Final_Data_Report_KVK_AC_HARS_2013.pdf

Data Report

Kill van Kull and Anchorage Channels – 50-foot SRUC, Delivery Orders #39/#01

Prepared by Battelle 397 Washington Street Duxbury, MA 02332

Prepared for

USACE/NYD

26 Federal Plaza Jacob Javitz Building New York, NY 10278

February 2013

Table of Contents – Kill van Kull and Anchorage Channels Delivery Orders #39/#01, HARS

Description Page Number

Sample Custody 1

Water/Elutriate Metals QA/QC Narrative 37

Water/Elutriate Metals Data 41

Water/Elutriate PCB/Pesticide QA/QC Narrative, Batch 12-0552 45

Water/Elutriate PCB/Pesticide Data, Batch 12-0552 48

Water/Elutriate PCB/Pesticide QA/QC Narrative, Batch 12-0572 71

Water/Elutriate PCB/Pesticide Data, Batch 12-0572 74

Tissue Metals QA/QC Narrative 94

Tissue Metals Data – dry weight 97

Tissue Metals Data – wet weight 101

Tissue Pesticide QA/QC Narrative, Batch 12-0756 104

Tissue Pesticide Data, Batch 12-0756 107

Tissue PCB/PAH QA/QC Narrative, Batch 12-0756 119

Tissue PCB/PAH Data, Batch 12-0756 122

Tissue Pesticide QA/QC Narrative, Batch 12-0757 141

Tissue Pesticide Data, Batch 12-0757 144

Tissue PCB/PAH QA/QC Narrative, Batch 12-0757 155

Tissue PCB/PAH Data, Batch 12-0757 159

Tissue Pesticide QA/QC Narrative, Batch 12-0758 177

Tissue Pesticide Data, Batch 12-0758 180

Tissue PCB/PAH QA/QC Narrative, Batch 12-0758 192

Tissue PCB/PAH Data, Batch 12-0758 196

Tissue Dioxin QA/QC Narrative 215

Tissue Dioxin Data, Batch 53720-02 220

Tissue Dioxin Data, Batch 53720-09 237

Tissue Dioxin Data, Batch 53720-13 252

Bligh & Dyer Lipid Data 267

Sample Custody

PEVEN

Text Box Updated Custody form received from ASI after data finalized. Sample ID's have been redline updated in this data report. cspm 2/28/2013

Baltelle usincs [ovation

ShpNo SHP-120921-03

Battelle Project No:1

Project Number:

32-103

Received by:

Schumitz, Mat

No. of Shipping Containers:

SHIPMENT

Method of Delivery: Commercial Carrier

CAC Forms:

J Shipped with samples

Cooler(s)/Sox(es

1z 238 6X4 01 5097 7262 .'ustody Seal5

1z 238 6X4 01,5097 1277 ' justody Seatt

V Sample labels agree with COC forms

Discrepancies (see Sample Custody Corrective Action Form)

V Tape J Custody Seals INl Other Seals (See sample Log) V Seals intact for each shipping container

Seals broken (See sample log for impacted samples)

Condition of Samples:

V; Sample containers intact

1 Sample containers broken/leaking (See Custody Corrective Action Form)

Temperature upon receipt (°C):

1.2

Temperature Blank used d^ Yes

No (Note: If temperature upon receipt differs from required conditions, see sample log comment field)

Samples Acidified: V' Unknown

Initial pH 5-9?:

Yes

I No di NA If no, individual sample adjustments on the Auxiliary Sample Receipt Form

Total Residual Chlorine Present?:

i No V NA If yes, individual sample adjustments on the Auxiliary Sample Receipt Form

Head Space <1% in samples for water VOC analysis:

No V NA Individual sample deviations noted on sample log

Samples Containers:

Samples returned in PC-grade jars:

No V Unknown /Lot No.: Unknown

Storage Location:

Chem South: Refrigerator - R0003 (Upper Cold BOO IDs Assigned:

N5326- N5328

Samples logged in by:

Schumitz, Matt

Date/Time:

09/21/2012 12:00 AM

Approved By:

Approved On:

Authorized By:

Authorized On:

Client: ACOE-KVK

Date/Time Received: Friday, September 21, 2012 12:00 AM

Tracking Number:

No Forms

Cooler Cooler

Samples

Sample Labels:

Container Seats:

1.2

Intact

Intact

Intact Intact

Printed on 912112012

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Baltelie ShpNo

Received by:

No. of Shipping Containers:

SHIPMENT

Method of Delivery: Hand Delivered

Tracking Number:

Not R

COC Forms:

`V Shipped with samples

No Forms

Cooler(s)/Box(es)

Not Applicable

Ambient

Samples

Sample Labels:

V Sample labels agree with COC forms

I^ Discrepancies (see Sample Custody Corrective Action Form)

Container Seals: q Tape q Custody Seals q Other Seals (See sample Log) EVI Seals intact for each shipping container q Seals broken (See sample log for impacted samples)

Sample containers intact

Sample containers broken/leaking (See Custody Corrective Action Form

Temperature upon receipt ('C):

Temperature Blank used q Yes [V1 No (A?ote: /,temperature upon receipt differs from required conditions, see sample log comment field)

Samples Acidified: q Yes q Na EVI Unknown

Initial pH 5-9?:

q Yes q No V NA If no, individual sample adjustments on the Auxiliary Sample Receipt Form

Residual Chlorine Present?:

(i Yes nents on the I uxiliar

Storage Location:

Samples logged in by:

Approved By:

Authorized Btr:

BOO IDs Assigned:

N5:

Approved On:

Authorized On fi

Ba fte lle in s

I r1

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N o

P ro je ct

I V u m b l e n t:

R e ce iv e d b y a te

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N o o f S h ip p in g u ri ta in e rs io n

D og in D s:

M at em p:

p

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V O re d

I oc o

C o n ti n en ts

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A T

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Q J fl^ i r

'e C on da y, S ep te m be r

, 2

3:

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Elutriate Preparation Form and Checklist

Project Name:

Reach ID:

Sediment sample ID:

• sample ID:

Elutriate sample ID:

Checklist:

Sediment Volume:

Water Volume:

(Reach A Elutriate for example)

Mix ratio of 1:4 (sediment to water by volume Mixing start time: A Manual mix # 1 start time:

Manual mix #2 start time: 1.2 Final manual mix and end time:

4 Allow to settle for 1 hour (+/- 5 minutes) Sampling time: I Centrifuge: ( minutes C C rpm COC to sample custodian for new Battelle ID

K Subsample for metals (if metals analysis r equired) Acidify metals split with nitric acid:

(a. t

(date/time)

Batte lle ShpNo SHP-120925-02

Hargis, I

SHIPMENT

be or uenvery:

Client:

Date/Time Received:

i racKmg Drum

CDC Fod Shipped with samples No Forms

Intact

0.4

Sample Labels:

Container Seals:

Sam

V Discrepancies (see Sample Custody C on F+

Tape

Custody Seals

Other Seals (See sample Log) V Seals intact for each shipping container

Seals broken (See sample log for impacted samples)

Condition of Samples: V Sample containers intact

Sample containers broken/h e Custody Corrective Action Fori perature upon receipt (IC):

0.4

Temperature Blank used J Yes

No ee sample I

Samples Acidified: Yes V Unknown

Initial pH 5-9?: Yes nts on the Auxilia

V NA

Receipt formsarnpii

Report Corrective Actions Approved:Authorized

Corrective Action No: 1 of

ShpNo: SHP-120925-02

Battelle Project No:

COC Client:

COC Project:

COC Date: 9/25/2012 8:34:00 AM

Documentation of project manager notification

Date: 9/25/2012 9:16:00 AM

Date: 11/14/2012 10:44:00 A

Date: 11/14/2012 10:43:00 A

Documentation of client notification (should be completed by project manager within 24 hrs):

On I contacted at

Results of communication with client (Describe any corrective action directed by the client):

The identity of the samples were clear and sediment composites were used for elutriate sample preparation.

Date this form was received back to the custodian:

Reference Number:

Sample Custodian Schumitz, Matt

Laboratory Manager: McInerney, Kevin

Project Manager: Peven-McCarthy, Carole

Description of Problem: Explanation:

Sample KVK-East End Composite came in listed as Composite KVK-EE-HARS on the sample container.

Jars and C-O-C do not have matching IdsClient Id

Sample Anchorage Channel Composite came in listed as ACOE-AC-HARS Composite on the sample container.

Jars and C-O-C do not have matching Ids

Printed on 11/14/2012 Page 1 of 1 h p N o

B a tt e lle

P ro je c t N o

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N A

N A r, :3

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N A

C A

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N

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P n te d r v e I o f

8 LBS

SHIP ATTN: SAMPLE RECEIVING (781) 952-52I

BATTELLE

397 WASHINGTON STREET

D XS RY MA 02332-4546

MA 025 9 -02

UPS EARLY A.M.

TRACKING #: 1 Z 238 6X4 15 4824 6100

BILLING: PIP

i

A 111111 11

Baltelle ShpNo SHP-120925-04

Battelle Project No:

Project Number:

Received by:

No. of Shipping Containers:

SHIPMENT

Method of Delivery: Tracking Number:

CDC Forms:

V Shipped with samples

No Forms

V Sample labels agree with COC forms

Discrepancies {see Sample Custody Corrective Action Form)

Seals broken (See sample log for impacted samples)

V Sample containers intact

Sample containers broken/leaking (See Custody Corrective Action Form

Samples

Sample Labels:

Container Seals:

Condition of Samples:

Temperature upon receipt (°C):

('sole: If temperature upon rece pies Acidified:

Ambient

VI Yes

Temperature Blank used

Yes V No see sample logcommentfteld)

Unknown on the Initial pH 5-9?:

If no, individual

Total Residual Chlorine Present?:

No VI" y Sample Re( ition:

Chem South: Refrigerator - R0003 (Upper Cold BDO IDs Assigned:

N 5

Samples logged in by:

Schurrritz, Mat'

Approved On:

Ba lte lle I n u v t i

S h p

F -1 v t°

B a tt e ll e P ro je c t

N

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SHIPMEN7

Method of Del

CDC Forms:

Samples

Sample La

Container Seals:

Condition of Samples: V Sample cot

Sample contaii ive Actio

Temperature upon receipt 2.5

If-ternperature upon receipt daffersfrom required c pies Acidified:

No V Unknown p N o i

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Baltelle tint)v ..tio n

ShpNo SHP-120927-01

Battelle Project No:

Set urnit

SHIPMENT

Method of Delivery:

Client:

Date /Time Received:

Tracking Number:

Sample Labels:

Container Seals:

Seals broken (See sample log for impacted samples)

V Sample containers intact

Sample containers broken/leaking (See Custody Corrective Action Form)

Temperature upon receipt (°C):

(,ote: If temperature upon receip

Temperature Blank used Yes V No ired conditions, see sample log comme

Samples Acidified: V Yes

No Unknown

Total Residual Chlorine Present?:

Storage Location:

Samples logg€

BDO IDs Assigned:

N 5

Approved On:

are

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E lutriate Preparation Form and Checklist

Project Name:

Reach ID:

Sediment sample ID:

Water sample ID:

Sediment Volume:

Water Volume:

E lutriate sample ID:

(Reach A Elutriate for example)

Checklist:

eY, Mix ratio of 1:4 (sediment to water by volume) Mixing start time: _ Manual mix # 1 start time:

Manual mix #2 start time:

Final manual mix and end time:

Allow to settle for 1 hour (-+/- 5 minutes) Sampling time: I I Centrifuge: / minutes *, *° rpm

COC to sample custodian for new Battelle ID J Subsample for metals (if metals analysis required) 01 Acidify metals split with nitric acid:

(date/time

Battelle

Schumit

Client: AST

Date/Time Received: 6

SHIPMENT

Method of Delivery:

COC Forms:

Tracking Number:

No FormsV Shipped with samples

UPS

Cooler

Sample Labels:

dy Seal:

:,ustody Seal.

'OC forms ustody Corrective Action Form)

Intact 24

5X4

1Z 238 6X4 4945 2536

Container Seals:

Seals broken (See sample log for impacted samples)

V Sample containers intact

Sample containers broken/leaking (See Custody Corrective Action

Temperature upon receipt (°C): Temperature Blank used

I conditions, see sample In receipt dill

1.1 s No d)

Samples Acidified:

No V Unknown

Pal

Sample Receipt Form Details

ShpNo SHP-121120-02

Approved: Authorized

Project Number: Client: ASI

Received by: Schumitz, Matt Date/Time Received: Tuesday, November 20, 2012 12:00 AM

No. of Shipping Containers: 2 BDO Id: Client Sample ID: Collection Date: Login Date: Ctrs: Matrix: Temp: pH: TRC: VOC: Stored In: Loc: No: Comments:

Battelle Project No:16704-0001

N6778 20121151 10/06/12 0:00 11/20/12 13:37 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Clean Tissue N6779 20121152 10/06/12 0:00 11/20/12 13:37 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Pretest A N6780 20121153 10/06/12 0:00 11/20/12 13:38 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Pretest B N6781 20121154 10/06/12 0:00 11/20/12 13:38 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Pretest C N6782 20121092 11/03/12 0:00 11/20/12 13:38 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Mud Dump Ref Tan N6783 20121093 11/03/12 0:00 11/20/12 13:39 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Mud Dump Ref Tan N6784 20121094 11/03/12 0:00 11/20/12 13:39 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Mud Dump Ref Tan N6785 20121095 11/03/12 0:00 11/20/12 13:39 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Mud Dump Ref Tan N6786 20121096 11/03/12 0:00 11/20/12 13:39 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN Mud Dump Ref Tan N6787 20121097 11/03/12 0:00 11/20/12 13:39 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #1 N6788 20121098 11/03/12 0:00 11/20/12 13:40 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #23 N6789 20121099 11/03/12 0:00 11/20/12 13:40 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #22 N6790 20121100 11/03/12 0:00 11/20/12 13:40 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #19 N6791 20121101 11/03/12 0:00 11/20/12 13:40 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #2 N6792 20121102 11/03/12 0:00 11/20/12 13:41 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #20 N6793 20121103 11/03/12 0:00 11/20/12 13:41 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #9 N6794 20121104 11/03/12 0:00 11/20/12 13:41 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #3 N6795 20121105 11/03/12 0:00 11/20/12 13:41 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-EE Tank #24 N6796 20121106 11/03/12 0:00 11/20/12 13:41 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN KVK-WE Tanks #4, N6797 20121107 11/03/12 0:00 11/20/12 13:42 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN AC Tank #10 N6798 20121108 11/03/12 0:00 11/20/12 13:42 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN AC Tank #15 N6799 20121109 11/03/12 0:00 11/20/12 13:42 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN AC Tank #21 N6800 20121110 11/03/12 0:00 11/20/12 13:42 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN AC Tank #11 N6801 20121111 11/03/12 0:00 11/20/12 13:43 1 TISSUE 0.9 NA NA NA F0002 (Walk-in) MN AC Tank #18 N6802 20120948 10/05/12 0:00 11/20/12 13:47 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Clean Tissue N6803 20120949 10/05/12 0:00 11/20/12 13:47 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Pretest A N6804 20120950 10/05/12 0:00 11/20/12 13:47 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Pretest B N6805 20120951 10/05/12 0:00 11/20/12 13:47 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Pretest C

Printed on 11/26/2012 Page 1 of 2

Sample Receipt Form Details

ShpNo SHP-121120-02

Approved: Authorized

Project Number: Client: ASI

Received by: Schumitz, Matt Date/Time Received: Tuesday, November 20, 2012 12:00 AM

No. of Shipping Containers: 2 BDO Id: Client Sample ID: Collection Date: Login Date: Ctrs: Matrix: Temp: pH: TRC: VOC: Stored In: Loc: No: Comments:

Battelle Project No:16704-0001

N6806 20121069 11/02/12 0:00 11/20/12 13:47 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Mud Dump Ref Tank N6807 20121070 11/02/12 0:00 11/20/12 13:48 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Mud Dump Ref Tank N6808 20121071 11/02/12 0:00 11/20/12 13:48 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Mud Dump Ref Tank N6809 20121072 11/02/12 0:00 11/20/12 13:48 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Mud Dump Ref Tank N6810 20121073 11/02/12 0:00 11/20/12 13:48 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV Mud Dump Ref Tank N6811 20121074 11/02/12 0:00 11/20/12 13:49 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-EE Tank #5 N6812 20121075 11/02/12 0:00 11/20/12 13:49 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-EE Tank #15 N6813 20121076 11/02/12 0:00 11/20/12 13:49 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-EE Tank #21 N6814 20121077 11/02/12 0:00 11/20/12 13:49 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-EE Tank #18 N6815 20121078 11/02/12 0:00 11/20/12 13:50 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-EE Tanks #22, N6816 20121079 11/02/12 0:00 11/20/12 13:50 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-WE Tank #27 N6817 20121080 11/02/12 0:00 11/20/12 13:51 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-WE Tank #10 N6818 20121081 11/02/12 0:00 11/20/12 13:51 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-WE Tank #14 N6819 20121082 11/02/12 0:00 11/20/12 13:51 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-WE Tank #7 N6820 20121083 11/02/12 0:00 11/20/12 13:51 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV KVK-WE Tank #4 N6821 20121084 11/02/12 0:00 11/20/12 13:51 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV AC Tank #25 N6822 20121085 11/02/12 0:00 11/20/12 13:52 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV AC Tank #6 N6823 20121086 11/02/12 0:00 11/20/12 13:52 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV AC Tank #17 N6824 20121087 11/02/12 0:00 11/20/12 13:52 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV AC Tank #16 N6825 20121088 11/02/12 0:00 11/20/12 13:52 1 TISSUE 1.1 NA NA NA F0002 (Walk-in) NV AC Tank #20,13,24

Total Samples: 48

Printed on 11/26/2012 Page 2 of 2

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Water/Elutriate Data

QA/QC NARRATIVE

QA/QC Narrative Preparation SOP MSL-D-004 Page 1 of 4

PROJECT: USACE/NYD Kill van Kull and Anchorage Channel 2012 PARAMETER: Metals LABORATORY: Battelle Marine Sciences Laboratory, Sequim, Washington MATRIX: Seawater

SAMPLE CUSTODY

AND PROCESSING:

Three site waters, three elutriate samples, and one deionized water (DI) equipment blank for trace metals were received in three shipments on 09/20/12, 09/26/12 and 09/28/12. All samples were received in good condition (i.e., no sample containers were broken). Samples were assigned a Battelle Central File (CF) identification number (3337) and were entered into Battelle’s laboratory information management system. See the analytical note below for information about the DI equipment blank.

The following lists information on sample receipt and processing activities:

Lab Sample IDs: 3337*1-3 3337*4-6 3337*7 Description: Site Water Elutriate Equipment Blank

Sample collection dates 09/24-25/12 09/24-25/12, 09/27/12

9/27/12

Laboratory arrival date 09/20/12, 09/26/12 09/26/12, 09/28/12 9/28/12 Cooler temp. on arrival 2.5°C, 2.4C 2.3C, 4.4°C 4.4°C

Preconcentration (sweater by ICP/MS) 10/10/12 NA CVAF analysis (Hg) 10/05/12, 10/11/12 10/05/12

ICP-MS analysis (Ag, Cd, Cr, Cu, Pb, Ni, and Zn)

10/12/12 10/15/12

DATA QUALITY OBJECTIVES:

Analyte

Analytical Method

Range of Recovery

SRM Accuracy

Relative Precision

Target Detection

Limits (µg/L)

Achieved

PDL(2)

(µg/L)

Ag ICP-MS 75-125% 20% (1) ≤20% (1) 0.1 0.01 Cd ICP-MS 75-125% 20% (1) ≤20% (1) 0.025 0.013 Cr ICP-MS 75-125% 20% (1) ≤20% (1) 1 0.06 Cu ICP-MS 75-125% 20% (1) ≤20% (1) 0.3 0.09 Hg CVAF 75-125% 20% (1) ≤20% (1) 0.002 0.0001 Ni ICP-MS 75-125% 20% (1) ≤20% (1) 0.3 0.06 Pb ICP-MS 75-125% 20% (1) ≤20% (1) 0.3 0.0011 Zn ICP-MS 75-125% 20% (1) ≤20% (1) 0.15 0.02

(1) Evaluated for analytes >10x the MDL

(2) Batch specific practical detection limit (PDL) reported for all metals except Hg and Ag. The Ag is based on the low-level standard analyzed with the analytical batch. The PDL for Hg was less than the Annually Verified MDL; therefore, the MDL was reported..

METHODS:

Seawater samples were analyzed by three methods for eight low-level metals including:

silver (Ag), cadmium (Cd), chromium (Cr), copper (Cu), mercury (Hg), nickel (Ni), lead (Pb), and zinc (Zn).

Samples were analyzed for Hg without a preconcentration step using cold-vapor atomic fluorescence (CVAF) spectroscopy according to Battelle SOP MSL-I-013, Total Mercury in Aqueous Samples by CVAF, following EPA Method 1631 revision E.

All other metals were determined after a preconcentration using iron (Fe) and palladium (Pd) in accordance with the Battelle SOP MSL-I-025, Methods of Sample Preconcentration, which is derived from EPA Method 1640. The preconcentrated samples were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) for Ag, Cd, Cr, Cu, Ni, Pb and Zn

QA/QC Narrative Preparation SOP MSL-D-004 Page 2 of 4

METHODS:

following Battelle SOP MSL-I-022, Determination of Elements in Aqueous and Digestate Samples by ICP-MS. Base methods for this SOP are EPA Methods: 1640, 1638, and 200.8.

The DI water equipment blank (3337-7) was analyzed for Hg as described above. For all other metals, the DI water matrix does not require the Fe/Pd preconcentration prior to ICP- MS. Therefore it was analyzed following the total metal recoverable (TRM) method established in EPA Method 1640 prior to analysis by ICP-MS. In summary, this preparation brings the pH of the sample to 2% and heats the capped samples for 2 hours at 85˚C to solubilize particulates.

All results were reported in units of µg/L. Data were not blank corrected; however, the metals determined using Fe/Pd reductive precipitation preconcentration for Cr should be reagent blank corrected. The required preconcentration procedure for low level seawater samples includes the addition of chelating agents to induce precipitation of metals under specific conditions. Subsequently, reagents added to the samples should be of the purest quality to result in zero addition of metals to the seawater samples. See note in the Standard Reference Material (SRM) section.

HOLDING

TIMES:

The recommended holding times for metals analyses in water are 90 days from sample collection for Hg analysis and 6 months for analysis of all other metals. All samples were analyzed within their respective holding times.

DETECTION

LIMITS:

PDL Verification:

Target MDLs are provided from the USACE-NYD/EPA Region II RTM. Analytical results were reported to the batch specific laboratory achieved practical detection limits (PDL) as defined in the RTM. Since Ag was not detected in the PDL samples, the lowest passing low level standard spike level was used to qualify the data. For Hg, the PDL was less than the Annually Verified MDL; therefore the MDL was reported. Data were evaluated and flagged in accordance with the following criteria:

U Analyte not detected above the laboratory practical detection limit, PDL/MDL reported

& QC value outside the accuracy or precision criteria goal

B Blank concentration > 3 times the Target MDL and sample concentration < 10 times the detected blank

In accordance with the RTM, four replicates of a clean seawater (Sequim Bay seawater) were analyzed with the samples to provide a PDL verification study. The PDL verification study is defined as the analysis of four replicates of unspiked seawater. The standard deviation of the mean results was multiplied by the Student's-t value (4.541) for 4 (n-1) replicates.

REAGENT

BLANKS:

A minimum of three reagent blanks were analyzed with the set of seawater samples. The analyses of multiple reagent blanks allow for accurate quantification of the metal contribution from the reagents and provide the means to reagent blank correct the data if necessary. Metals detected in the reagent blanks were less than three times the PDL with the exception of Zn. However, the detected blanks for Zn were less than the target MDL.

The data are not blank corrected; however, reagent blank correcting is recommended for Fe/Pd metals, particularly Cr, due to trace amounts in the chelating reagents used to preconcentrate seawater. These reagents can not be obtained 100% pure (see SRM section below for details).

LABORATORY

CONTROL

In accordance with the RTM, the laboratory control sample (LCS) samples were fortified no greater than 10 times the target MDL. This level varies for each metal and is provided in the

QA/QC Narrative Preparation SOP MSL-D-004 Page 3 of 4

SAMPLE

ACCURACY:

table header. Two types of LCS samples were analyzed: 1) Sequim Bay seawater to verify low-level seawater recovery and 2) freshwater LCS samples to verify analytical accuracy within 10x the target MDL. The seawater LCS sample included one replicate of clean Sequim Bay seawater processed as an unspiked sample (SB Blank) and one as a spiked sample (SB LCS). All LCS recoveries were within the QC acceptance criteria of ± 25% recovery for all metals.

MATRIX SPIKE

ACCURACY:

One matrix spike (MS) sample was prepared with this batch of samples. The MS recoveries were within the QC acceptance criteria of ± 25% recovery for all metals. The RTM states the fortification level should be no greater than 10x the target MDL. The target fortification levels were achieved for all metals except Cd. There was no impact to data because the seawater SRM demonstrated acceptable accuracy for Cd near the target MDL level.

The issue of fortification or spiking levels in MS sample analyses for metals is different from organics analyses in that there are large differences between the metal target MDLs and the naturally occurring metals concentrations of the native sample. Because metal concentrations in the native samples are unknown, we choose a fortification or spiking level based on best professional judgment that will provide the most usable QC data to assess potential matrix interferences. In order to assess matrix interference, the target fortification levels should be no greater than 10X the native concentrations of metals in the field collected samples.

In order to attain usable matrix spike recovery data, the fortification level needs to exceed the achievable precision. Acceptable analytical precision is stated as <20% RSD, which means that the error associated with each concentration, is actually the concentration ± 20%.

Fortifying the spike sample within the error range of the number can result in attaining a spiking level within the analytical noise of the concentration. Therefore, good spike recoveries will not actually demonstrate there are no matrix interferences because they are also falling within the analytical noise.

TRIPLICATE

PRECISION:

Precision for this set of samples was assessed by the analysis of laboratory triplicates and expressed as the relative standard deviation (RSD) of replicate results. All samples were analyzed in triplicate. The RSD values were within the QC criterion of ≤20% RSD for all metals.

STANDARD

REFERENCE

MATERIAL

ACCURACY:

Two SRMs were analyzed with this set of samples: Seawater SRM CASS-5 and freshwater SRMs 1640a for ICP-MS metals and SRM 1641d for Hg. The SRM accuracy was expressed as the percent difference (PD) between the measured and certified values.

The SRM CASS-5 is a low-level seawater reference material. Currently, there is no seawater SRMs certified at a practical quantification level for all analytes of interest. The required preconcentration procedure for low level seawater samples includes the addition of chelating agents to induce precipitation of metals under specific conditions. Subsequently, reagents added to the samples should be of the purest quality to result in zero addition of metals to the samples. The current reagents available contain traces of the metals of interest and are not certified for Ag or Hg. The percent differences were within the QC acceptance criterion of ±20% with the exception of Cr. As noted in the method blank, there are detectable levels of Cr in the current reagents. Therefore, reagent correcting the CASS-5 concentration for Cr, subsequently meets the QC criterion (see table).

The SRM 1641 is a certified freshwater reference material for Hg, as no seawater SRM is certified for Hg. One replicate of SRM 1641 was analyzed with the samples for Hg. The PD for SRM 1641 was within the QC acceptance criterion of 20% (PD).

The SRM 1640a is a certified freshwater instrument check SRM. One replicate of SRM 1640a was analyzed with the set of samples by ICP-MS. The percent differences for metals

QA/QC Narrative Preparation SOP MSL-D-004 Page 4 of 4 certified or referenced in SRM 1640a were within the QC acceptance criterion of 20%

(PD).

ANALYTICAL

NOTE:

The trace metal samples are typically collected in pre-cleaned Teflon containers provided by Battelle MSL. Due to a laboratory error, one sample (3337-6 Anchorage Channel Elutriate) was collected in a pre-cleaned glass jar instead of Teflon. The impact to the sample was assessed through the collection of a DI water equipment blank in a glass bottle from the same lot as the sample. The bottle was filled with DI water and treated as a sample by the laboratory. The only difference was due to the freshwater matrix instead of seawater, the preconcentration procedure prior to ICP-MS analysis was not required. The sample was prepared and analyzed as described above.

The metals were not detected in the equipment blank greater than three times the target MDL except as noted below. The equipment blank concentrations for Hg, Cu, Ni, Pb, and Zn were greater than the PDL. The data were evaluated and the detected blank made up less than 3% of the concentration from the 3337-6 Elutriate. The only exception was the detected Cu equipment blank which comprised 28% of the elutriate concentration and could potentially bias the concentration high.

BATTELLE MARINE SCIENCES LABORATORIES

Jill Brandenberger, Project Manager USACE/NYD 1529 West Sequim Bay Rd. DO#39 Kill van Kull and Anchorage Channel Sequim, Washington 98382 METALS IN SITE WATER AND ELUTRIATE

(360) 681-4564

(concentrations in µg/L - not blank corrected) Client Code BOS Code

MSL

Code Matrix

Collection Date Hg Ag Cd Cr Cu Ni Pb Zn

Instrument: CVAF ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS

Target MDL 1 0.002 0.1 0.025 1 0.3 0.3 0.3 0.15

Batch Specific PDL2 0.0001 0.01 0.013 0.06 0.09 0.06 0.0011 0.02 Spiking Level 0.020 1.0 0.25 10 3.0 3.0 3.0 1.5

2012 0822 KVK West End 3337-1 R1 Site Water 09/18/12 0.0113 0.0129 0.0601 0.778 2.50 1.43 1.31 7.14 2012 0822 KVK West End 3337-1 R2 Site Water 09/18/12 0.0114 0.0146 0.0656 0.810 2.59 1.47 1.36 7.30 2012 0822 KVK West End 3337-1 R3 Site Water 09/18/12 0.0114 0.0137 0.0594 0.788 2.56 1.46 1.35 7.37

2012 0822 KVK West End 3337-1 Site Water 09/18/12 0.0114 0.0137 0.0617 0.792 2.55 1.45 1.34 7.27 Replicate Precision RSD 1% 6% 6% 2% 2% 1% 2% 2%

2012 0823 KVK East End 3337-2 Site Water 09/18/12 0.00848 0.0196 0.0501 0.952 2.29 1.39 1.31 4.67 2012 0823 KVK East End 3337-2 Site Water 09/18/12 0.00861 0.0214 0.0530 0.981 2.32 1.44 1.38 4.74 2012 0823 KVK East End 3337-2 Site Water 09/18/12 0.00922 0.0202 0.0529 0.968 2.33 1.40 1.34 4.70

2012 0823 KVK East End 3337-2 Site Water 09/18/12 0.00877 0.0204 0.0520 0.967 2.31 1.41 1.34 4.70 Replicate Precision RSD 5% 4% 3% 2% 1% 2% 3% 1%

20120824 Anchorage Channel 3337-3 R1 Site Water 09/24/12 0.00386 0.0144 0.0654 0.509 2.45 1.07 0.571 3.94 20120824 Anchorage Channel 3337-3 R2 Site Water 09/24/12 0.00410 0.0134 0.0656 0.543 2.50 1.12 0.596 4.13 20120824 Anchorage Channel 3337-3 R3 Site Water 09/24/12 0.00427 0.0142 0.0626 0.512 2.44 1.07 0.580 3.98

20120824 Anchorage Channel 3337-3 Site Water 09/24/12 0.00408 0.0140 0.0645 0.521 2.46 1.09 0.582 4.02 Replicate Precision RSD 5% 4% 3% 4% 1% 3% 2% 2%

N5394 KVK East Elutriate 3337-4 R1 Elutriate 09/25/12 0.0302 0.0661 0.0265 3.30 3.02 4.32 3.49 7.89 N5394 KVK East Elutriate 3337-4 R2 Elutriate 09/25/12 0.0324 0.0685 0.0299 3.40 3.01 4.43 3.51 8.25 N5394 KVK East Elutriate 3337-4 R3 Elutriate 09/25/12 0.0307 0.0645 0.0273 3.39 3.06 4.37 3.51 7.95

N5394 KVK East Elutriate 3337-4 Elutriate 09/25/12 0.0311 0.0664 0.0279 3.36 3.03 4.37 3.50 8.03 Replicate Precision RSD 4% 3% 6% 2% 1% 1% 0% 2%

N5384 KVK West Elutriate 3337-5 R1 Elutriate 09/24/12 0.0242 0.0405 0.0170 2.09 2.02 11.1 2.70 8.29 N5384 KVK West Elutriate 3337-5 R2 Elutriate 09/24/12 0.0252 0.0391 0.0182 2.03 2.04 11.1 2.69 8.27 N5384 KVK West Elutriate 3337-5 R3 Elutriate 09/24/12 0.0248 0.0392 0.0185 2.03 2.02 11.0 2.67 8.23

N5384 KVK West Elutriate 3337-5 Elutriate 09/24/12 0.0247 0.0396 0.0179 2.05 2.03 11.1 2.69 8.26 Replicate Precision RSD 2% 2% 4% 2% 1% 1% 1% 0%

1529 West Sequim Bay Rd. DO#39 Kill van Kull and Anchorage Channel Sequim, Washington 98382 METALS IN SITE WATER AND ELUTRIATE

(360) 681-4564

(concentrations in µg/L - not blank corrected) Client Code BOS Code

MSL

Code Matrix

Collection Date Hg Ag Cd Cr Cu Ni Pb Zn

Instrument: CVAF ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS

Target MDL 1 0.002 0.1 0.025 1 0.3 0.3 0.3 0.15

Batch Specific PDL2 0.0001 0.01 0.013 0.06 0.09 0.06 0.0011 0.02 Spiking Level 0.020 1.0 0.25 10 3.0 3.0 3.0 1.5

N5475 Anchorage Elutriate 3337-6 R1 Elutriate 09/27/12 0.0186 0.01 U 0.0503 1.28 3.37 2.00 2.68 18.4 N5475 Anchorage Elutriate 3337-6 R2 Elutriate 09/27/12 0.0189 0.01 U 0.0491 1.27 3.35 1.98 2.67 18.6 N5475 Anchorage Elutriate 3337-6 R3 Elutriate 09/27/12 0.0216 0.01 U 0.0524 1.24 3.33 1.90 2.65 18.6

N5475 Anchorage Elutriate 3337-6 Elutriate 09/27/12 0.0197 0.01 U 0.0506 1.26 3.35 1.96 2.67 18.5 Replicate Precision RSD 9% NA 3% 2% 1% 3% 1% 1%

Glass Bottle Blank EQP Blank 3337-7 R1 DI water 09/27/12 0.000236 0.01 U 0.013 U 0.06 U 0.956 0.06 U 0.0673 0.0401 EQP Blank 3337-7 R2 DI water 09/27/12 NA 0.01 U 0.013 U 0.06 U 0.933 0.06 U 0.0680 0.0498 EQP Blank 3337-7 R3 DI water 09/27/12 NA 0.01 U 0.013 U 0.06 U 0.932 0.06 U 0.0643 0.0377

EQP Blank 3337-7 DI water 09/27/12 NA 0.01 U 0.013 U 0.06 U 0.940 0.06 U 0.0665 0.0425 Replicate Precision RSD NA NA NA NA 1% 0% 3% 15%

Method Blank Reagent Blank 1 DI Blank R1 0.0001 U 0.01 U 0.013 U 0.0530 0.09 U 0.06 U 0.001 U 0.119 Reagent Blank 2 DI Blank R2 0.0001 U 0.01 U 0.013 U 0.0418 0.09 U 0.06 U 0.001 U 0.0865 Reagent Blank 3 DI Blank R3 0.0001 U 0.01 U 0.013 U 0.0466 0.09 U 0.06 U 0.001 U 0.0807

MEAN REAGENT BLANK 0.0001 U 0.01 U 0.013 U 0.0471 0.09 U 0.06 U 0.001 U 0.0954

10 times detected mean blank 0.471 0.954

TRM Blank for Freshwater TRM Blank NA 0.01 U 0.013 U 0.06 U 0.09 U 0.06 U 0.0011 U 0.02 U

1529 West Sequim Bay Rd. DO#39 Kill van Kull and Anchorage Channel Sequim, Washington 98382 METALS IN SITE WATER AND ELUTRIATE

(360) 681-4564

(concentrations in µg/L - not blank corrected) Client Code BOS Code

MSL

Code Matrix

Collection Date Hg Ag Cd Cr Cu Ni Pb Zn

Instrument: CVAF ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS

Target MDL 1 0.002 0.1 0.025 1 0.3 0.3 0.3 0.15

Batch Specific PDL2 0.0001 0.01 0.013 0.06 0.09 0.06 0.0011 0.02 Spiking Level 0.020 1.0 0.25 10 3.0 3.0 3.0 1.5

BLANK SPIKE ACCURACY

SBW SB Blank -- 0.01 U 0.0597 0.203 0.298 0.352 0.00229 0.260

LCS 1 SBLCS SBW -- 1.81 1.90 2.12 2.15 2.22 1.97 1.97

Spike Concentration 2 2 2 2 2 2 2 % Recovery -- 91% 92% 96% 93% 93% 98% 86%

LCS 2 TRM LCS FW -- 1.01 0.980 0.850 1.04 1.01 1.04 1.01

Spike Concentration -- 1.0 1.0 1.0 1.0 1.0 1.0 1.0 % Recovery -- 101% 98% 85% 104% 101% 104% 101%

Blank Blank 100412 0.0001 U -- -- -- -- -- -- -- LCS OPR 100412 run1 0.00515 -- -- -- -- -- -- -- LCS OPR 100412 run2 0.00549 -- -- -- -- -- -- --

Spike Concentration 0.00496 % Recovery 104% -- -- -- -- -- -- -- % Recovery 111% -- -- -- -- -- -- --

Blank BLANK 101012 0.000147 -- -- -- -- -- -- -- LCS OPR 101012 run1 0.00529 -- -- -- -- -- -- -- LCS OPR 101012 run2 0.00503 -- -- -- -- -- -- --

Spike Concentration 0.00496 % Recovery 104% -- -- -- -- -- -- -- % Recovery 98% -- -- -- -- -- -- --

MATRIX SPIKE ACCURACY

MS 3337-1 MS 0.0314 0.920 0.984 1.73 3.46 2.37 2.35 8.16

2012 0822 KVK West End 3337-1 R1 Site Water 09/18/12 0.0113 0.0129 0.0601 0.778 2.50 1.43 1.31 7.14

Spike Concentration 0.0195 1.0 1.0 1.0 1.0 1.0 1.0 1.0 % Recovery, MS 103% 91% 92% 95% 96% 94% 104% 102%

1529 West Sequim Bay Rd. DO#39 Kill van Kull and Anchorage Channel Sequim, Washington 98382 METALS IN SITE WATER AND ELUTRIATE

(360) 681-4564

(concentrations in µg/L - not blank corrected) Client Code BOS Code

MSL

Code Matrix

Collection Date Hg Ag Cd Cr Cu Ni Pb Zn

Instrument: CVAF ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS ICP-MS

Target MDL 1 0.002 0.1 0.025 1 0.3 0.3 0.3 0.15

Batch Specific PDL2 0.0001 0.01 0.013 0.06 0.09 0.06 0.0011 0.02 Spiking Level 0.020 1.0 0.25 10 3.0 3.0 3.0 1.5

STANDARD REFERENCE MATERIAL ACCURACY

SRM - Freshwater 1640a or 1641d (Hg) 1525 8.04 3.94 42.5 85.2 24.5 11.7 54.7 SRM - Freshwater 1640a or 1641d (Hg) 1568 8.02 3.99 37.5 86.2 25.1 12.4 55.3

Certified or Reference Value 1557 8.081 3.99 40.54 85.75 25.32 12.1 55.64 Range ± 20 ± 0.046 ± 0.074 ± 0.3 ± 0.51 ± 0.14 ± 0.05 ± 0.35

PD 2% 1% 1% 5% 1% 3% 3% 2%

PD 1% 1% 0% 7% 1% 1% 2% 1%

SRM - Seawater CASS-5 NA NA 0.0235 0.172 0.427 0.337 0.00986 0.621

Certified or Reference Value -- -- 0.0215 0.106 3 0.38 3 0.33 3 0.011 0.719 Range -- -- ± 0.0018 ± 0.013 ± 0.11 ± 0.023 ± 0.002 ± 0.068

PD NA NA 9% 62% 3 12% 3 2% 3 10% 14%

Reagent Corrected NA NA -- 18% -- -- -- --

PDL Verification

PDL (1) SBPDL1 SBW 0.000193 0.0000 0.0553 0.171 0.267 0.313 0.00192 0.231

PDL (2) SBPDL2 SBW 0.000196 0.0000 0.0521 0.173 0.280 0.317 0.00205 0.229

PDL (3) SBPDL3 SBW 0.000212 0.0000 0.0590 0.171 0.238 0.303 0.00238 0.237

PDL (4) SBPDL4 SBW 0.000206 0.0000 0.0565 0.196 0.275 0.334 0.00238 0.225

Mean 0.000202 NA 0.0557 0.178 0.265 0.317 0.00218 0.231 Stdev 0.000009 NA 0.0029 0.0122 0.019 0.013 0.000234 0.005 PDL Verification (SD * 4.541) 0.00004 0.01 0.013 0.06 0.09 0.06 0.0011 0.02

1 Target MDL reported from the USACE NYD/EPA Region II RTM.

2 Reported from batch specific PDL, except Ag and Hg. Ag DL is based on the low-level standard analyzed with the analytical batch due to low or no Ag measured in the PDL sample. The PDL for Hg was less than our annual MDL of 0.0001 µg/L; therefore MDL was used to evaluate the data set.

3 Certified value is less than 10x PDL; results to be used with caution

U Analyte not detected above the laboratory PDL, PDL/MDL reported B Mean reagent blank concentration > 3 times the achieved PDL and sample concentration < 10 times the mean reagent blank.

& QC value outside the accuracy or precision criteria goal: spike accuracy ± 25% recovery;

replicate precision <20% (RSD); SRM accuracy <20% (PD) SBW Sequim Bay water (clean seawater) RSD Relative standard deviation

PD Percent difference SL Sample was underspiked relative to the native sample concentration

QA/QC Summary Batch 12-0552

Project: USACE/NYD DO#39 – Kill van Kull and Anchorage Channel

Parameters: PCB and Pesticides

Laboratory: Battelle‐Duxbury, MA

Matrix: Water and Elutriate

Data Set: DP‐12‐0847

Analytical SOP: 5‐128‐12

Method Reference:

EPA 8081B/8082A modified

Sample Custody

Collection Date Receipt Date Temp (°C)

9/18/2012 (site water) 9/24‐25/2012 (elutriate prepared)

9/21/2012 (site water) 9/24‐25/2012 (elutriate)

0.9‐1.2

Corrective Actions No corrective actions.

Sample Storage The water samples were stored refrigerated until extraction.

Related samples NA

METHOD SUMMARIES

Sample Preparation

Water and elutriate samples were extracted for PCB and pesticides analysis according to Battelle SOP 5‐200, Water Extraction for Trace Level Semi‐Volatile Organic Contaminant Analysis. Approximately 1 liter of water was spiked with surrogates and extracted three times with dichloromethane using separatory funnel techniques. The combined extract was dried over anhydrous sodium sulfate, concentrated, processed through alumina cleanup column, concentrated and further purified using size exclusion chromatography High Performance Liquid Chromatography cleanup. The final concentrated extract was solvent exchanged into hexane and fortified with internal standard (IS) compounds.

Prep comments Note: all samples in this batch are from the Kill van Kull site.

Analysis PCB and pesticides were analyzed by gas chromatography electron capture detection (GC/ECD). An initial calibration consisting of target analytes was analyzed prior to sample analysis to demonstrate the linear range. Calibration verification was performed at the beginning and end of each 12‐hr period in which samples were analyzed. Concentrations of target compounds were calculated versus internal standards using the average response factors (RF) generated from the initial calibration.

Holding Times Extraction Date(s) Analysis Date(s)

9/25/2012 ‐ 10/10‐12/2012 10/20‐21/2012

Procedural Blank

(PB)

A PB was prepared with this analytical batch to ensure the sample extraction and analysis methods are free of contamination. Additionally, a Duxbury seawater blank, identified as BW547PB, was processed and analyzed with this batch.

<3 X MDL

Samples >3X PB

No exceedences noted.

No comments.

Laboratory Control Spike (LCS)

A LCS was prepared with this analytical batch. The percent recoveries of target analytes were calculated to measure accuracy.

50‐120% recovery

Surrogate

Surrogate compounds were added prior to extraction. The surrogate recoveries are calculated to measure extraction efficiency.

30‐150% recovery No exceedences noted.

Matrix Spike (MS) A matrix spike sample was prepared with this analytical batch. The percent recoveries of target analytes were calculated to measure data quality in terms of accuracy.

One exceedence noted.

Dieldrin was over‐recovered in the MS sample at 121%. All calibrations, integrations, and calculations were reviewed. Dieldrin was over‐recovered in bracketing CCVs. The recovery in the LCS sample was within criteria at 97%.

This compound was not detected in any field sample at a level above the reporting limit. Because it was over‐recovered, no additional corrective actions were taken.

Laboratory Triplicates

Triplicate extractions/analyses of each water and elutriate were prepared with this analytical batch. The relative standard deviation (RSD) between the three samples was calculated to measure data quality in terms of precision.

< 30% RSD

for analytes >10x the MDL

One primary exceedence noted.

The triplicate RSD for PCB Cl2(08) in elutriate samples N5394 was 74%. This congener was detected at 3 ng/L , 2.6 ng/L, and was not detected in one of the replicates, resulting in the high RSD. Because these are water samples they cannot be re‐processed. No further corrective actions taken. Two other control criteria exceedences are noted, for PCB Cl10(209) and 4,4’‐DDD, however the concentrations detected do not meet contingency criteria and therefore are not to be used for data quality assessment.

Standard Reference Material (SRM)

A standard reference material was prepared for this analytical batch to measure data in terms of analytical accuracy.

<30% difference evaluated for analytes >10x the

MDL

One exceedence noted.

2,4’‐DDD was over‐recovered in the SRM. This target pesticide co‐elutes with an uncertified PCB congener in the SRM (PCB 154). No further corrective action taken. Recoveries of this compound were within criteria in the LCS and MS samples.

Initial Calibration

(ICAL)

The GC/ECD was calibrated with six‐level quadratic forced calibration curve for all compounds using an instrument response factor (RF).

Mean ≤ 15% Indiv ≤ 25% R2 ≥ 0.995

Independent Calibration Check

(ICC)

The independent check was run after each initial calibration to verify the calibration. This standard is from a different source than the ICAL.

≤ 15% difference individual and mean

One exceedence noted.

Heptachor is over‐recovered in the ICC check. All integrations were reviewed.

This compound was not detected in any field sample and therefore no addition corrective actions were taken.

Continuing Calibration Verification (CCV)

Continuing calibration standards were run every 12 hours to ensure that initial calibration is still valid.

≤ 20% difference individual; <15% difference mean

Fourteen exceedences noted.

Several analytes were outside the quality control criteria, all over‐responding. In each case the analyte that was over‐recovered in the CCV was either not detected in any field sample, or the sample itself was re‐analyzed and bracketed by passing CCV standards. No further corrective actions required.

Procedural Blank-Milli- Q Water

BW546PB-P

PB

09/25/2012

09/25/2012

10/10/2012

ECD

NA

NA

LIQUID

1.00

L_LIQUID

NG/L_LIQUID

Procedural Blank- Duxbury Bay Water

BW547PB-P

PB

09/25/2012

09/25/2012

10/10/2012

ECD

NA

NA

LIQUID

1.00

L_LIQUID

NG/L_LIQUID

Client ID

Battelle ID

Sample Type

Collection Date

Extraction Date

Analysis Date

Analytical Instrument

% Moisture

% Lipid

Matrix

Sample Size

Size Unit-Basis

Units

Project Client: USACE/NYD

Project Name: DO#39 KvK and Anchorage Channel

Project Number: 100016704-0001 aldrin 0.32 U 0.32 U a-chlordane 0.34 U 0.34 U trans-nonachlor 0.58 U 0.58 U dieldrin 0.59 U 0.59 U

4,4'-DDT 0.27 U 0.27 U

2,4'-DDT 0.46 U 0.46 U

4,4'-DDD 0.54 U 0.54 U

2,4'-DDD 0.68 U 0.68 U

4,4'-DDE 0.34 U 0.34 U

2,4'-DDE 0.64 U 0.64 U

endosulfan I 0.52 U 0.52 U endosulfan II 0.41 U 0.41 U endosulfan sulfate 0.45 U 0.45 U heptachlor 0.49 U 0.49 U heptachlor epoxide 0.58 U 0.58 U

Cl2(8) 0.31 U 0.31 U

Cl3(18) 0.44 U 0.44 U

Cl3(28) 0.31 U 0.31 U

Cl4(44) 0.23 U 0.23 U

Cl4(49) 0.28 U 0.28 U

Cl4(52) 0.43 U 0.43 U

Cl4(66) 0.45 U 0.45 U

Cl5(87) 0.35 U 0.35 U

Cl5(101) 0.32 U 0.32 U

Cl5(105) 0.30 U 0.30 U

Cl5(118) 0.37 U 0.37 U

Cl6(128) 0.47 U 0.47 U

Cl6(138) 0.73 U 0.73 U

Cl6(153) 0.32 U 0.32 U

Cl7(170) 0.66 U 0.66 U

Cl7(180) 0.52 U 0.52 U

Cl7(183) 0.31 U 0.31 U

Cl7(184) 0.42 U 0.42 U

Cl7(187) 0.26 U 0.26 U

Cl8(195) 0.20 U 0.20 U

Cl9(206) 0.26 U 0.26 U

Cl10(209) 0.34 U 0.34 U

Not Surrogate Corrected

Analyzed By Restucci Jr, Richard

12/7/2012 L12-0552ECD-Master_128:FINAL

Procedural Blank-Milli- Q Water

BW546PB-P

PB

09/25/2012

09/25/2012

10/10/2012

ECD

NA

NA

LIQUID

1.00

L_LIQUID

NG/L_LIQUID

Procedural Blank- Duxbury Bay Water

BW547PB-P

PB

09/25/2012

09/25/2012

10/10/2012

ECD

NA

NA

LIQUID

1.00

L_LIQUID

NG/L_LIQUID

Client ID

Battelle ID

Sample Type

Collection Date

Extraction Date

Analysis Date

Analytical Instrument

% Moisture

% Lipid

Matrix

Sample Size

Size Unit-Basis

Units

Project Client: USACE/NYD

Project Name: DO#39 KvK and Anchorage Channel

Project Number: 100016704-0001

Surrogate Recoveries (%)

Cl3(34) 87 85

Cl6(152) 78 85

Not Surrogate Corrected

Analyzed By Restucci Jr, Richard

BW548LCS-P

LCS

09/25/2012

09/25/2012

10/11/2012

ECD

NA

NA

LIQUID

1.00

L_LIQUID

NG/L_LIQUID

Client ID

Battelle ID

Sample Type

Collection Date

Extraction Date

Analysis Date

Analytical Instrument

% Moisture

% Lipid

Matrix

Sample Size

Size Unit-Basis

Units Target % REC Qual

Project Client: USACE/NYD

Project Name: DO#39 KvK and Anchorage Channel

Project Number: 100016704-0001 aldrin 14.58 25.01 58 a-chlordane 20.66 25.15 82 trans-nonachlor 21.59 25.11 86 dieldrin 24.32 25.04 97

4,4'-DDT 29.03 25.03 116

2,4'-DDT 19.37 25.18 77

4,4'-DDD 23.59 25.04 94

2,4'-DDD 22.04 25.13 88

4,4'-DDE 20.95 25.03 84

2,4'-DDE 19.26 25.10 77

endosulfan I 22.06 25.02 88 endosulfan II 19.39 25.01 78 endosulfan sulfate 15.15 25.05 60 heptachlor 18.47 25.01 74 heptachlor epoxide 22.23 25.14 88

Cl2(8) 17.18 25.00 69

Cl3(18) 18.63 25.00 75

Cl3(28) 17.98 25.00 72

Cl4(44) 20.32 25.00 81

Cl4(49) 19.49 25.00 78

Cl4(52) 19.33 25.00 77

Cl4(66) 23.79 25.00 95

Cl5(87) 21.54 25.00 86

Cl5(101) 22.08 25.00 88

Cl5(105) 23.62 25.00 94

Cl5(118) 23.33 25.00 93

Cl6(128) 25.05 25.00 100

Cl6(138) 24.17 25.00 97

Cl6(153) 22.17 25.00 89

Cl7(170) 22.89 25.00 92

Cl7(180) 24.30 25.00 97

Cl7(183) 24.46 25.13 97

Cl7(184) 22.60 25.10 90

Cl7(187) 23.95 25.00 96

Cl8(195) 23.23 25.00 93

Cl9(206) 23.59 25.00 94

Cl10(209) 22.33 25.00 89

Not Surrogate Corrected

Analyzed By Restucci Jr, Richard

BW548LCS-P

LCS

09/25/2012

09/25/2012

10/11/2012

ECD