20080868 Ver 2_Draft EIS Additions_20061106

4709 COLLEGE ACRES DRIVE
1 SUITE 2
i N: ? R P O R AT E D WILMINGTON, NORTH CAROLINA 28403 1725
>f .
ENVIRONMENTAL CONSULTANTS TEL [phone]
FAX [phone]
[e-mail]
LETTER OF TRANSMITTAL
TO:
FROM:
DATE:
Mr. Tom Regan - PCS USA
Mr. William Schimming - PCS USA
Ms. Karen Torain - PCS USA
Mr. George House - BPMH
Mr. Derb Carter - SELC
Mr. Mike Wicker - USFWS
Dr. David McNaught - Env. Defense
Mr. Kyle Barnes - NC DWQ
Mr.Adam Daigneault - US EPA
USEPA, Office of Federal Activities
Ms. Robina Norman - Aurora Library
Ms. Mary Jane Carbo - BHM Reg. Library
Mr. Jeff Furness - PCS, Aurora.
Mr. Bob Finch - US ACE
Mr. Jimmie Overton - NC DWQ
Mr. Sean McKenna - NC DMF
Mr. Terry Moore - NC DCM
Sam Cooper/Julia Kirkland Berger
02 November 2006
Mr. Ted Tyndall - NC DCM
Mr. Ron Sechler - NMFS
Mr. John Domey - NC DWQ
Ms.Joanne Straight - Craven County Library
Ms Julia Cox - Pamlico County Library
Mr. David Moye - NC DCM
Ms. Becky Fox - US EPA
Mr. David Cox - NC WRC
Mr. Tom Walker - US ACE
Ms. Brooke Lamson - US ACE
Mr. David Lekson - US ACE
Ms. Emily Coffman - Faulkner $ Associates
Mr. Ross Smith - PCS, Aurora
Ms. Mary Alsentzer - PTR Foundation
Ms. Maria Tripp - NC WRC
Mr. Ricky Peed - NC DLR
SUBJECT: DEIS FOR PCS PHOSPHATE MINE CONTINUATON
WE ARE SENDING YOU: ® Enclosed via US Postal Service

1 )F tc.
Item Number Material for Dated
,
Description VM"WIQ AM
1 1 each of Volume I October Abstract and Summary to be inserted as first pages of
3 pages 2006 Volume 1
2 1 each of Volume II September Appendices 1, 2, 3, 4, & 5, to be inserted into APPENDIX
11 pages 2006 E of Volume 11, in the 1999 Final Report for the Cadmium
and Other Metals Study on and Adjacent to PCS
Phosphate Reclamation Areas (R-1, R-2, R-3, and the
Charles Tract), at the end of Attachment B.
THESE ARE TRANSMITTED: ® For review ® For your information ® For your action
REMARKS: Please insert these pages as appropriate in Volume I and Volume II:
Item 1 pages should be inserted in Volume I before the Table of Contents. These pages have a few
formatting and editing corrections compared to what Tom Walker provided to you via email and hard copy.
Item 2 pages were/may have been omitted by the DEIS printing

File: 1745.62.24
Cc: Ross Smith, PCS Phosphate
Signed:
Julia Kirkland Berger
A,'%N , '
1061 EAST INDIANTOWN ROAD • SUITE 100 • JUPITER, FLORIDA 33477-5143
TEL [phone] • FAX [phone] • [e-mail] • www.CZRINC.com
DRAFT
ENVIRONMENTAL IMPACT STATEMENT
FOR THE PCS PHOSPHATE MINE CONTINUATION
AURORA, NORTH CAROLINA
The responsible lead agency is the US Army Corps of Engineers, Wilmington District.
Abstract: The Potash Corporation of Saskatchewan Phosphate Division, Aurora Operation
(PCS) has applied for Department of the Army authorization pursuant to Section 404 of the Clean
Water Act and Section 10 of the Rivers and Harbors Act to advance its current mining operation
into a 3,608-acre area east of its current mining operation located north of Aurora, Beaufort
County, North Carolina. The proposed expansion would impact approximately 2,408 acres of
waters of the United States including wetlands adjacent to the Pamlico River and South Creek.
Pursuant to the National Environmental Policy Act, the Corps of Engineers has prepared this
Draft Environmental Impact Statement (DEIS) to examine the impacts of the proposed action and
alternatives to the proposed action.
Written comments pertinent to the proposed work, as outlined above, and the DEIS will be
received by the Corps of Engineers, Wilmington District, until 5pm, 27 January 2007. Comments
should be submitted to US Army Corps of Engineers, Wilmington District, Regulatory Division.
ATTN: File Number 2001-10096, Post Office Box 1890, Wilmington, NC 28402-1890. Questions
about the proposed action and DEIS can be directed to Mr. Tom Walker, Project Manager,
Regulatory Division, telephone: [phone] extension 222.
A public hearing on this project and the DEIS will be held at Southside High School located at 5700
Highway 33 East, Chocowinity, Beaufort County, NC on 14 December 2006 at 6:30 P.M.
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PCS Phosphate Mine Continuation DEIS a October 2006
Aurora, North Carolina
SUMMARY
On 2 November 2000, The Potash Corporation of Saskatchewan Phosphate Division, Aurora
Operation (PCS) applied for Department of the Army authorization to continue its phosphate
mining operation on the Hickory Point peninsula adjacent to the Pamlico River and South Creek,
north of Aurora, Beaufort County, North Carolina, once reserves are depleted under the existing
permitted area. The Corps circulated a Public Notice describing this application on 2 January
2001 (Action ID No. 200110096). PCS elected to further reduce proposed impacts to waters of
the US in response to comments on this Public Notice and submitted a revised permit application
on 13 August 2001. The Corps circulated a second Public Notice on 4 October 2001, describing
the revised application.
The PCS facility includes an open pit mining operation that supplies phosphate ore to its onsite
manufacturing facilities producing sulfuric acid, phosphoric acid, purified acid, liquid fertilizer,
superphosphoric acid, diammonium phosphate, defluorinated phosphate, animal feed and solid
fertilizers. Phosphate mining activities began at this site in 1965. On 27 August 1997, PCS was
issued a Department of the Army permit to impact 1,268 acres of waters and wetlands to continue
its mining operation into the current mine area. This action is more fully described in the August
1996 Final Environmental Impact Statement for the Texasgulf Inc. Mine Continuation. PCS is
nearing the end of the current mining area and is seeking to continue its mining operation into the
adjacent tract.
•
The proposed action includes a request for authorization to impact approximately 2,408 acres of
waters of the US including wetlands to continue the mine advance into a 3,608-acre area located
adjacent to the Pamlico River and several of its tributaries. The applicant's stated purpose and
need for this project is to continue mining its phosphate reserve in an economically viable fashion.
More specifically, the applicant's stated purpose and need is to implement a long-term systematic
and cost-effective mine advance within the project area for the ongoing PCS mine operation at
Aurora, NC. The waters and wetlands impacted by the proposed action have been categorized
into community types as follows:
1. Creeks/Open Water 11 acres
2. Brackish Marsh Complex 38 acres
3. Bottomland Hardwood Forest 102 acres
4. Herbaceous Assemblage 253 acres
5. Scrub-Shrub Assemblage 202 acres
6. Pine Plantation 514 acres
7. Hardwood Forest 508 acres
8. Mixed Pine-Hardwood Forest 564 acres
9. Pine Forest 195 acres
10. Ponds 19 acres
Total 2,408 acres
Pursuant to the National Environmental Policy Act (NEPA) federal agencies are required to
prepare an Environmental Impact Statement (EIS) for any agency action, including the issuance
of a permit, if that action may significantly affect the quality of the human environment. The
Corps of Engineers has prepared this draft Environmental Impact Statement to examine the
environmental and socioeconomic impacts of the proposed action and explore reasonable
alternatives. A public scoping meeting was held on 28 February 2001 and an interdisciplinary
Review Team (Review Team) comprised of representatives from other state and federal
regulatory and commenting agencies, environmental advocacy groups, the applicant, and CZR
Incorporated (CZR) (third party consultant to the Corps in accordance with RGL-05-08) was
PCS Phosphate Mine Continuation DEIS b October 2006
Aurora, North Carolina

formed. The purpose of the Review Team is to identify major issues to be addressed in the EIS
and to provide input on potential alternatives to be explored and potentially evaluated.
The Corps, working with the applicant and the Review Team, established a project area
comprised of three basic tracts; a 3,608-acre area east of the current operation and adjacent to
South Creek identified as the NCPC Tract, a 8,686-acre area south of the current operation and
south of NC Highway 33 identified as the S33 Tract, and an 2,806-acre area west of the current
operation and adjacent to Durham Creek identified as the Bonnerton Tract. The S33 Tract
contains fewer wetlands than either of the other tracts (S33 = 1,130 acres, NCPC = 2,408 acres,
and Bonnerton = 2,130 acres).
Within this project area, a No Action mining alignment and nine alternative mining alignments
have been identified for further study. A detailed description of each alternative can be found in
Section 2.0 and maps of each alternative can be found in Section 5.0 of the DEIS (pages 543
through 5-53). The No Action mining alignment is not an alignment that involves no mining but
rather an alignment that avoids all waters of the US and therefore requires no Department of the
Army authorization. Seven of the alternatives (DI-1 B, EAPA, EAPB, SCRA, SCRB, SJAA, SJAB)
involve some mining activity in each of the three tracts. All mining in the AP alternative is
contained within the NCPC Tract and the No Action and S33AP alternatives limit mining to only
the S33 Tract.
The applicant contends that the AP and EAPA alternatives are the only economically practicable
alternatives. The Corps has reviewed all information submitted by the applicant as well as other
available information regarding the economics of phosphate and phosphate mining. At this time,
the Corps concurs with the applicant that the AP and EAPA alternatives are economically
practicable and that the No Action, S33AP and DL1 B alternatives are not economically
practicable. The Corps has not concurred with the applicant's determination on the other
alternatives.
The DEIS was released Friday, 20 October 2006. The DEIS document and the public notice may
be viewed and downloaded from the Wilmington District's website at
http://www.saw.usace.army.miI/WETLANDS/index.html. The Corps is seeking public input on the
completeness of the document as well as the environmental and socioeconomic impacts of PCS'
proposed mine alignment and the various alternatives. A public hearing on this project will be
held 14 December 2006 and comments will be accepted until 27 January 2007.
•
PCS Phosphate Mine Continuation DEIS c October 2006
Aurora, North Carolina
•
•
0
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APPENDIX 1.
Quality assurance and quality control (QA/QC) data for the sediment metal analyses.

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•
1999 CZR Incorporated Cadmium Report Attachment B
Results for the Marine Sediment Standard Reference Material (SRM) BCSS-1. Mean and (Standard
Deviation). NRC is the National Research Council of Canada.
SRM Ag AI As Cd Cr Cu Fe Mo Se Zn
(Pgtg) N (Ng/9) W/O (ugtg) W/O (°/a) (Ng/g) (ug/g) (Ng1g)
NRC BCSS-1 0.13 6.18 11.2 0.24 124 19.5 3.24 1.91 0.49 116
This Study 0.12 6.26 10.7 0.23 120 19.5 3.32 1.94 0.49 119
0.09 6.17 12.2 0.24 111 18.5 3.22 2.05 0.47 114
- - - 0.23 - - - - - -
0.26 - - - - - -
Certified Mean 0.11 6.26 11.1 0.25 123 18.5 3.29 1.9" 0.43 119
Standard (0.03) (0.22) (14
Deviation ) (0.04) (4) (2.7) (0.10) - (0.06) (12)
Reference Value, not Certified.
Procedural Blanks.
Sample Ag AI As Cd Cr Cu Fe Mo Se Zn
(ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (r4ml) (ng/mL) (ng/mL)
Blank 1 0.08 N.D. N.D. N.D. N.D. N.D. 152 0.17 N.D. 19
Blank 2 0.04 N.D. N.D. N.D. N.D. N.D. 152 0.04 N.D. 8 is
Blank 3 N.D. N.D. N.D. 0.02 N.D. N.D. N.D. 0.09 0.77 3
Blank 4 - - - N.D. - - - - - -
Percent Spike Recovery.
Sample Element Spike Spike Recovered Percent Recovery
Station (ng) (ng)
1 Ag 1.00 0.92 92.0
6 Ag 1.00 0.94 94.0
R-3 North End Ag 1.00 0.95 95.0
1 AI 10000 9760 97.6
3 Ai 10000 9140 91.4
R-3 North End AI 10000 9370 93.7
1999 CZR Incorporated Cadmium Report Attachment B
Percent Spike Recovery (continued).

Sample Element Spike Spike Recovered Percent Recovery
Station (ng) (ng)
1 As 10.0 9.0 90.0
6 As 10.0 9.8 98.0
R-3 North End As 10.0 9.4 94.0
1 Cd 125 117 93.6
3 Cd 125 125 100.0
8 Cd 0.250 0.218 87.2
R-3 North End Cd 0.250 0.237 94.8
1 Cr 2500 2530 101.2
3 Cr 2500 2430 97.2
R-3 North End Cr 2500 2510 100.4
1 Cu 250 255 102.0
3 Cu 250 248 99.2
R-3 North End Cu 250 251 100.4
1 Fe 2500 2480 99.2
3 Fe 2500 2450 98.0
R-3 North End Fe 2500 2400 96.0
1 Mo 5.00 4.79 95.8
6 Mo 5.00 5.11 102.2
R-3 North End MO 5.00 4.65 93.0
1 Se 10.0 9.1 91.0
6 Se 10.0 9.3 93.0
R-3 North End Se 10.0 10.5 105.0
1 Zn 250 242 96.8
3 Zn 250 252 100.8
R-3 North End Zn 250 242 96.8
is
1999 CZR Incorporated Cadmium Report Attachment B
Analytical Precision as RSD**.
Sample
Station Ag Al
As
Cd
Cr
Cu
Fe
Mo
Se
Zn
7 6.7 2.8 1.4 0.0 2.8 3.8 2.8 2.8 1.8 2.8
17 12.9 2.8 6.1 23.6 1.0 0.8 0.0 0.0 0.0 6.2
** RSD = (standard deviation / mean) X 100
Method Detection Limits (MDL).
Ag A! As Cd Cr Cu Fe MO Se Zn
(Ng/g) N (pg/g) (pg/g) (pg/g) (Ng/g) M (pg/g) (Ng/g) (Ng/g)
MDL*** 0.01 0.006 0.1 0.002 6.7 1 0.001 0.03 0.03 1
*** Based on 0.45 grams of sediment.
r-,
1999 CZR Incorporated Cadmium Report Attachment B

APPENDIX 2.
Quality assurance and quality control (QA/QQ data for the dissolved metal analyses.

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1999 CZR Incorporated Cadmium Report Attachment B
Results for the Seawater Standard Reference Material (SRM) CASS-3 and Trace Metals in Elements
#1643d. Mean and (Standard Deviation). (NRC = National Research Council of Canada ; NIST = National
Institute of Standards and Technology).
SRM As Cd Cr Cu Mo Zn
(N9,L) (pg/L) (u9/) (pg/L) (pg/L) (N9/9)
NRC CASS-3 1.12 0.031 0.095 0.482 - 1.02
This Study 1.12 0.032 0.095 0.551 - 1.05
1.14 0.030 0.097 0.533 - 1.03
1.12 0.029 0.095 0.545 - 1.06
1.08 0.032 0.094 0.549 - 1.28
Certified Mean 1.09 0.030 0.092 0.517 8.95 1.24
Standard Deviation (0.07) (0.005) (0.006) (0.062) (0.26) (0.25)
NIST #1643d - - - - 113.9 -
This Study - - - - 112.5 -
Certified Mean 56.02 6.47 18.53 20.5 112.9 72.47
Standard Deviation (0.73) (0.37) (0.20) (3.8) (1.7) (0.65)
Procedural Blanks.
Sample As Cd Cr Cu MO Zn
(pg/L) (leg/) (pg/L) (pg/L) (pg/L) (pg/L)
Blank 1 N.D. 0.002 0.104 0.034 N.D. 0.086
Blank 2 N.D. 0.001 0.107 0.029 N.D. 0.117
Blank 3 N.D. 0.001 0.127 0.057 N.D. 0.125
Blank 4 N.D. 0.002 0.118 0.040 - 0.093
Analytical Precision as RSD*.
Sample Station As Cd Cr Cu Mo Zn
22 Surface 4.7 9.4 9.4 2.1 0.0 1.6
23 Surface 4.2 7.4 7.9 1.7 0.0 0.5
RSD = (standard deviation / mean) X 100
1999 CZR Incorporated Cadmium Report Attachment B
Percent Spike Recovery.
Sample
Station
Element
Spike
(ng)
Spike Recovered
(ng)
Percent Recovery
16 As 1590 1480 93.1
22 As 1620 1520 93.8
' GWM 4B As 1640 1570 95.7
Archbell Point As 1650 1530 92.7
16 Cd 12.0 12.4 103.3
22 Cd 14.4 13.6 94.4
GWM 4B Cd 12.8 12.8 100.0
Archbell Point Cd 9.6 10.4 108.3
16 Cr 81.2 80.8 99.5
22 Cr 81.6 86.0 105.4
GWM 4B Cr 78.8 73.6 93.4
Archbell Point Cr 80.0 82.0 102.5
16 Cu 200 182 91.0
22 Cu 203 184 90.6
GWM 413 Cu 199 183 92.0
Archbell Point Cu 200 199 99.5
3 Mo 333 327 98.2
9 Mo 572 569 99.5
Charles Tract #1 Mo 364 344 94.5
16 Zn 627 629 100.3
22 Zn 579 530 91.5
GWM 4B Zn 587 641 109.2
Archbell Point Zn 764 707 92.5

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1999 CZR Incorporated Cadmium Report Attachment B
Method Detection Limits (MDL).
As Cd Cr Cu Mo Zn
(u9/L) (u9AL) (N9/L) (N9tL) (Ng/L) (u9/L)
MDL'" 0.008 0.001 0.005 0.003 0.13 0.10
Based on 400 ml aliquots for extracted metals (As, Cd, Cr, Cu and Zn), and no dilution for Mo.

?J
1999 CZR Incorporated Cadmium Report Attachment B
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APPENDIX 3.
Quality assurance and quality control (QA/QC) for the particulate metal analyses.

•
CJ
1999 CZR Incorporated Cadmium Report Attachment B
t
Results for the Standard Reference Material (SRM ) Buffalo River Sediment #2704 and Trace Elements
in Water #1643d. Mean and (Standard Deviation). (KIST = National Institute of Standards and Technology).
SRM AI As Cd Cr Cu Fe Mo Zn
N (Ng/g) (Ng/g) (Ng/g) (pg/g) (%) (Pg/g) (Ng/g)
NIST #2704 6.01 23.9 3.67 136 99.6 4.09 3.5 434
This Study 6.13 24.2 3.61 139 100.6 4.16 3.5 443
5.95 23.8 3.65 139 99.5 4.08 4.4 446
6.09 24.0 3.60 138 101.9 4.17 3.8 444
6.05 23.7 3.59 132 101.3 4.14 4.6 443
Certified Mean 6.11 23.4 3.45 135 98.6 4.11 - 438
Standard Deviation (0.16) (0.8) (0.22) (5) (5.0) (0.11) - (12)
NIST #1643d - - - - - - 111.9 -
This Study - - - - - - 111.5 -
- - - - - - 112.5 -
Certified Mean - - - - - - 112.9 -
Standard Deviation - - - - - - (1.7) -
Procedural Blanks.
Sample AI As Cd Cr Cu Fe Mo Zn
(ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL)
Blank 1 N.D. 0.61 N.D. 0.05 0.17 30 0.05 20
Blank 2 N.D. 0.30 0.01 0.03 N.D. N.D. 0.05 20
Blank 3 N.D. 0.56 N.D. 0.02 0.29 N.D. 0.13 20
Blank 4 N.D. 0.40 N.D. N.D. 0.52 N.D. N.D. 17

Method Detection Limits (MDL).
Al As Cd Cr Cu Fe Mo Zn
(%) (Ng/g) (Ng/g) (pg/g) (Vg/g) (%) (pg/g) (Ng/g)
MDL* 0.02 5.5 0.05 0.5 0.7 0.02 0.7 35
Based on 1 mg of suspended matter.
0
Percent Spike Recovery.

Sample Element Spike Spike Recovered Percent Recovery
Station (ng) (ng)
3 Al 2500 2470 98.8
12 AI 2500 2540 101.6
20 AI 1250 1170 93.6
23 Bottom AI 1250 1240 99.2
4 Bottom As 10.0 9.7 97.0
12 As 10.0 9.3 93.0
22 Surface As 10.0 9.9 99.0
23 Bottom As 10.0 10.2 102.0
4 Bottom Cd 0.50 0.54 108.0
12 Cd 0.50 0.53 106.0
22 Surface Cd 0.50 0.53 106.0
23 Bottom Cd 0.50 0.54 108.0
4 Bottom Cr 1.00 0.93 93.0
. 12 Cr 2.00 1.80 90.0
22 Surface Cr 1.00 0.94 94.0
23 Bottom Cr 1.00 0.91 91.0
4 Bottom Cu 5.00 4.77 95.4
12 Cu 5.00 4.51 90.2
22 Surface Cu 5.00 4.52 90.4
23 Bottom Cu 5.00 4.55 91.0
3 Fe 500 459 91.8
12 Fe 2500 2400 96.0
20 Fe 1250 1190 95.2
23 Bottom Fe 1250 1210 96.8

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1999 CZR Incorporated Cadmium Report Attachment B
Percent Spike Recovery (continued).
Sample Element Spike Spike Recovered Percent Recovery
Station (ng) (ng)
4 Bottom Mo 1.00 0.95 95.0
12 Mo 1.00 0.94 94.0
22 Surface Mo 1.00 0.99 99.0
23 Bottom Mo 1.00 0.96 96.0
3 Zn 125 120 96.0
12 Zn 125 114 91.2
20 Zn 125 130 104.0
23 Bottom Zn 125 124 99.2
Analytical Precision as RSD"*.
Sample Al As Cd Cr Cu Fe MO Zn
Station

16 2.7 1.0 5.2 7.2 2.7 6.4 10.9 0.6
22 Surface 9.6 1.6 7.3 1.9 0.3 2.8 0.0 6.8
22 Bottom 0.4 1.5 5.9 0.7 2.7 0.5 1.6 2.4 •
23 Surface 6.0 7.1 6.6 3.4 1.4 2.4 6.7 4.7
** RSD = (standard deviation / mean) X 100
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1999 CZR Incorporated Cadmium Report AttachmentB

APPENDIX 4.
Quality assurance and quality control (QA/QC) data for the tissue metal analyses.
is
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1999 CZR Incorporated Cadmium Report Attachment B
Results for the Standard Reference Material (SRM) DORM-2 (Dogfish Muscle). Mean and (Standard
Deviation). (NRC = National Res earch Cou ncil of Can ada).
SRM Ag As Cd Cr Cu Fe Se Zn
(p9/g) (p9/g) (pg/g) (pg/g) (pg/g) (p9/g) (pg/g) (pg/9)
NRC DORM-2 0.043 18.9 0.045 30.0 2.48 136 1.44 24.1
This Study 0.036 18.5 0.049 32.8 2.30 134 1.40 25.1
0.031 18.8 0.045 29.8 2.27 137 1.36 24.2
0.034 17.4 0.042 29.7 2.31 144 1.34 24.6
0.034 18.4 0.046 31.2 2.37 133 1.48 24.4
0.034 18.2 0.046 31.1 2.18 135 1.45 25.4
Certified Mean 0.041 18.0 0.043 34.7 2.34 142 1.40 25.6
Standard Deviation (0.013) (1.1) (0.008) (5.5) (0.18) (10) (0.09) (2.3)
Procedural Blanks.
Sample Ag As Cd Cr Cu Fe Se Zn
(ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL) (ng/mL)
Blank 1 0.09 N.D. 0.01 0.26 N.D. 121 0.31 22
Blank 2 0.07 N.D. 0.01 0.30 N.D. 121 N.D. 30
Blank 3 0.04 N.D. N.D. 0.29 N.D. N.D. N.D. 27
Blank 4 0.05 N.D. 0.01 0.26 N.D. N.D. N.D. 42
Blank 5 0.07 0.81 0.02 0.21 N.D. N.D. N.D. 4
Blank 6 0.10 N.D. 0.02 0.19 N.D. N.D. N.D. 4
Analytical Precision as RSD`.
Sample Station Organism Ag As Cd Cr Cu Fe Se Zn
12 male crab 1.9 3.5 8.3 5.7 3.1 2.7 13.1 0.0
Durham Greek male crab 4.6 3.1 5.4 1.3 4.3 2.9 2.1 1.1
Durham Creek clams 6.9 0.9 7.5 2.8 1.4 3.4 5.7 0.6
Long Creek Pumpkinseed N.D. 7.9 6.3 2.8 6.5 6.7 4.7 1.6
Pamlico River Longnose Gar 17.7 4.7 8.3 2.1 3.0 2.2 2.2 3.1
RSD = (standard deviation / mean) X 100
1999 CZR Incorporated Cadmium Report Attachment B

Percent Spike Recovery.
Sample Station &
Organism

is
Element Spike Spike Recovered Percent Recovery
(ng) (ng)
7A, Crab male Ag 1.00 0.92 92.0
12, Crab male Ag 1.00 0.91 91.0
Short Creek, Clam Ag 1.00 0.91 91.0
Long Creek, Clam Ag 1.00 0.93 93.0
Long Creek, Crab Ag 1.00 0.95 95.0
Upper Bond Creek, Crab Ag 1.00 0.90 90.0
7A, Crab male As** 10.0 6.8 68.0
12, Crab male As** 10.0 7.1 71.0
Short Creek, Clam As** 20.0 15.4 77.0
Long Creek, Clam As** 20.0 18.1 90.5
Long Creek, Crab As 10.0 9.1 91.0
Upper Bond Creek, Crab As 10.0 9.3 93.0
7A, Crab male Cd** 0.250 0.195 78.0
12, Crab male Cd** 0.125 0.089 71.2
Short Creek, Clam Cd 0.100 0.102 102.0
Long Creek, Clam Cd 0.250 0.228 91.2
Long Creek, Crab Cd 0.100 0.091 91.0
Upper Bond Creek, Crab Cd 0.100 0.092 92.0
7A, Crab male Cr 2.50 2.25 90.0
12, Crab male Cr 2.50 2.33 93.2
Short Creek, Clam Cr 1.00 1.08 108.0
Long Creek, Clam Cr 1.00 0.94 94.0
Long Creek, Crab Cr 1.00 0.90 90.0
Upper Bond Creek, Crab Cr 1.00 0.97 97.0
** Metal concentrations reported from these tissue digests been corrected for percent spike recovery.
•
1999 CZR Incorporated Cadmium Report Attachment B
Percent Spike Recovery (continued).
Sample Station &
Organism Element Spike
(ng) Spike Recovered
(ng) Percent Recovery
7A, Crab male Cu 500 479 95.8
12, Crab male Cu 500 497 99.4
Short Creek, Clam Cu 250 239 95.6
Long Creek, Clam Cu 250 250 100.0
Long Creek, Crab Cu 250 244 97.6
Upper Bond Creek, Crab Cu 250 251 100.4
7A, Crab male Fe 1000 1030 103.0
12, Crab male Fe 1000 1010 101.0
Short Creek, Clam Fe 1000 1050 105.0
Long Creek, Clam Fe 1000 960 96.0
Long Creek, Crab Fe 1000 995 99.5
Upper Bond Creek, Crab Fe 1000 982 982
7A, Crab male Se 10.0 10.6 106.0
12, Crab male Se 10.0 10.2 102.0
Short Creek, Clam Se 10.0 10.3 103.0
Long Creek, Clam Se 10.0 10.8 108.0
Long Creek, Crab Se 10.0 10.2 102.0
Upper Bond Creek, Crab Se 10.0 10.1 101.0
7A, Crab male Zn 500 497 99.4
12, Crab male Zn 500 475 95.0
Short Creek, Clam Zn 250 251 100.4
Long Creek, Clam Zn 250 241 96.4
Long Creek, Crab Zn 125 115 92.0
Upper Bond Creek, Crab Zn 125 117 93.6
1999 CZR Incorporated Cadmium Report Attachment B
C7
n
U
Method Detection Limits (MDL).
Ag As Cd Cr Cu Fe Se Zn
(pg/g) (pg/g) (pg/g) (Ngfg) (Ng/g) (pg/g) (pg/g) (Pg?9)
MDL""" 0.002 0.029 0.0003 0.003 0.7 2.5 0.05 0.4
Based on 0.5 grams of tissue (dry weight).

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1999 CZR Incorporated Cadmium Report Attachment B

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APPENDIX 5.
Evaluation of quality assurance and quality control (QA/QC) results for metal analyses.
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1999 CZR Incorporated Cadmium Report Attachment B
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The QA/QC results from the source study are evaluated based on the Data Quality Objectives
(DQOs) listed below in Table 1.
All initial calibrations used met the requirement that (r) be greater than 0.999.
All continuing calibrations were within a 10% deviation.
Sediment Metals.
Results for the sediment SRMs met the DQOs. All results were within the certified limits
established by the National Research Council of Canada (NRC).
None of the sediment metal blanks exceeded 5x the MDLs. Reviewers should note that blanks are
in ng/mL (ppb) and MDLs are in µg/g (ppm) and % (where I % equals 10,000 gg/g). Therefore, the
Ag concentration of Blank #1, at 0.08 ng/mL (ppb), would be 0.00008 gg/mL (ppm). Corrected to
µg/g material, the blank is roughly equivalent to 0.003 µg/g and 3x lower than the MDL for the
sediment method. The highest blank concentrations were observed for Fe, 152 ng/mL in Blanks # 1
and #2. Converted to pg/g material, this concentration is roughly equivalent to 7 µg/g, and less than
the MDL value of 0.001% (10 gg/g). The blank concentrations for Cd, Mo, Se and Zn are all
similarly below their respective MDL values.
Matrix spike recoveries for the sediment samples were within the range of 90-110% for all elements
except Cd from Station 8 (87.2%). No spike correction was applied because the other spiked
samples all exceeded 90% recovery for Cd.
Analytical precision from laboratory duplicates was better than 10% for all elements except Ag and
Cd in sediment from Station 17 (12.9% and 23.6%, respectively). The lower precision for these
elements in this sample is due to their very low concentrations. The DQO requirements for
• analytical precision were met (Table 1).
Dissolved Metals.
Results for the dissolved metal SRMs met the DQOs. All results were within the certified limits
established by the NRC and National Institute of Standards and Technology (MIST).
None of the dissolved metal blanks exceeded 5x the MDLs for As, Cd, Mo and Zn. Reviewers
should note that both the dissolved blank metal concentrations and MDL values are in µg/L (ppb).
The greatest blank concentrations relative to MDL values were observed for Cr, at 0.104-0.127 µg/L.
The bulk of the Cr blank is derived from the membrane filters required in the
extraction/preconcentration procedure. These fitters are acid-washed prior to use, but a small
amount of residual Cr remains. This small, residual Cr cannot be removed from the membrane
material without significantly damaging the filter. The blank concentrations for Cu also exceed 5x
the MDL. In this case, the blank is not filter related and comes from the reagents needed to preform
the metal extraction/preconcentration. Reagents from several commercial sources were tested and
only the highest purity materials were selected for use.
Matrix spike recoveries for the dissolved metal samples were within the range of 90-110% for all
elements.
Analytical precision from laboratory duplicates was better than 10% for all elements.
Particulate Metals.
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1999 CZR Incorporated Cadmium Report Attachment B
Results for dissolved metals in the SRMs met the DQOs. All results were within the certified limits
established by the NRC and NIST.
None of the particulate metal blanks exceeded 5x the MDLs. Reviewers should note that blanks are
in ng/mL (ppb) and MDLs are in pg/g (ppm) and % (where I% equals 10,000 µg/g). Therefore, the
As concentration of Blank #1, at 0.61 ng/mL (ppb), would be 0.00061 µg/mL (ppm). Corrected to
µg/g material, the blank is roughly equivalent to 3 gg/g and 2x lower than the MDL value. The
greatest blank concentration was again observed for Fe, 30 ng/mL in Blank #1. Converted to gg/g
material, this concentration is equivalent to 30 gg/g, and -7x less than the MDL value of 0.02% (200
µg/g). Blank concentrations for Cd, Cr, Cu, Mo and Zn are all below their respective MDL values.
Matrix spike recoveries for the particulate metal samples were within the range of 90-110% for all
elements.
Analytical precision from laboratory duplicates was better than 10% for all elements except Mo in
particulate samples from Station 16 (10.91/6); however, the DQO requirements for analytical
precision were met (Table 1).
Tissue Metals.
Results for metals in the tissue SRMs met the DQOs. All results were within the certified limits
established by the NRC.
- None of the tissue metal blanks exceeded 5x the MDLs. Reviewers should note that blanks are in
ng/mL- (ppb) and MDLs are in ttg/g (ppm) dry weight. Therefore, the Ag concentration of Blank # 1,
at 0.09 ng/mL (ppb), would be 0.00009 gg/mL (ppm). Corrected to gg/g material, the blank is
roughly equivalent to 0.004 gg/g and 2x greater than the MDL value. The greatest blank
concentration was again observed for Fe, 121 ng/mL in Blanks #1 and #2. Converted to gg/g
material, this concentration is equivalent to 5 gg/g, and 2x greater than the MDL value of 2.5 µg/g.
Of the remaining analytes, tissue blank concentrations of Cd, Cu and Se were below their respective
MDL values; As, Cr and Zn blank concentrations ranged from 1-4x their MDL values. Thus, the
DQO requirements were met.
Matrix spike recoveries for the tissue metal samples were within the range of 90-110% for all
elements except As in two tissue digests (averaging 69.5% and 83.7%, respectively) and Cd in one
tissue digest (averaging 74.61/6). Arsenic and Cd concentrations in these tissue digests have been
corrected for their low spike recovery. Empirically, the low recoveries seem to havebeen associated
with tissues and organisms that were noticeably oily in texture. A modification was made to the
digestion procedure to correct this problem; the amount of hydrogen peroxide used to oxidize the
tissue samples was doubled. Subsequently, all matrix spike recoveries were within the desired 90-
110% range.
Analytical precision from laboratory duplicates was better than 10% for all elements except Ag in
Longnose Gar from the Pamlico River (17.7%) and Se in crab tissue from Station 12 (13.1%). In
the case of Ag, the comparatively low precision is due to the very low tissue concentrations present.
For Se in crab tissue from Station 12, the relatively low precision may be due to inhomogeneity
between the samples of crab flesh; however, the DQO requirements for analytical precision were met
(Table 1).
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1999 CZR Incorporated Cadmium Report Attachment B
Table 1 Data Quality Objectives and Criteria
Element or Minimum Frequency Data Quality
Sample Type Objective/Acceptance Criteria
Initial Calibration Prior to every batch 3-5 point curve depending on the
of samples element and a blank. Standard
curve correlation coefficient
r z 0.999 for all analytes.
Continuing Must end every % RSD s 15% for all analytes
Calibration analytical sequence;
for flame, repeat all
standards every 5
samples; for graphite
furnace and ICP-MS
recheck standard
after every 10 samples
SRMs from NRC One per batch of Values must be within f 20% of
and NIST 20 samples accepted values for >85% of the
certified analytes and within f 25%
for Hg.
• Method Blank One per batch of No more than 2 analytes to exceed
20 samples 5x MDL unless analyte not detected
in associated sample(s)
Matrix Spike and One per batch of %RSD 80-120%
Spike Method Blank 20 samples
Lab Duplicate One per batch of RSD <25% for 65% analytes
20 samples
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1999 CZR Incorporated Cadmium Report Attachment B