysis Method:

METHOD

624

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

5.0 09/04/151 KWG150850209/04/150.030UNDChloromethane

5.0 09/04/151 KWG150850209/04/150.031UNDVinyl Chloride

5.0 09/04/151 KWG150850209/04/150.072UNDBromomethane

5.0 09/04/151 KWG150850209/04/150.14UNDChloroethane

5.0 09/04/151 KWG150850209/04/150.080UNDTrichlorofluoromethane

5.0 09/04/151 KWG150850209/04/150.039UND1,1-Dichloroethene

5.0 09/04/151 KWG150850209/04/150.14UNDMethylene Chloride

5.0 09/04/151 KWG150850209/04/150.032UNDtrans-1,2-Dichloroethene

5.0 09/04/151 KWG150850209/04/150.025UND1,1-Dichloroethane

5.0 09/04/151 KWG150850209/04/150.062J0.11Chloroform

5.0 09/04/151 KWG150850209/04/150.057UND1,1,1-Trichloroethane (TCA)

5.0 09/04/151 KWG150850209/04/150.12UNDCarbon Tetrachloride

5.0 09/04/151 KWG150850209/04/150.031UNDBenzene

5.0 09/04/151 KWG150850209/04/150.036UND1,2-Dichloroethane (EDC)

5.0 09/04/151 KWG150850209/04/150.044UNDTrichloroethene (TCE)

5.0 09/04/151 KWG150850209/04/150.044UND1,2-Dichloropropane

5.0 09/04/151 KWG150850209/04/150.086UNDBromodichloromethane

10 09/04/151 KWG150850209/04/150.12UND2-Chloroethyl Vinyl Ether

5.0 09/04/151 KWG150850209/04/150.045UNDtrans-1,3-Dichloropropene

5.0 09/04/151 KWG150850209/04/150.032UNDToluene

5.0 09/04/151 KWG150850209/04/150.035UNDcis-1,3-Dichloropropene

5.0 09/04/151 KWG150850209/04/150.045UND1,1,2-Trichloroethane

5.0 09/04/151 KWG150850209/04/150.032UNDTetrachloroethene (PCE)

5.0 09/04/151 KWG150850209/04/150.081UNDDibromochloromethane

5.0 09/04/151 KWG150850209/04/150.031UNDChlorobenzene

5.0 09/04/151 KWG150850209/04/150.030UNDEthylbenzene

5.0 09/04/151 KWG150850209/04/150.17UNDBromoform

5.0 09/04/151 KWG150850209/04/150.092UND1,1,2,2-Tetrachloroethane

5.0 09/04/151 KWG150850209/04/150.071UND1,3-Dichlorobenzene

5.0 09/04/151 KWG150850209/04/150.073UND1,4-Dichlorobenzene

5.0 09/04/151 KWG150850209/04/150.086UND1,2-Dichlorobenzene

50 09/04/151 KWG150850209/04/153.7UNDAcrolein†

10 09/04/151 KWG150850209/04/150.14UNDAcrylonitrile†

Comments:

2of1Page13:10:2309/17/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181838u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 145 of 196

Page 146: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

K1509368-001

ug/L

NA

PP

08/26/2015

08/26/2015

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Volatile Organic Compounds

Lab Code:

Surrogate Name %Rec

Control

Limits NoteDate

Analyzed

80-120 AcceptableToluene-d8 09/04/15102

68-120 Acceptable4-Bromofluorobenzene 09/04/1598

76-132 AcceptableDibromofluoromethane 09/04/1595

† Analyte Comments

This compound is unstable under normal conditions. As per EPA Method 624 guidelines, the reported value was an estimate.Acrolein

This compound is unstable under normal conditions. As per EPA Method 624 guidelines, the reported value was an estimate.Acrylonitrile

Comments:

2of2Page13:10:2309/17/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181838u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 146 of 196

Page 147: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508502-4

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Volatile Organic Compounds

Lab Code:

Level: LowExtraction Method:

Analysis Method:

METHOD

624

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

5.0 09/04/151 KWG150850209/04/150.030UNDChloromethane

5.0 09/04/151 KWG150850209/04/150.031UNDVinyl Chloride

5.0 09/04/151 KWG150850209/04/150.072UNDBromomethane

5.0 09/04/151 KWG150850209/04/150.14UNDChloroethane

5.0 09/04/151 KWG150850209/04/150.080UNDTrichlorofluoromethane

5.0 09/04/151 KWG150850209/04/150.039UND1,1-Dichloroethene

5.0 09/04/151 KWG150850209/04/150.14UNDMethylene Chloride

5.0 09/04/151 KWG150850209/04/150.032UNDtrans-1,2-Dichloroethene

5.0 09/04/151 KWG150850209/04/150.025UND1,1-Dichloroethane

5.0 09/04/151 KWG150850209/04/150.062UNDChloroform

5.0 09/04/151 KWG150850209/04/150.057UND1,1,1-Trichloroethane (TCA)

5.0 09/04/151 KWG150850209/04/150.12UNDCarbon Tetrachloride

5.0 09/04/151 KWG150850209/04/150.031UNDBenzene

5.0 09/04/151 KWG150850209/04/150.036UND1,2-Dichloroethane (EDC)

5.0 09/04/151 KWG150850209/04/150.044UNDTrichloroethene (TCE)

5.0 09/04/151 KWG150850209/04/150.044UND1,2-Dichloropropane

5.0 09/04/151 KWG150850209/04/150.086UNDBromodichloromethane

10 09/04/151 KWG150850209/04/150.12UND2-Chloroethyl Vinyl Ether

5.0 09/04/151 KWG150850209/04/150.045UNDtrans-1,3-Dichloropropene

5.0 09/04/151 KWG150850209/04/150.032UNDToluene

5.0 09/04/151 KWG150850209/04/150.035UNDcis-1,3-Dichloropropene

5.0 09/04/151 KWG150850209/04/150.045UND1,1,2-Trichloroethane

5.0 09/04/151 KWG150850209/04/150.032UNDTetrachloroethene (PCE)

5.0 09/04/151 KWG150850209/04/150.081UNDDibromochloromethane

5.0 09/04/151 KWG150850209/04/150.031UNDChlorobenzene

5.0 09/04/151 KWG150850209/04/150.030UNDEthylbenzene

5.0 09/04/151 KWG150850209/04/150.17UNDBromoform

5.0 09/04/151 KWG150850209/04/150.092UND1,1,2,2-Tetrachloroethane

5.0 09/04/151 KWG150850209/04/150.071UND1,3-Dichlorobenzene

5.0 09/04/151 KWG150850209/04/150.073UND1,4-Dichlorobenzene

5.0 09/04/151 KWG150850209/04/150.086UND1,2-Dichlorobenzene

50 09/04/151 KWG150850209/04/153.7UNDAcrolein†

10 09/04/151 KWG150850209/04/150.14UNDAcrylonitrile†

Comments:

2of1Page13:10:2709/17/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181838u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 147 of 196

Page 148: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508502-4

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Volatile Organic Compounds

Lab Code:

Surrogate Name %Rec

Control

Limits NoteDate

Analyzed

80-120 AcceptableToluene-d8 09/04/15102

68-120 Acceptable4-Bromofluorobenzene 09/04/15102

76-132 AcceptableDibromofluoromethane 09/04/1597

† Analyte Comments

This compound is unstable under normal conditions. As per EPA Method 624 guidelines, the reported value was an estimate.Acrolein

This compound is unstable under normal conditions. As per EPA Method 624 guidelines, the reported value was an estimate.Acrylonitrile

Comments:

2of2Page13:10:2709/17/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181838u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 148 of 196

Page 149: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508530-4

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Volatile Organic Compounds

Lab Code:

Level: LowExtraction Method:

Analysis Method:

METHOD

624

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

5.0 09/05/151 KWG150853009/05/150.030UNDChloromethane

5.0 09/05/151 KWG150853009/05/150.031UNDVinyl Chloride

5.0 09/05/151 KWG150853009/05/150.072UNDBromomethane

5.0 09/05/151 KWG150853009/05/150.14UNDChloroethane

5.0 09/05/151 KWG150853009/05/150.080UNDTrichlorofluoromethane

5.0 09/05/151 KWG150853009/05/150.039UND1,1-Dichloroethene

5.0 09/05/151 KWG150853009/05/150.14UNDMethylene Chloride

5.0 09/05/151 KWG150853009/05/150.032UNDtrans-1,2-Dichloroethene

5.0 09/05/151 KWG150853009/05/150.025UND1,1-Dichloroethane

5.0 09/05/151 KWG150853009/05/150.062J0.080Chloroform

5.0 09/05/151 KWG150853009/05/150.057UND1,1,1-Trichloroethane (TCA)

5.0 09/05/151 KWG150853009/05/150.12UNDCarbon Tetrachloride

5.0 09/05/151 KWG150853009/05/150.031UNDBenzene

5.0 09/05/151 KWG150853009/05/150.036UND1,2-Dichloroethane (EDC)

5.0 09/05/151 KWG150853009/05/150.044UNDTrichloroethene (TCE)

5.0 09/05/151 KWG150853009/05/150.044UND1,2-Dichloropropane

5.0 09/05/151 KWG150853009/05/150.086UNDBromodichloromethane

10 09/05/151 KWG150853009/05/150.12UND2-Chloroethyl Vinyl Ether

5.0 09/05/151 KWG150853009/05/150.045UNDtrans-1,3-Dichloropropene

5.0 09/05/151 KWG150853009/05/150.032UNDToluene

5.0 09/05/151 KWG150853009/05/150.035UNDcis-1,3-Dichloropropene

5.0 09/05/151 KWG150853009/05/150.045UND1,1,2-Trichloroethane

5.0 09/05/151 KWG150853009/05/150.032UNDTetrachloroethene (PCE)

5.0 09/05/151 KWG150853009/05/150.081UNDDibromochloromethane

5.0 09/05/151 KWG150853009/05/150.031UNDChlorobenzene

5.0 09/05/151 KWG150853009/05/150.030UNDEthylbenzene

5.0 09/05/151 KWG150853009/05/150.17U *NDBromoform

5.0 09/05/151 KWG150853009/05/150.092UND1,1,2,2-Tetrachloroethane

5.0 09/05/151 KWG150853009/05/150.071UND1,3-Dichlorobenzene

5.0 09/05/151 KWG150853009/05/150.073UND1,4-Dichlorobenzene

5.0 09/05/151 KWG150853009/05/150.086UND1,2-Dichlorobenzene

50 09/05/151 KWG150853009/05/153.7U *NDAcrolein†

10 09/05/151 KWG150853009/05/150.14UNDAcrylonitrile†

Comments:

2of1Page13:10:3109/17/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181838u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 149 of 196

Page 150: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508530-4

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Volatile Organic Compounds

Lab Code:

* See Case Narrative

Surrogate Name %Rec

Control

Limits NoteDate

Analyzed

80-120 AcceptableToluene-d8 09/05/15100

68-120 Acceptable4-Bromofluorobenzene 09/05/1584

76-132 AcceptableDibromofluoromethane 09/05/1583

† Analyte Comments

This compound is unstable under normal conditions. As per EPA Method 624 guidelines, the reported value was an estimate.Acrolein

This compound is unstable under normal conditions. As per EPA Method 624 guidelines, the reported value was an estimate.Acrylonitrile

Comments:

2of2Page13:10:3109/17/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR181838u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 150 of 196

Page 151: Grays Harbor Energy, LLC 401 Keys Road

ALS Group USA, Corp. dba ALS Environmental

Extraction Method:

QA/QC Report

Surrogate Recovery Summary

Grays Harbor Energy, LLC K1509368

Low

Water

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Units:

Level:

Sample Name Lab Code

Volatile Organic Compounds

METHOD

Analysis Method: 624

Sur1 Sur2 Sur3

Percent

K1509292-009Batch QC 101 100 97

K1509368-001PP 102 98 95

KWG1508502-4Method Blank 102 102 97

KWG1508530-4Method Blank 100 84 83

KWG1508502-1Batch QCMS 102 96 95

KWG1508502-2Batch QCDMS 99 98 94

KWG1508502-3Lab Control Sample 102 98 94

KWG1508530-3Lab Control Sample 108 86 90

Form 2A - OrganicPrinted: 09/17/2015 13:10:36 1 of 1

Surrogate Recovery Control Limits (%)

80-120

68-120

76-132

Toluene-d8

4-Bromofluorobenzene

Dibromofluoromethane

Results flagged with an asterisk (*) indicate values outside control criteria.

Page

Results flagged with a pound (#) indicate the control criteria is not applicable.

RR181838SuperSet Reference:

Sur1

Sur2

Sur3

=

=

=

u:\Stealth\Crystal.rpt\Form2.rpt

Page 151 of 196

Page 152: Grays Harbor Energy, LLC 401 Keys Road

Matrix Spike/Duplicate Matrix Spike Summary

Sample

Result %Rec

Matrix Spike

%Rec

Limits

Duplicate Matrix Spike

%Rec RPD

RPD

Limit

QA/QC Report

Grays Harbor Energy, LLC

Batch QC

K1509292-009

624

K1509368

ug/L

NA

Volatile Organic Compounds

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Sample Name:

Lab Code:

Extraction Method:

Analysis Method:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result Result

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed:

09/04/2015

09/04/2015

METHOD

KWG1508502

KWG1508502-2KWG1508502-1

Batch QCMS Batch QCDMS

Spike

Amount

Spike

Amount

10-234ND 10.0 1181,1-Dichloroethene 10.0 117 30111.7 11.8

37-1510.67 10.0 117Benzene 10.0 114 30312.0 12.4

71-157ND 10.0 111Trichloroethene (TCE) 10.0 113 30111.3 11.1

47-15016 10.0 115Toluene 10.0 103 30426.1 27.2

37-1600.080 10.0 121Chlorobenzene 10.0 115 30511.6 12.2

18-190ND 10.0 1161,2-Dichlorobenzene 10.0 112 30411.2 11.6

Form 3A - OrganicPrinted: 09/17/2015 13:10:40 Page 1 of 1

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

RR181838SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3DMS.rpt

Page 152 of 196

Page 153: Grays Harbor Energy, LLC 401 Keys Road

Lab Control Spike Summary

%Rec

Lab Control Spike

%Rec

Limits

QA/QC Report

Grays Harbor Energy, LLC K1509368

624

ug/L

NA

Lab Control Sample

KWG1508502-3

Volatile Organic Compounds

KWG1508502

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result

Extraction Method:

Analysis Method:

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed: 09/04/2015

09/04/2015

METHOD

Spike

Amount

10-273Chloromethane 10.0 10010.0

10-251Vinyl Chloride 10.0 10510.5

10-242Bromomethane 10.0 969.62

14-230Chloroethane 10.0 10810.8

17-181Trichlorofluoromethane 10.0 908.96

10-2341,1-Dichloroethene 10.0 979.73

10-221Methylene Chloride 10.0 888.78

54-156trans-1,2-Dichloroethene 10.0 969.59

59-1551,1-Dichloroethane 10.0 10810.8

51-138Chloroform 10.0 989.83

52-16210.0 979.741,1,1-Trichloroethane (TCA)

70-140Carbon Tetrachloride 10.0 989.75

37-151Benzene 10.0 10310.3

49-1551,2-Dichloroethane (EDC) 10.0 939.34

71-157Trichloroethene (TCE) 10.0 10110.1

10-2101,2-Dichloropropane 10.0 979.68

35-155Bromodichloromethane 10.0 939.33

10-3052-Chloroethyl Vinyl Ether 10.0 828.20

17-183trans-1,3-Dichloropropene 10.0 929.21

47-150Toluene 10.0 10110.1

10-227cis-1,3-Dichloropropene 10.0 979.65

52-1501,1,2-Trichloroethane 10.0 919.14

64-148Tetrachloroethene (PCE) 10.0 10610.6

53-149Dibromochloromethane 10.0 909.02

37-160Chlorobenzene 10.0 10610.6

37-162Ethylbenzene 10.0 10310.3

45-169Bromoform 10.0 908.96

46-1571,1,2,2-Tetrachloroethane 10.0 909.04

59-1561,3-Dichlorobenzene 10.0 10510.5

18-1901,4-Dichlorobenzene 10.0 10310.3

18-1901,2-Dichlorobenzene 10.0 989.79

27-200Acrolein 100 6261.7

61-141Acrylonitrile 10.0 908.98

Form 3C - OrganicPrinted: 09/17/2015 13:10:44 Page 1 of 1

Results flagged with an asterisk (*) indicate values outside control criteria.

RR181838SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3LCS.rpt

Page 153 of 196

Page 154: Grays Harbor Energy, LLC 401 Keys Road

Lab Control Spike Summary

%Rec

Lab Control Spike

%Rec

Limits

QA/QC Report

Grays Harbor Energy, LLC K1509368

624

ug/L

NA

Lab Control Sample

KWG1508530-3

Volatile Organic Compounds

KWG1508530

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result

Extraction Method:

Analysis Method:

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed: 09/05/2015

09/05/2015

METHOD

Spike

Amount

10-273Chloromethane 10.0 11111.1

10-251Vinyl Chloride 10.0 12212.2

10-242Bromomethane 10.0 807.97

14-230Chloroethane 10.0 13213.2

17-181Trichlorofluoromethane 10.0 10110.1

10-2341,1-Dichloroethene 10.0 10510.5

10-221Methylene Chloride 10.0 10610.6

54-156trans-1,2-Dichloroethene 10.0 10310.3

59-1551,1-Dichloroethane 10.0 10210.2

51-138Chloroform 10.0 10910.9

52-16210.0 979.711,1,1-Trichloroethane (TCA)

70-140Carbon Tetrachloride 10.0 939.30

37-151Benzene 10.0 10610.6

49-1551,2-Dichloroethane (EDC) 10.0 10810.8

71-157Trichloroethene (TCE) 10.0 10410.4

10-2101,2-Dichloropropane 10.0 999.86

35-155Bromodichloromethane 10.0 999.94

10-3052-Chloroethyl Vinyl Ether 10.0 919.07

17-183trans-1,3-Dichloropropene 10.0 757.49

47-150Toluene 10.0 11711.7

10-227cis-1,3-Dichloropropene 10.0 909.02

52-1501,1,2-Trichloroethane 10.0 939.34

64-148Tetrachloroethene (PCE) 10.0 10710.7

53-149Dibromochloromethane 10.0 767.55

37-160Chlorobenzene 10.0 10510.5

37-162Ethylbenzene 10.0 10810.8

45-169Bromoform 10.0 666.59

46-1571,1,2,2-Tetrachloroethane 10.0 898.89

59-1561,3-Dichlorobenzene 10.0 10810.8

18-1901,4-Dichlorobenzene 10.0 10510.5

18-1901,2-Dichlorobenzene 10.0 10710.7

27-200*Acrolein 100 1615.9

61-141Acrylonitrile 10.0 939.28

Form 3C - OrganicPrinted: 09/17/2015 13:10:48 Page 1 of 1

Results flagged with an asterisk (*) indicate values outside control criteria.

RR181838SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3LCS.rpt

Page 154 of 196

Page 155: Grays Harbor Energy, LLC 401 Keys Road

Semi-Volatile Organic Compounds by GC/MS

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 155 of 196

Page 156: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

K1509368-001

ug/L

NA

PP

08/26/2015

08/26/2015

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Semi-Volatile Organic Compounds by GC/MS

Lab Code:

Level: LowExtraction Method:

Analysis Method:

EPA 3520C

625

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

2.2 08/27/151 KWG150814010/03/150.47UNDN-Nitrosodimethylamine

0.44 08/27/151 KWG150814010/03/150.039UNDBis(2-chloroethyl) Ether

0.55 08/27/151 KWG150814010/03/150.070UNDPhenol

0.55 08/27/151 KWG150814010/03/150.060UND2-Chlorophenol

0.22 08/27/151 KWG150814010/03/150.029UNDBis(2-chloroisopropyl) Ether

0.22 08/27/151 KWG150814010/03/150.027UNDHexachloroethane

0.44 08/27/151 KWG150814010/03/150.041UNDN-Nitrosodi-n-propylamine

0.44 08/27/151 KWG150814010/03/150.031UNDNitrobenzene

0.22 08/27/151 KWG150814010/03/150.018UNDIsophorone

0.55 08/27/151 KWG150814010/03/150.070UND2-Nitrophenol

4.4 08/27/151 KWG150814010/03/152.5UND2,4-Dimethylphenol

0.22 08/27/151 KWG150814010/03/150.027UNDBis(2-chloroethoxy)methane

0.55 08/27/151 KWG150814010/03/150.052UND2,4-Dichlorophenol

0.22 08/27/151 KWG150814010/03/150.018UND1,2,4-Trichlorobenzene

0.22 08/27/151 KWG150814010/03/150.025UNDNaphthalene

0.22 08/27/151 KWG150814010/03/150.030UNDHexachlorobutadiene

0.55 08/27/151 KWG150814010/03/150.041UND4-Chloro-3-methylphenol

1.1 08/27/151 KWG150814010/03/150.21UNDHexachlorocyclopentadiene

0.55 08/27/151 KWG150814010/03/150.064UND2,4,6-Trichlorophenol

0.22 08/27/151 KWG150814010/03/150.046UND2-Chloronaphthalene

0.22 08/27/151 KWG150814010/03/150.017UNDAcenaphthylene

0.22 08/27/151 KWG150814010/03/150.024UNDDimethyl Phthalate

0.44 08/27/151 KWG150814010/03/150.037UND2,6-Dinitrotoluene

0.22 08/27/151 KWG150814010/03/150.029UNDAcenaphthene

4.4 08/27/151 KWG150814010/03/150.19UND2,4-Dinitrophenol

2.2 08/27/151 KWG150814010/03/150.31UND4-Nitrophenol

1.1 08/27/151 KWG150814010/03/150.020UND2,4-Dinitrotoluene

0.22 08/27/151 KWG150814010/03/150.030UNDFluorene

0.22 08/27/151 KWG150814010/03/150.030UND4-Chlorophenyl Phenyl Ether

0.22 08/27/151 KWG150814010/03/150.014UNDDiethyl Phthalate

2.2 08/27/151 KWG150814010/03/150.028UND2-Methyl-4,6-dinitrophenol

0.22 08/27/151 KWG150814010/03/150.053UNDN-Nitrosodiphenylamine

0.22 08/27/151 KWG150814010/03/150.024UNDAzobenzene†

Comments:

3of1Page16:52:1210/08/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR182516u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 156 of 196

Page 157: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

K1509368-001

ug/L

NA

PP

08/26/2015

08/26/2015

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Semi-Volatile Organic Compounds by GC/MS

Lab Code:

Level: LowExtraction Method:

Analysis Method:

EPA 3520C

625

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

0.22 08/27/151 KWG150814010/03/150.029UND4-Bromophenyl Phenyl Ether

0.22 08/27/151 KWG150814010/03/150.025UNDHexachlorobenzene

1.1 08/27/151 KWG150814010/03/150.38UNDPentachlorophenol

0.22 08/27/151 KWG150814010/03/150.025UNDPhenanthrene

0.22 08/27/151 KWG150814010/03/150.027UNDAnthracene

55 08/27/151 KWG150814009/09/1532U *NDBenzidine

0.22 08/27/151 KWG150814010/03/150.026J0.039Di-n-butyl Phthalate

0.22 08/27/151 KWG150814010/03/150.022UNDFluoranthene

0.22 08/27/151 KWG150814010/03/150.021U *NDPyrene

0.22 08/27/151 KWG150814010/03/150.020UNDButyl Benzyl Phthalate

2.2 08/27/151 KWG150814010/03/150.48UND3,3'-Dichlorobenzidine

0.22 08/27/151 KWG150814010/03/150.020UNDBenz(a)anthracene

0.22 08/27/151 KWG150814010/03/150.031UNDChrysene

1.1 08/27/151 KWG150814010/03/150.15UNDBis(2-ethylhexyl) Phthalate

1.1 08/27/151 KWG150814010/03/150.020UNDDi-n-octyl Phthalate

0.22 08/27/151 KWG150814010/03/150.019UNDBenzo(b)fluoranthene

0.22 08/27/151 KWG150814010/03/150.027UNDBenzo(k)fluoranthene

0.22 08/27/151 KWG150814010/03/150.035UNDBenzo(a)pyrene

0.22 08/27/151 KWG150814010/03/150.22UNDPerylene†

0.55 08/27/151 KWG150814010/03/150.55UND3-Methylcholanthrene†

0.22 08/27/151 KWG150814010/03/150.024UNDIndeno(1,2,3-cd)pyrene

0.22 08/27/151 KWG150814010/03/150.019UNDDibenz(a,h)anthracene

0.22 08/27/151 KWG150814010/03/150.021UNDBenzo(g,h,i)perylene

0.55 08/27/151 KWG150814010/03/150.55UNDDibenzo(a,i)pyrene†

0.55 08/27/151 KWG150814010/03/150.55UNDDibenzo(a,e)pyrene†

0.55 08/27/151 KWG150814010/03/150.55UNDDibenz(a,h)acridine†

0.55 08/27/151 KWG150814010/03/150.55UNDDibenzo(a,h)pyrene†

0.55 08/27/151 KWG150814010/03/150.55UNDDibenz(a,j)acridine†

* See Case Narrative

Comments:

3of2Page16:52:1210/08/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR182516u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 157 of 196

Page 158: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

K1509368-001

ug/L

NA

PP

08/26/2015

08/26/2015

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Semi-Volatile Organic Compounds by GC/MS

Lab Code:

Surrogate Name %Rec

Control

Limits NoteDate

Analyzed

23-121 Acceptable2-Fluorophenol 10/03/1591

31-122 AcceptablePhenol-d6 10/03/1591

38-124 AcceptableNitrobenzene-d5 10/03/1585

38-102 Acceptable2-Fluorobiphenyl 10/03/1585

27-128 Acceptable2,4,6-Tribromophenol 10/03/1594

56-138 AcceptableTerphenyl-d14 10/03/1580

† Analyte Comments

1,2-Diphenylhydrazine is reported as Azobenzene.Azobenzene

This compound is searched for as a tentatively identified compound.Perylene

This compound is searched for as a tentatively identified compound.3-Methylcholanthrene

This compound is searched for as a tentatively identified compound.Dibenzo(a,i)pyrene

This compound is searched for as a tentatively identified compound.Dibenzo(a,e)pyrene

This compound is searched for as a tentatively identified compound.Dibenz(a,h)acridine

This compound is searched for as a tentatively identified compound.Dibenzo(a,h)pyrene

This compound is searched for as a tentatively identified compound.Dibenz(a,j)acridine

Comments:

3of3Page16:52:1210/08/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR182516u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 158 of 196

Page 159: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508140-5

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Semi-Volatile Organic Compounds by GC/MS

Lab Code:

Level: LowExtraction Method:

Analysis Method:

EPA 3520C

625

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

1.9 08/27/151 KWG150814010/03/150.42UNDN-Nitrosodimethylamine

0.38 08/27/151 KWG150814010/03/150.035UNDBis(2-chloroethyl) Ether

0.48 08/27/151 KWG150814010/03/150.063UNDPhenol

0.48 08/27/151 KWG150814010/03/150.054UND2-Chlorophenol

0.19 08/27/151 KWG150814010/03/150.026UNDBis(2-chloroisopropyl) Ether

0.19 08/27/151 KWG150814010/03/150.024UNDHexachloroethane

0.38 08/27/151 KWG150814010/03/150.037UNDN-Nitrosodi-n-propylamine

0.38 08/27/151 KWG150814010/03/150.028UNDNitrobenzene

0.19 08/27/151 KWG150814010/03/150.016UNDIsophorone

0.48 08/27/151 KWG150814010/03/150.063UND2-Nitrophenol

3.8 08/27/151 KWG150814010/03/152.2UND2,4-Dimethylphenol

0.19 08/27/151 KWG150814010/03/150.024UNDBis(2-chloroethoxy)methane

0.48 08/27/151 KWG150814010/03/150.047UND2,4-Dichlorophenol

0.19 08/27/151 KWG150814010/03/150.016UND1,2,4-Trichlorobenzene

0.19 08/27/151 KWG150814010/03/150.022UNDNaphthalene

0.19 08/27/151 KWG150814010/03/150.027UNDHexachlorobutadiene

0.48 08/27/151 KWG150814010/03/150.037UND4-Chloro-3-methylphenol

0.95 08/27/151 KWG150814010/03/150.19UNDHexachlorocyclopentadiene

0.48 08/27/151 KWG150814010/03/150.058UND2,4,6-Trichlorophenol

0.19 08/27/151 KWG150814010/03/150.041UND2-Chloronaphthalene

0.19 08/27/151 KWG150814010/03/150.015UNDAcenaphthylene

0.19 08/27/151 KWG150814010/03/150.021UNDDimethyl Phthalate

0.38 08/27/151 KWG150814010/03/150.033UND2,6-Dinitrotoluene

0.19 08/27/151 KWG150814010/03/150.026UNDAcenaphthene

3.8 08/27/151 KWG150814010/03/150.17UND2,4-Dinitrophenol

1.9 08/27/151 KWG150814010/03/150.28UND4-Nitrophenol

0.95 08/27/151 KWG150814010/03/150.018UND2,4-Dinitrotoluene

0.19 08/27/151 KWG150814010/03/150.027UNDFluorene

0.19 08/27/151 KWG150814010/03/150.027UND4-Chlorophenyl Phenyl Ether

0.19 08/27/151 KWG150814010/03/150.012UNDDiethyl Phthalate

1.9 08/27/151 KWG150814010/03/150.025UND2-Methyl-4,6-dinitrophenol

0.19 08/27/151 KWG150814010/03/150.048UNDN-Nitrosodiphenylamine

0.19 08/27/151 KWG150814010/03/150.021UNDAzobenzene†

Comments:

3of1Page16:52:1610/08/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR182516u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 159 of 196

Page 160: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508140-5

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Semi-Volatile Organic Compounds by GC/MS

Lab Code:

Level: LowExtraction Method:

Analysis Method:

EPA 3520C

625

NoteMDLMRLQResultAnalyte Name

Extraction

Lot

Date

Analyzed

Date

Extracted

Dilution

Factor

0.19 08/27/151 KWG150814010/03/150.026UND4-Bromophenyl Phenyl Ether

0.19 08/27/151 KWG150814010/03/150.022UNDHexachlorobenzene

0.95 08/27/151 KWG150814010/03/150.34UNDPentachlorophenol

0.19 08/27/151 KWG150814010/03/150.022UNDPhenanthrene

0.19 08/27/151 KWG150814010/03/150.024UNDAnthracene

48 08/27/151 KWG150814009/08/1529U *NDBenzidine

0.19 08/27/151 KWG150814010/03/150.023J0.042Di-n-butyl Phthalate

0.19 08/27/151 KWG150814010/03/150.020UNDFluoranthene

0.19 08/27/151 KWG150814010/03/150.019U *NDPyrene

0.19 08/27/151 KWG150814010/03/150.018J0.030Butyl Benzyl Phthalate

1.9 08/27/151 KWG150814010/03/150.43UND3,3'-Dichlorobenzidine

0.19 08/27/151 KWG150814010/03/150.018UNDBenz(a)anthracene

0.19 08/27/151 KWG150814010/03/150.028UNDChrysene

0.95 08/27/151 KWG150814010/03/150.13UNDBis(2-ethylhexyl) Phthalate

0.95 08/27/151 KWG150814010/03/150.018UNDDi-n-octyl Phthalate

0.19 08/27/151 KWG150814010/03/150.017UNDBenzo(b)fluoranthene

0.19 08/27/151 KWG150814010/03/150.024UNDBenzo(k)fluoranthene

0.19 08/27/151 KWG150814010/03/150.031UNDBenzo(a)pyrene

0.19 08/27/151 KWG150814010/03/150.19UNDPerylene†

0.48 08/27/151 KWG150814010/03/150.48UND3-Methylcholanthrene†

0.19 08/27/151 KWG150814010/03/150.021UNDIndeno(1,2,3-cd)pyrene

0.19 08/27/151 KWG150814010/03/150.017UNDDibenz(a,h)anthracene

0.19 08/27/151 KWG150814010/03/150.019UNDBenzo(g,h,i)perylene

0.48 08/27/151 KWG150814010/03/150.48UNDDibenzo(a,i)pyrene†

0.48 08/27/151 KWG150814010/03/150.48UNDDibenzo(a,e)pyrene†

0.48 08/27/151 KWG150814010/03/150.48UNDDibenz(a,h)acridine†

0.48 08/27/151 KWG150814010/03/150.48UNDDibenzo(a,h)pyrene†

0.48 08/27/151 KWG150814010/03/150.48UNDDibenz(a,j)acridine†

* See Case Narrative

Comments:

3of2Page16:52:1610/08/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR182516u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 160 of 196

Page 161: Grays Harbor Energy, LLC 401 Keys Road

Analytical Results

Grays Harbor Energy, LLC K1509368

KWG1508140-5

ug/L

NA

Method Blank

NA

NA

GHEC NPDES

Water

Client:

Project:

Sample Matrix:

Service Request:

Date Collected:

Date Received:

ALS Group USA, Corp. dba ALS Environmental

Units:

Basis:

Sample Name:

Semi-Volatile Organic Compounds by GC/MS

Lab Code:

Surrogate Name %Rec

Control

Limits NoteDate

Analyzed

23-121 Acceptable2-Fluorophenol 10/03/1592

31-122 AcceptablePhenol-d6 10/03/1590

38-124 AcceptableNitrobenzene-d5 10/03/1579

38-102 Acceptable2-Fluorobiphenyl 10/03/1578

27-128 Acceptable2,4,6-Tribromophenol 10/03/1593

56-138 AcceptableTerphenyl-d14 10/03/1577

† Analyte Comments

1,2-Diphenylhydrazine is reported as Azobenzene.Azobenzene

This compound is searched for as a tentatively identified compound.Perylene

This compound is searched for as a tentatively identified compound.3-Methylcholanthrene

This compound is searched for as a tentatively identified compound.Dibenzo(a,i)pyrene

This compound is searched for as a tentatively identified compound.Dibenzo(a,e)pyrene

This compound is searched for as a tentatively identified compound.Dibenz(a,h)acridine

This compound is searched for as a tentatively identified compound.Dibenzo(a,h)pyrene

This compound is searched for as a tentatively identified compound.Dibenz(a,j)acridine

Comments:

3of3Page16:52:1610/08/2015Printed: Form 1A - Organic

Merged SuperSet Reference: RR182516u:\Stealth\Crystal.rpt\Form1mNew.rpt

Page 161 of 196

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ALS Group USA, Corp. dba ALS Environmental

Extraction Method:

QA/QC Report

Surrogate Recovery Summary

Grays Harbor Energy, LLC K1509368

Low

Water

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Units:

Level:

Sample Name Lab Code

Semi-Volatile Organic Compounds by GC/MS

EPA 3520C

Analysis Method: 625

Sur1 Sur2 Sur3 Sur4 Sur5 Sur6

Percent

K1509368-001PP 91 91 85 809485

KWG1508140-5Method Blank 92 90 79 779378

KWG1508140-1PPMS 82 86 79 749976

KWG1508140-2PPDMS 92 93 84 7910577

KWG1508140-3Lab Control Sample 91 91 84 7810377

KWG1508140-4Duplicate Lab Control Sample 81 84 75 7410079

2,4,6-Tribromophenol

Form 2A - OrganicPrinted: 10/08/2015 16:52:21 1 of 1

Surrogate Recovery Control Limits (%)

23-121

31-122

38-124

2-Fluorophenol

Phenol-d6

Nitrobenzene-d5

2-Fluorobiphenyl 38-102

27-128

56-138Terphenyl-d14

Results flagged with an asterisk (*) indicate values outside control criteria.

Page

Results flagged with a pound (#) indicate the control criteria is not applicable.

RR182516SuperSet Reference:

Sur1

Sur2

Sur3

Sur4

Sur5

Sur6

=

=

=

=

=

=

u:\Stealth\Crystal.rpt\Form2.rpt

Page 162 of 196

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Matrix Spike/Duplicate Matrix Spike Summary

Sample

Result %Rec

Matrix Spike

%Rec

Limits

Duplicate Matrix Spike

%Rec RPD

RPD

Limit

QA/QC Report

Grays Harbor Energy, LLC

PP

K1509368-001

625

K1509368

ug/L

NA

Semi-Volatile Organic Compounds by GC/MS

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Sample Name:

Lab Code:

Extraction Method:

Analysis Method:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result Result

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed:

08/27/2015

10/01/2015 -

10/02/2015

EPA 3520C

KWG1508140

KWG1508140-2KWG1508140-1

PPMS PPDMS

Spike

Amount

Spike

Amount

5-112ND 5.43 106Phenol 5.38 101 3065.41 5.75

23-134ND 5.43 1002-Chlorophenol 5.38 93 3085.00 5.44

0.01-230ND 5.43 100N-Nitrosodi-n-propylamine 5.38 96 3065.14 5.43

44-142ND 5.43 781,2,4-Trichlorobenzene 5.38 83 3054.47 4.26

22-147ND 5.43 924-Chloro-3-methylphenol 5.38 93 3005.02 5.00

47-145ND 5.43 85Acenaphthene 5.38 85 3014.59 4.63

0.01-132ND 5.43 884-Nitrophenol 5.38 93 3044.99 4.78

39-139ND 5.43 1032,4-Dinitrotoluene 5.38 103 3015.54 5.60

14-176ND 5.43 105Pentachlorophenol 5.38 102 3045.49 5.69

52-115ND 5.43 104Pyrene 5.38 100 3055.37 5.67

Form 3A - OrganicPrinted: 10/08/2015 16:52:25 Page 1 of 1

Results flagged with an asterisk (*) indicate values outside control criteria.

Results flagged with a pound (#) indicate the control criteria is not applicable.

RR182516SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3DMS.rpt

Page 163 of 196

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Lab Control Spike/Duplicate Lab Control Spike Summary

%Rec

Lab Control Spike

%Rec

Limits

Duplicate Lab Control Spike

%Rec RPD

RPD

Limit

QA/QC Report

Duplicate Lab Control Sample

KWG1508140-4

Grays Harbor Energy, LLC K1509368

625

ug/L

NA

Lab Control Sample

KWG1508140-3

Semi-Volatile Organic Compounds by GC/MS

KWG1508140

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Extraction Method:

Analysis Method:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result Result

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed:

08/27/2015

09/08/2015 -

10/01/2015

EPA 3520C

Spike

Amount

Spike

Amount

46-1225.00 101 30N-Nitrosodimethylamine 5.00 115 135.75 5.07

12-1585.00 83 30Bis(2-chloroethyl) Ether 5.00 96 154.79 4.14

5-1125.00 90 30Phenol 5.00 99 94.93 4.52

23-1345.00 86 302-Chlorophenol 5.00 103 185.13 4.28

36-1665.00 79 305.00 85 8Bis(2-chloroisopropyl) Ether 4.25 3.93

40-1135.00 69 30Hexachloroethane 5.00 74 73.69 3.44

0.01-2305.00 79 30N-Nitrosodi-n-propylamine 5.00 98 214.91 3.96

35-1805.00 83 30Nitrobenzene 5.00 94 134.70 4.13

21-1965.00 84 30Isophorone 5.00 93 104.65 4.21

29-1825.00 95 302-Nitrophenol 5.00 102 75.09 4.74

32-11915.0 91 302,4-Dimethylphenol 15.0 106 1515.9 13.7

33-1845.00 85 305.00 98 15Bis(2-chloroethoxy)methane 4.91 4.23

39-1355.00 104 302,4-Dichlorophenol 5.00 123 166.13 5.22

44-1425.00 79 301,2,4-Trichlorobenzene 5.00 92 164.60 3.93

21-1335.00 84 30Naphthalene 5.00 93 104.66 4.21

24-1165.00 67 30Hexachlorobutadiene 5.00 76 133.81 3.35

22-1475.00 92 304-Chloro-3-methylphenol 5.00 105 135.27 4.61

10-475.00 13 30Hexachlorocyclopentadiene 5.00 15 170.775 0.652

37-1445.00 103 302,4,6-Trichlorophenol 5.00 104 25.22 5.13

60-1185.00 90 302-Chloronaphthalene 5.00 89 14.45 4.48

33-1455.00 95 30Acenaphthylene 5.00 93 24.67 4.77

0.01-1125.00 86 30Dimethyl Phthalate 5.00 89 34.45 4.32

50-1585.00 106 302,6-Dinitrotoluene 5.00 108 15.39 5.31

47-1455.00 86 30Acenaphthene 5.00 88 24.39 4.32

0.01-1915.00 56 302,4-Dinitrophenol 5.00 49 142.44 2.79

0.01-1325.00 88 304-Nitrophenol 5.00 88 04.38 4.39

39-1395.00 100 302,4-Dinitrotoluene 5.00 101 15.04 5.02

59-1215.00 95 30Fluorene 5.00 95 04.74 4.75

25-1585.00 89 305.00 90 04-Chlorophenyl Phenyl Ether 4.48 4.46

0.01-1145.00 88 30Diethyl Phthalate 5.00 88 04.39 4.42

0.01-1815.00 74 305.00 73 12-Methyl-4,6-dinitrophenol 3.67 3.69

44-1115.00 82 30N-Nitrosodiphenylamine 5.00 84 24.18 4.08

43-1165.00 87 30Azobenzene 5.00 91 44.53 4.34

53-1275.00 90 305.00 98 94-Bromophenyl Phenyl Ether 4.92 4.48

0.01-1525.00 90 30Hexachlorobenzene 5.00 101 115.03 4.52

Form 3C - OrganicPrinted: 10/08/2015 16:52:29 Page 1 of 2

Results flagged with an asterisk (*) indicate values outside control criteria.

RR182516SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3DLC.rpt

Page 164 of 196

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Lab Control Spike/Duplicate Lab Control Spike Summary

%Rec

Lab Control Spike

%Rec

Limits

Duplicate Lab Control Spike

%Rec RPD

RPD

Limit

QA/QC Report

Duplicate Lab Control Sample

KWG1508140-4

Grays Harbor Energy, LLC K1509368

625

ug/L

NA

Lab Control Sample

KWG1508140-3

Semi-Volatile Organic Compounds by GC/MS

KWG1508140

Water

Low

GHEC NPDES

Client:

Project:

Sample Matrix:

Service Request:

Extraction Method:

Analysis Method:

Units:

Basis:

Level:

Extraction Lot:

Analyte Name Result Result

ALS Group USA, Corp. dba ALS Environmental

Date Extracted:

Date Analyzed:

08/27/2015

09/08/2015 -

10/01/2015

EPA 3520C

Spike

Amount

Spike

Amount

14-1765.00 85 30Pentachlorophenol 5.00 92 84.62 4.25

54-1205.00 86 30Phenanthrene 5.00 94 94.70 4.32

27-1335.00 89 30Anthracene 5.00 96 74.78 4.44

70-130** 105 66 30Benzidine 105 66 068.9 68.9

1-1185.00 92 30Di-n-butyl Phthalate 5.00 97 64.86 4.58

26-1375.00 88 30Fluoranthene 5.00 94 64.70 4.41

52-115* 5.00 104 30Pyrene 5.00 116 115.79 5.18

0.01-1525.00 105 30Butyl Benzyl Phthalate 5.00 115 95.75 5.25

0.01-262** 5.00 0 303,3'-Dichlorobenzidine 5.00 0 NCND ND

33-1435.00 92 30Benz(a)anthracene 5.00 101 95.06 4.61

17-1685.00 89 30Chrysene 5.00 99 104.95 4.46

8-1585.00 105 305.00 115 9Bis(2-ethylhexyl) Phthalate 5.73 5.23

4-1465.00 109 30Di-n-octyl Phthalate 5.00 110 15.50 5.44

24-1595.00 98 30Benzo(b)fluoranthene 5.00 97 14.85 4.90

11-1625.00 99 30Benzo(k)fluoranthene 5.00 101 25.05 4.94

17-1635.00 100 30Benzo(a)pyrene 5.00 99 14.95 4.98

0.01-1715.00 106 30Indeno(1,2,3-cd)pyrene 5.00 104 25.19 5.32

0.01-2275.00 101 30Dibenz(a,h)anthracene 5.00 98 34.92 5.06

0.01-2195.00 104 30Benzo(g,h,i)perylene 5.00 102 25.10 5.20

Form 3C - OrganicPrinted: 10/08/2015 16:52:29 Page 2 of 2

Results flagged with an asterisk (*) indicate values outside control criteria.

RR182516SuperSet Reference:

Percent recoveries and relative percent differences (RPD) are determined by the software using values in the calculation which have not been rounded.

u:\Stealth\Crystal.rpt\Form3DLC.rpt

Page 165 of 196

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Subcontract Lab Results

ALS Environmental—Kelso Laboratory 1317 South 13th Avenue, Kelso, WA 98626 Phone (360)577-7222 Fax (360)636-1068 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 166 of 196

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September 14, 2015. Service Request No: K1509368

Chris Leaf.

ALS Environmental 1317 South 13th Avenue Kelso, WA 98626

Laboratory Result for: Grays Harbor Energy, LLC. Dear Chris: Enclosed are the results of the sample(s) submitted to our laboratory on August 28, 2015. For Your reference, these analyses have been assigned our service request number: K1509368. Analyses were performed according to our laboratory’s NELAP-approved quality assurance program. The test results meet requirements of the current TNI standards, where applicable, and considered in their entirety, and ALS Environmental is not responsible for use of less than the final complete report. Results apply only to the items submitted to the laboratory for analysis and individual items (samples) analyzed, as listed in the report. In accordance to the TNI 2009 Standard, a statement on the estimated uncertainty of measurement of any quantitative analysis will be supplied upon request. Please contact me if you have any questions. My direct line is 281-575-2279. You may also contact me via email at [email protected] Respectfully submitted, ALS Group USA Corp., dba ALS Environmental

Arthi Kodur Project Manager Page 1 of __________

Page 167 of 196

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Certificate of Analysis

ALS Environmental - Houston HRMS 10450 Stancliff Rd, Suite 210, Houston TX 77099 Phone (713)266-1599 Fax (713)266-0130 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 168 of 196

Page 169: Grays Harbor Energy, LLC 401 Keys Road

ALS ENVIRONMENTAL Client: Grays Harbor Energy, LLC Service Request No.: K1509368 Project: GHEC NPDES Date Received: 8/28/15 Sample Matrix: Water

ALS ENVIRONMENTAL NARRATIVE All analyses were performed in adherence to the quality assurance program of ALS Environmental. This report contains analytical results for samples designated for Tier II. When appropriate to the method, method blank results have been reported with each analytical test. Sample Receipt One water sample was received for analysis at ALS Environmental – Houston HRMS on 8/28/15. The date of receipt currently references the date ALS Environmental-Kelso received the samples (8/26/15) and not the date ALS Environmental-Houston HRMS received the samples (8/28/15). The sample was received at 0.9C in good condition and is consistent with the accompanying chain of custody form. The sample was stored in a refrigerator at 4C upon receipt at the laboratory. Data Validation Notes and Discussion

MS/MSD

EQ1500524: Laboratory Control Spike/Duplicate Laboratory Control Spike (LCS/DLCS) samples were analyzed and reported in lieu of to an MS/DMS for this extraction batch. The batch quality control criteria were met.

Detection Limits Detection limits are calculated for each analyte in each sample by measuring the height of the noise level for each quantitation ion for the associated labeled standard. The concentration equivalent to 2.5 times the height of the noise is then calculated using the appropriate response factor and the weight of the sample. The calculated concentration equals the detection limit. The results of analyses are given in the attached laboratory report. All results are intended to be considered in their entirety, and ALS Environmental (ALS) is not responsible for utilization of less than the complete report.

Use of ALS group USA Corp dba ALS Environmental (ALS)’s Name. Client shall not use ALS’s name or trademark in any marketing or reporting materials, press releases or in any other manner (“Materials”) whatsoever and shall not attribute to ALS any test result, tolerance or specification derived from ALS’s data (“Attribution”) without ALS’s prior written consent, which may be withheld by ALS for any reason in its sole discretion. To request ALS’s consent, Client shall provide copies of the proposed Materials or Attribution and describe in writing Client’s proposed use of such Materials or Attribution. If ALS has not provided written approval of the Materials or Attribution within ten (10) days of receipt from Client, Client’s request to use ALS’s name or trademark in any Materials or Attribution shall be deemed denied. ALS may, in its discretion, reasonably charge Client for its time in reviewing Materials or Attribution requests. Client acknowledges and agrees that the unauthorized use of ALS’s name or trademark may cause ALS to incur irreparable harm for which the recovery of money damages will be inadequate. Accordingly, Client acknowledges and agrees that a violation shall justify preliminary injunctive relief. For questions contact the laboratory.

Page 169 of 196

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PPK1509368-001 8/26/2015 0745

Client: Grays Harbor Energy, LLC Service Request:K1509368Project: GHEC NPDES

SAMPLE CROSS-REFERENCE

SAMPLE # CLIENT SAMPLE ID DATE TIME

Printed 9/14/2015 12:46:04 PM Sample SummaryPage 170 of 196

Page 171: Grays Harbor Energy, LLC 401 Keys Road

Service Request SummaryFolder #:Client Name:Project Name:Project Number:

Report To: Peter ValinskeGrays Harbor Energy, LLC401 Keys RoadElma, WA 98541USA

Phone Number:Cell Number:Fax Number:E-mail:

K1509368Grays Harbor Energy, LLCGHEC NPDES

360-482-6292360-359-5144

[email protected]

Project Chemist:Originating Lab:

Logged By:Date Received:

Internal Due Date:QAP:

Qualifier Set:Formset:

Merged?:Report to MDL?:

P.O. Number:EDD:

Chris LeafKELSOSWOLF

9/11/2015

Lab StandardLab Standard

LAB QAP

08/26/15

YY

WAEIM v2013

7 1000 ml-Glass Bottle NM AMBER Teflon Liner Unpreserved3 1000 mL-Plastic Bottle NM CLEAR Unpreserved2 500 mL-Plastic Bottle NM CLEAR HNO33 40 ml-Glass Vial VOA CLEAR Tef/Silicone Septa HCL2 1000 mL-Glass Bottle NM AMBER Teflon Liner HCL1 500 ml-Plastic Bottle WM CLEAR HNO31 500 mL-Plastic Bottle NM CLEAR Unpreserved1 500 mL-Plastic Bottle NM CLEAR NaOH1 500 mL-Plastic Bottle NM CLEAR H2SO41 500 mL-Plastic Bottle NM NaOH,ZincAcetat1 500 mL-Fluoropoly Blue Label HCL1 300 mL-Glass Bottle NM CLEAR Unpreserved1 250 mL-Plastic Bottle NM CLEAR EDTA1 100 ml-Plastic Cup Sterile Na2S2O3

K-Disposed, K-Delilah-46, In Lab, K-Delilah-06, K-METALS, K-PETUNIA-11, E-Disposed, K-GenChem

Location:

Pressure Gas:

NPDES

KELSO

Lab Samp No. Client Samp No Matrix Collected Am

mon

ia/S

M 4

500-

NH

3 E

BO

D 5

Day

/SM

521

0 B

Br/3

00.0

Chl

orin

e R

esid

/SM

450

0-C

l G

CN

T/3

35.4

CO

D T

/SM

522

0 C

Col

or/S

M 2

120

B

F/30

0.0

Fec

Col

i MT/

SM

922

1 E

MB

AS

/SM

554

0 C

NO

2 N

O3

Cal

c/C

alcu

latio

n

NO

2/30

0.0

NO

3/30

0.0

O P

hos

T/36

5.3

OG

HE

M/1

664A

Oxy

gen/

SM

450

0-O

G

K1509368-001 PP Water 08/26/15 0745 V V V V V V V V V V V V V V V V

Printed 9/14/2015 12:46:07 PMPage 171 of 196

Page 172: Grays Harbor Energy, LLC 401 Keys Road

KELSO KELSO KELSO HOUSTON KELSO

SO

4/30

0.0

Sul

fide

T/S

M 4

500-

S2-

D

Sul

fite/

SM

450

0-S

O32

- B

TDS

/SM

254

0 C

TKN

/AS

TM D

1426

-08B

TOC

T/S

M 5

310

C

TON

Cal

c/C

alcu

latio

n

TSS

/SM

254

0 D

Cr6

/701

0

Hg

LL T

/163

1E

Met

als

D/2

00.8

Met

als

T/20

0.7

Met

als

T/20

0.8

PE

ST_

PC

B/6

08

SV

O L

L/62

5

Dio

xins

Fur

ans/

1613

B

VO

C_F

P/6

24

V V V V V V V V V V V V V V V II V

Printed 9/14/2015 12:46:07 PMPage 172 of 196

Page 173: Grays Harbor Energy, LLC 401 Keys Road

Service Request SummaryFolder #:Client Name:Project Name:Project Number:

Report To: Peter ValinskeGrays Harbor Energy, LLC401 Keys RoadElma, WA 98541USA

Phone Number:Cell Number:Fax Number:E-mail:

K1509368Grays Harbor Energy, LLCGHEC NPDES

360-482-6292360-359-5144

[email protected]

Project Chemist:Originating Lab:

Logged By:Date Received:

Internal Due Date:QAP:

Qualifier Set:Formset:

Merged?:Report to MDL?:

P.O. Number:EDD:

Chris LeafKELSOSWOLF

9/11/2015

Lab StandardLab Standard

LAB QAP

08/26/15

YY

WAEIM v2013

7 1000 ml-Glass Bottle NM AMBER Teflon Liner Unpreserved3 1000 mL-Plastic Bottle NM CLEAR Unpreserved2 500 mL-Plastic Bottle NM CLEAR HNO33 40 ml-Glass Vial VOA CLEAR Tef/Silicone Septa HCL2 1000 mL-Glass Bottle NM AMBER Teflon Liner HCL1 500 ml-Plastic Bottle WM CLEAR HNO31 500 mL-Plastic Bottle NM CLEAR Unpreserved1 500 mL-Plastic Bottle NM CLEAR NaOH1 500 mL-Plastic Bottle NM CLEAR H2SO41 500 mL-Plastic Bottle NM NaOH,ZincAcetat1 500 mL-Fluoropoly Blue Label HCL1 300 mL-Glass Bottle NM CLEAR Unpreserved1 250 mL-Plastic Bottle NM CLEAR EDTA1 100 ml-Plastic Cup Sterile Na2S2O3

K-Disposed, K-Delilah-46, In Lab, K-Delilah-06, K-METALS, K-PETUNIA-11, E-Disposed, K-GenChem

Location:

Pressure Gas:

NPDES

Test Comments:Group Test/Method Samples CommentsGenChem Fec Coli MT/SM 9221 E 1 Report in ALS Std Lab format.Metals Cr6/7010 1 + QC Dup/MSMetals Metals T/200.8 1 Al Sb As Ba Be B Cd Cr Co Cu Pb Mn Mo Ni Se Ag Tl Sn ZnMetals Metals T/200.7 1 Fe,Mg,P,TiMetals Metals D/200.8 1 AsSemivoa GCMS Dioxins Furans/1613B 1 2,3,7,8-TCDD ALS Houston

Printed 9/14/2015 12:46:07 PMPage 173 of 196

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Printed 9/14/2015 12:46:07 PMPage 174 of 196

Page 175: Grays Harbor Energy, LLC 401 Keys Road

B Indicates the associated analyte was found in the method blank at >1/10th the reported value.

E Estimated value. The reported concentration is above the calibration range of the instrument.

H Sample extracted and/or analyzed out of suggested holding time.J Estimated value. The reported concentration is below the MRL.K The ion abundance ratio between the primary and secondary ions were outside of

theoretical acceptance limits. Reported concentration is a conservative estimate, however EMPC correction was not applied.

P Chlorodiphenyl ether interference was present at the retention time of the target analyte. Reported result should be considered an estimate.

Q Monitored lock-mass indicates matrix-interference. Reported result is estimated.S Signal saturated detector. Result reported from dilution.U Compound was analyzed for, but was not detected (ND).X See Case Narrative.Y Isotopically Labeled Standard recovery outside of acceptance limits. In all cases, the

signal-to-nois ratios are greater than 10:1, making the recoveries acceptable.i The MDL/MRL have been elevated due to a matrix interference.

Data QualifiersHRMS Qualifier Set

Page 175 of 196

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Cal CalibrationConc CONCentrationDioxin(s) Polychlorinated dibenzo-p-dioxin(s)EDL Estimated Detection LimitEMPC Estimated Maximum Possible ConcentrationFlags Data qualifiersFuran(s) Polychlorinated dibenzofuran(s)g GramsICAL Initial CALibrationID IDentifierIons Masses monitored for the analyte during data acquisitionL Liter (s)LCS Laboratory Control SampleDLCS Duplicate Laboratory Control SampleMB Method BlankMCL Method Calibration LimitMDL Method Detection LimitmL MillilitersMS Matrix Spiked sampleDMS Duplicate Matrix Spiked sampleNO Number of peaks meeting all identification criteriaPCDD(s) Polychlorinated dibenzo-p-dioxin(s)PCDF(s) Polychlorinated dibenzofuran(s)ppb Parts per billionppm Parts per millionppq Parts per quadrillionppt Parts per trillionQA Quality AssuranceQC Quality ControlRatio Ratio of areas from monitored ions for an analyte% Rec. Percent recoveryRPD Relative Percent DifferenceRRF Relative Response FactorRT Retention TimeSDG Sample Delivery GroupS/N Signal-to-noise ratioTEF Toxicity Equivalence FactorTEQ Toxicity Equivalence Quotient

Acronyms

ALS Laboratory Group

Page 176 of 196

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State Certifications, Accreditations, and Licenses

Agency Number Expire DateAmerican Association for Laboratory Accreditation 2897.01 11/30/2015Arizona Department of Health Services AZ0793 5/27/2016Arkansas Department of Environmental Quality 14-038-0 6/16/2016California Department of Health Services 2452 2/28/2017Florida Department of Health E87611 6/30/2016Illinois Environmental Protection Agency 200057 10/6/2015Kansas Department of Health and Environment E-10406 1/31/2016Louisiana Department of Environmental Quality 03048 6/30/2016Louisiana Department of Health and Hospitals LA150026 12/31/2015Maine Center for Disease Control and Prevention 2014019 6/5/2016Maryland Department of the Environment 343 6/30/2016Michigan Depratment of Environmental Quality 9971 6/30/2016Minnesota Department of Health 840911 12/31/2015Nebraska Department of Health and Human Services NE-OS-25-13 6/30/2016New Mexico Environment Department TX02694 6/30/2016New York Department of Health 11707 4/1/2016Oregon Environmental Laboratory Accreditation Program TX200002 3/24/2016Pennsylvania Department of Environmental Protection 68-03441 6/30/2016Texas Commision on Environmental Quality TX104704216-14-5 6/30/2016United States Department of Agriculture P330-14-00067 2/21/2017Washington Department of Health c819 11/14/2015West Virginia Department of Environmental Protection 347 6/30/2016

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Chain of Custody

ALS Environmental - Houston HRMS 10450 Stancliff Rd, Suite 210, Houston TX 77099 Phone (713)266-1599 Fax (713)266-0130 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 179 of 196

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Page 180 of 196

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Page 181 of 196

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10450 Stancliff Rd., Suite 210 Houston, TX 77099 T: +1 713 266 1599 F: +1 713 266 1599 www.alsglobal.com

R I G H T S O L U T I O N S | R I G H T P A R T N E R

SAMPLE ACCEPTANCE POLICY

This policy outlines the criteria samples must meet to be accepted by ALS Environmental – Houston HRMS.

Cooler Custody Seals (desirable, mandatory if specified in SAP):

Intact on outside of cooler, signed and dated

Chain-of-Custody (COC) documentation (mandatory):

The following is required on each COC:

Sample ID, the location, date and time of collection, collector’s name, preservation type, sampletype, and any other special remarks concerning the sampleThe COC must be completed in ink.

Signature and date of relinquishing party.

In the absence of a COC at sample receipt, the COC will be requested from the client.

Sample Integrity (mandatory):

Samples are inspected upon arrival to ensure that sample integrity was not compromised during transfer to the laboratory.

Sample containers must arrive in good condition (not broken or leaking). Samples must be labeled appropriately, including Sample IDs, and requested test using durable

labels and indelible ink. The correct type of sample bottle must be used for the method requested. An appropriate sample volume, or weight, must be received. Sample IDs and number of containers must reconcile with the COC. Samples must be received within the method defined holding time.

Temperature Requirement (varies by sample matrix):

Aqueous and Non-aqueous samples must be shipped and stored cold, at 0 to 6ºC. Tissue samples must be shipped and stored frozen, at -20 to -10ºC. Air samples are shipped and stored cold, at 0 to 6ºC The sample temperature must be recorded on the COC

All cooler inspections are documented on the Cooler Receipt Form (CRF). A separate CRF is completed for each service request. Any samples not meeting the above criteria are noted on the CRF and the Project Manager notified. The Project Manager must resolve any sample integrity issues with the client prior to proceeding with the analysis. Such resolutions are documented in writing and filed with the project folder. Data associated with samples received outside of this acceptance policy will be qualified on the case narrative of the final report

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Preparation Information Benchsheets

ALS Environmental - Houston HRMS

10450 Stancliff Rd., Suite 210, Houston, TX 77099

Phone (713)266-1599 Fax (713)266-0130

www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

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Preparation Information BenchsheetPrep Run#: Prep WorkFlow:

Prep Date/Time: Team: Prep Method:Status:243698 OrgExtAq(365)

9/1/15 07:40 AMPrepped

Method Sep Funnel/JarSemivoa GCMS/LMCCRINK

# Lab Code Client ID B# Method /Test Matrix Amt. Ext. Sample DescriptionpH

1 E1500630-001RE 1613B/Dioxins Furans 1000mL .01 clear colorless liquid 5 AQ 1.5- LOD - 1613 Water

2 E1500818-001 1613B/Dioxins Furans 1000mL .01 clear colorless liquid 5 PE1373-2ML Water

3 E1500846-001 1613B/Dioxins Furans 1058mL .01 clear light yellow liquid 7 2090987 001 Water

4 E1500846-002 1613B/Dioxins Furans 1064mL .01 clear colorless liquid 5 2090987 002 EQUIPMENT BLANK Water

5 E1500849-001 1613B/Dioxins Furans 1004mL .01 clear light yellow liquid 7 2091274 001 Drinking Water

6 E1500850-001 1613B/Dioxins Furans 1041mL .01 clear light yellow liquid 6 2091011 001 Drinking Water

7 E1500851-001 1613B/Dioxins Furans 1019mL .01 clear colorless liquid 6 2090973 002 Drinking Water

8 E1500852-001 1613B/Dioxins Furans 1057mL .01 clear light yellow liquid 7 2090506 001 Drinking Water

9 E1500854-001 1613B/Dioxins Furans 957mL .01 clear colorless liquid 9 1H51840-01 Water

10 E1500857-001 1613B/Dioxins Furans 884mL .01 clear light yellow liquid 6 15-07454 Water

11 EQ1500524-01 1613B/Dioxins Furans 1000.0mL 5 MB Liquid

12 EQ1500524-02 1613B/Dioxins Furans 1000.0mL 5 LCS Liquid

13 EQ1500524-03 1613B/Dioxins Furans 1000.0mL 5 DLCS Liquid

14 K1509368-001 1613B/Dioxins Furans 906mL .05 clear colorless liquid 7 PP Water

15 R1506763-001 1613B/Dioxin Furans Unadjusted MRL

1043.0mL .01 clear colorless liquid 7 STE-08132015-24 HR Water

Spiking Solutions

Logbook Ref:Inventory ID Expires On:0.02-0.2ng/mL LM 1/16/1578144 01/13/2016Name: 1613B/23/TO-9A MDL Native Solution

E1500630-001 75.00µL

Logbook Ref:Inventory ID Expires On:83502 DE 8/20/15 2-20ng/ml83502 02/16/2016Name: 1613B Matrix Working Standard

EQ1500524-02 100.00µL EQ1500524-02 100.00µL EQ1500524-03 100.00µL EQ1500524-03 100.00µL

Logbook Ref:Inventory ID Expires On:83716 DE 8/27/15 2-4ng/ml83716 02/23/2016Name: 1613B Labeled Working Standard

E1500630-001 1,000.00µL E1500818-001 1,000.00µL E1500846-001 1,000.00µL E1500846-002 1,000.00µL E1500849-001 1,000.00µL E1500850-001 1,000.00µL

E1500851-001 1,000.00µL E1500852-001 1,000.00µL E1500854-001 1,000.00µL E1500857-001 1,000.00µL EQ1500524-01 1,000.00µL EQ1500524-01 1,000.00µL

EQ1500524-02 1,000.00µL EQ1500524-02 1,000.00µL EQ1500524-03 1,000.00µL EQ1500524-03 1,000.00µL K1509368-001 1,000.00µL R1506763-001 1,000.00µL

Logbook Ref:Inventory ID Expires On:83796 CID 08/31/2015 EXC83796 02/27/2016Name: 8290/1613B Cleanup Working Standard

E1500630-001 100.00µL E1500818-001 100.00µL E1500846-001 100.00µL E1500846-002 100.00µL E1500849-001 100.00µL E1500850-001 100.00µL

E1500851-001 100.00µL E1500852-001 100.00µL E1500854-001 100.00µL E1500857-001 100.00µL EQ1500524-01 100.00µL EQ1500524-01 100.00µL

EQ1500524-02 100.00µL EQ1500524-02 100.00µL EQ1500524-03 100.00µL EQ1500524-03 100.00µL K1509368-001 100.00µL R1506763-001 100.00µL

Preparation Information BenchsheetPrinted 9/9/15 8:25 Page 1Page 184 of 196

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Preparation Information BenchsheetPrep Run#: Prep WorkFlow:

Prep Date/Time: Team: Prep Method:Status:243698 OrgExtAq(365)

9/1/15 07:40 AMPrepped

Method Sep Funnel/JarSemivoa GCMS/LMCCRINK

Preparation Materials

Sensafe Free Chlorine WTR CHK

LM 3/19/15 (79756) Carbon, High Purity LM 8/27/15 (83730) Ethyl Acetate 99.9% Minimum EtOAc

AL 07/16/15 (82546)

Glass Wool AL 04/17/15 (80420) Sulfuric Acid Reagent Grade H2SO4

LM 3/4/15 (79265) Hexanes 95% LM 8/27/15 (83726)

Dichloromethane (Methylene Chloride) 99.9% MeCl2

AL 07/27/15 (82887) Sodium Hydroxide Reagent Grade NaOH

LM 09/02/14 (74232) Sodium Sulfate Anhydrous Reagent Grade Na2SO4

AL 07/15/15 (82507)

Tridecane (n-Tridecane) LM 8/27/15 (83731) ColorpHast pH-Indicator Strips AL 03/24/15 (79846) Silica Gel CID 08/18/2018 (83330)Toluene 99.9% Minimum LM 8/27/15 (83728)

Preparation Steps

9/1/15 07:40

9/1/15 09:15

Extraction

LMCCRINK

Step:

Started:

Finished:

By:

Comments

9/3/15 14:30

9/3/15 14:30

Acid Clean

CDIAZ

Step:

Started:

Finished:

By:

Comments

9/3/15 08:00

9/3/15 10:00

Silica Gel Clean

CDIAZ

Step:

Started:

Finished:

By:

Comments

9/4/15 13:05

9/4/15 13:43

Final Volume

DEDWARDS

Step:

Started:

Finished:

By:

Comments

Comments:

Date: Reviewed By:

NoYes

Extracts ExaminedDate:

Date: Received By:

Relinquished By:

Chain of Custody

Preparation Information BenchsheetPrinted 9/9/15 8:25 Page 2

00:00

00:00 10:10

ak 9/9/15ak 9/9/15

ak 9/9/15

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Analytical Results

ALS Environmental - Houston HRMS 10450 Stancliff Rd., Suite 210, Houston, TX 77099 Phone (713)266-1599 Fax (713)266-0130 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

Page 186 of 196

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K1509368-001Lab Code:Sample Name: PP

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

08/26/15 07:45

NApg/L

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/09/15 17:589/1/15

08/26/15 13:30

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 906mL Instrument Name: E-HRMS-07GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P50114906/30/15

P301354P501143

Native Analyte Results

Analyte Name QDilutionFactorMRLEDLResult

IonRatio RRT

2,3,7,8-TCDD ND U 0.847 5.52 1

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:13 PM 15-0000344261 rev 00Superset Reference:

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K1509368-001Lab Code:Sample Name: PP

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

08/26/15 07:45

NAPercent

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/09/15 17:589/1/15

08/26/15 13:30

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 906mL Instrument Name: E-HRMS-07GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P50114906/30/15

P301354P501143

Labeled Standard Results

Labeled Compounds % Rec QControlLimits

Conc.Found (pg)

SpikeConc.(pg)

IonRatio RRT

1.02213C-2,3,7,8-TCDD 2000 1019.975 25-164 0.7951

1.02237Cl-2,3,7,8-TCDD 800 451.155 35-197 NA56

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:13 PM 15-0000344261 rev 00Superset Reference:

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EQ1500524-01Lab Code:Sample Name: Method Blank

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

NA

NApg/L

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/10/15 22:219/1/15

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 1000.0mL Instrument Name: E-HRMS-05GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P30135408/21/15

P301354P301350

Native Analyte Results

Analyte Name QDilutionFactorMRLEDLResult

IonRatio RRT

2,3,7,8-TCDD ND U 2.87 5.00 1

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:12 PM 15-0000344261 rev 00Superset Reference:

Page 189 of 196

Page 190: Grays Harbor Energy, LLC 401 Keys Road

EQ1500524-01Lab Code:Sample Name: Method Blank

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

NA

NAPercent

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/10/15 22:219/1/15

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 1000.0mL Instrument Name: E-HRMS-05GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P30135408/21/15

P301354P301350

Labeled Standard Results

Labeled Compounds % Rec QControlLimits

Conc.Found (pg)

SpikeConc.(pg)

IonRatio RRT

1.01913C-2,3,7,8-TCDD 2000 865.151 25-164 0.7443

1.02037Cl-2,3,7,8-TCDD 800 374.441 35-197 NA47

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:12 PM 15-0000344261 rev 00Superset Reference:

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Accuracy & Precision

ALS Environmental - Houston HRMS 10450 Stancliff Rd., Suite 210, Houston TX 77099 Phone (713)266-1599 Fax (713)266-0130 www.alsglobal.com

RIGHT SOLUTIONS | RIGHT PARTNER

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Duplicate Lab Control SampleEQ1500524-03

Lab Control SampleEQ1500524-02

Analyte Name

K1509368Date Analyzed:Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Duplicate Lab Control Sample SummaryPolychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

Analysis Method:Prep Method:

1613BMethod Sep Funnel/Jar NA

pg/LBasis:Units:

Analysis Lot: 462027

09/10/15

Spike AmountResult % Rec % RecResult Spike Amount% Rec Limits RPD RPD Limit

09/01/15Date Extracted:

dba ALS EnvironmentalALS Group USA, Corp.

QA/QC Report

228 2002,3,7,8-TCDD 502 67-158116 200232 114

15-0000344261 rev 00Superset Reference:Printed 9/14/2015 12:46:12 PM

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EQ1500524-02Lab Code:Sample Name: Lab Control Sample

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

NA

NApg/L

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/10/15 16:119/1/15

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 1000.0mL Instrument Name: E-HRMS-07GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P50117506/30/15

P301354P501168

Native Analyte Results

Analyte Name QDilutionFactorMRLEDLResult

IonRatio RRT

2,3,7,8-TCDD 232 2.42 5.00 0.76 1.001 1

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:12 PM 15-0000344261 rev 00Superset Reference:

Page 193 of 196

Page 194: Grays Harbor Energy, LLC 401 Keys Road

EQ1500524-02Lab Code:Sample Name: Lab Control Sample

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

NA

NAPercent

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/10/15 16:119/1/15

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 1000.0mL Instrument Name: E-HRMS-07GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P50117506/30/15

P301354P501168

Labeled Standard Results

Labeled Compounds % Rec QControlLimits

Conc.Found (pg)

SpikeConc.(pg)

IonRatio RRT

1.02113C-2,3,7,8-TCDD 2000 858.281 25-164 0.7943

1.02237Cl-2,3,7,8-TCDD 800 401.245 35-197 NA50

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:12 PM 15-0000344261 rev 00Superset Reference:

Page 194 of 196

Page 195: Grays Harbor Energy, LLC 401 Keys Road

EQ1500524-03Lab Code:Sample Name: Duplicate Lab Control Sample

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

NA

NApg/L

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/10/15 17:009/1/15

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 1000.0mL Instrument Name: E-HRMS-07GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P50117606/30/15

P301354P501168

Native Analyte Results

Analyte Name QDilutionFactorMRLEDLResult

IonRatio RRT

2,3,7,8-TCDD 228 0.637 5.00 0.76 1.001 1

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:13 PM 15-0000344261 rev 00Superset Reference:

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EQ1500524-03Lab Code:Sample Name: Duplicate Lab Control Sample

Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans by HRGC/HRMS

NA

NAPercent

Basis:Units:

1613BAnalysis Method:Method Sep Funnel/JarPrep Method:

09/10/15 17:009/1/15

NA

K1509368

Date Received:Date Collected:

Service Request:

WaterGHEC NPDESGrays Harbor Energy, LLC

Sample Matrix:Project:Client:

Date Analyzed:Date Extracted:

Sample Amount: 1000.0mL Instrument Name: E-HRMS-07GC Column: DB-5MSUI

Blank File Name:Cal Ver. File Name:

Data File Name:ICAL Date:

P50117606/30/15

P301354P501168

Labeled Standard Results

Labeled Compounds % Rec QControlLimits

Conc.Found (pg)

SpikeConc.(pg)

IonRatio RRT

1.02113C-2,3,7,8-TCDD 2000 957.163 25-164 0.7948

1.02237Cl-2,3,7,8-TCDD 800 422.655 35-197 NA53

Analytical ReportALS Group USA, Corp. dba ALS Environmental

Printed 9/14/2015 12:46:13 PM 15-0000344261 rev 00Superset Reference:

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