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ANALYTICAL REPORT
PFOA/PFOS Analysis Lot# : D7J150133
Nicki Smith QC Laboratories, Inc. 1205 Industrial Highway. Southampton, PA 18966 TestAmerica Denver
November 5, 2007
4955 Yatrow Street
Arvada, CO 80002
tel 303.736.0100 .
fax 303.431.7171
w w w .testam ericainc.com
DEP2-SDWB-000239
Table Of Contents
Standard Deliverables
Report Contents
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Table of Contents Case Narrative Executive Summary - Detection Highlights Methods Summary Method/Analyst Summary Lot Sample Summary Analytical Results QC Data Association Summary Chain-of-Custody
Total Number of Pages
DEP2-SDWB-000240
Case Narrative
D 7 J1 50133
TestAmerica Denver utilizes USEPA approved methods in all analytical w ork. The samples presented in this report were analyzed fo r the parameters listed on the m ethods summary page in accordance with the methods indicated. Dilution factors and footnotes are provided on each datasheet to assist in the interpretation o f the results.
The results relate only to the samples in this report and meet all requirem ents o f NELAC. All data have been reviewed for compliance with the laboratory QA/QC plan and have found to be compliant with laboratory protocols with any exceptions noted below.
Please note that Non-Detect (ND) results have been evaluated down to the Method Detection Lim it (MDL) and should be considered ND a t the MDL. Unless otherwise noted, results for solids have been dry weight corrected.
This report shall not be reproduced except in full, without the written approval o f the laboratory.
Sam ple A rrival and R eceipt The following report contains the analytical results for one sample received 10/15/07, according to documented sample acceptance procedures. The sample was received in good condition at a temperature o f 16.8C. The receipt tem peraturels above the recommended temperature range o f 2-6C. The client was notified. No other anomalies were encountered during sample receipt.
Standards Analytical standards were prepared using the acid form o f the compound perfluorooctanoie acid (PFOA). PFOS is a commercial prepared and certified solution.
Perfluoro-n-[1I2,3,4-'3C,I]octanoic acid was introduced at the extraction step and was used as an internal standard fo r quantitation o f PFOA. Perfluoro-1-[1,2,3,4-13C4]octanatesulfonate was introduced at the extraction step and was used as an internal standard fo r quantitation of PFOS.
Sample Extraction and Analysis The sample presented in this report was analyzed for the target analyte by TestAmerica Denver's SOP DEN-LC-0012A.
For water samples a 250 mL aliquot o f each sample is acidified with 1 mL o f 6N HCI solution and it is extracted using solid phase extraction technique with methanol conditioned C18 cartridges. Each sam ple is spiked with the internal standard, prior to extraction. A fter the sample is passed through the cartridge, the analytes are eluted with 4 mL o f methanol. The final volume is brought to 5 mL using m ethanol and the extract Is analyzed by LC/MS/MS.
M ethod QC Sam ples The Method Blank is processed reagent water spiked with surrogate and prepared with each batch of 20 samples of the same matrix. The method blank was non-detect at the reporting lim it.
Each batch is prepared with a Laboratory Control Sample (LCS). The recoveries of two concentration levels o f Laboratory Control Samples were within control lim its.
DEP2-SDWB-000241
Analytical Comments The internal standard recovery fo r 13C4 PFOS was below the lower control lim it in the method blank associated w ith QC batch 7289213. The internal standard was in control in the associated sam ple and PFOS was non-detect; therefore, no corrective action was taken. The method required MS/MSD could not be performed for this batch, due to insufficient sample volume subm itted. The acceptable LCS analyte recoveries for two sets o f samples provide evidence that the laboratory is perform ing the method within acceptable guidelines. No other anomalies were observed.
DEP2-SDWB-000242
EXECUTIVE SUMMARY - Detection Highlights
D7J150133
PARAMETER_______________ L2468313-1 10/10/07 07:30 001
PFOA
RESULT
REPORTING LIMIT___ UNITS
ANALYTICAL METHOD
0.0082 J 0.010
ug/L
DEN -LC-0012
DEP2-SDWB-000243
METHODS SUMMARY
D7J150133
ANALYTICAL PARAMETER____________________________________________ METHOD______
LC/MS/MS, PFOA
DEN -LC-0012
References:
DEN Severn Trent Laboratorea, Denver, Facility Standard Operating Procedure.
PREPARATION METHOD
DEP2-SDWB-000244
METHOD / ANALYST SUMMARY
D7J150133
ANALYTICAL METHOD__________________________ ANALYST_________________________
DEN -LC-0012
Jaqueline Bonnett
References:
DEN Severn Trent Laboratores, Denver, Facility- Standard Operating Procedure.
ANALYST ID_____
003S01
DEP2-SDWB-000245
SAMPLE SUMMARY
D7J150133
SAMPLED SAMP
WO # SAMPLE# CLIENT SAMPLE ID_______________________________________ ____________ DATE
TIME
J804C 001 L2468313-1
10/10/07 07:30
NOTE(S) ;_____________________________________________________________________________________
- The analytical results of the samples listed above are presented on the following pages. All calculations are performed before rounding to avoid round-off errors in calculated results. - Results noted as "ND" were not detected at or above the stated limit. - This report must not be reproduced, except in full, without die written approval of die laboratory. - Results for the following parameters are never reported on a dry weight basis: color, corrosivity, density, flashpoint, ignitability, layers, odor, paint filter test, pH, porosity pressure, reactivity, redox potential, specific gravity, spot tests, solids, solubility, temperature, viscosity, and weight.
DEP2-SDWB-000246
QC Laboratories
Client Sample ID: L2468313-1
HPLC
Lot-Sample # -- Date Sampled-- Prep Date..... Prep Batch # -. Dilution Factor
D 7 J 1 5 0 1 3 3 -001 10/10/07 07:3' 10/16/07 7289213 1
Work Order # __ Date Received.. Analysis Date.. Analysis Time..
M e t h o d ........
J804C1AA 10/15/07 10/25/07 14:58
DEN -LC-0012
Matrix
PARAMETER PFOA PFOS
RESULT 0.0082 J ND
REPORTING LIMIT 0.010 0.010
UNITS ug/L ug/L
SURROGATE 13C4 PFOA 13C4 PFOS
PERCENT RECOVERY 82 63
RECOVERY LIMITS (SO - 200) (50 - 200)
NOTE(S) :______________ J Estimated result. Result Is less than RL.
: WATER
DEP2-SDWB-000247
QC DATA ASSOCIATION SUMMARY
D7J150133
Sample Preparation and Analysis Control Numbers
SAMPLE# 001
MATRIX WATER
ANALYTICAL METHOD
DEN -LC-0012
LEACH BATCH #
PREP BATCH #
72892X3
MS RUN#
DEP2-SDWB-000248
METHOD BLANK REPORT
HPLC
Client Lot #...: D7J150133 MB Lot-Sample #: R7J160000-213
Analysis Date..: 10/25/07 Dilution Factor: 1
Work Order #. ..: J82N41AA
Prep Date -- .,. 10/16/07 Prep Batch #.,. 7289213
M a t r i x .........: WATER Analysis T i m e ..: 12:49
PARAMETER PFOA PFOS
RESULT ND ND
REPORTING
LIMIT
UNITS
0.010
ug/L
0.010
ug/L
METHOD DEN -LC-0012 DEN -LC-0012
SURROGATE 3C4 PFOA 13C4 PFOS
PERCENT RECOVERY 63 46 *
RECOVERY LIMITS (50 - 200) (50 - 200)
NOTE(S) :_______________________________________ Calculations are performed before rounding to avoid round-off et rots in calculated resells. * Surrogale recovery is outside slated control limits.
DEP2-SDWB-000249
LABORATORY CONTROL SAMPLE EVALUATION REPORT
HPLC
Client Lot #.-.: D7J150133
Work Order #...
LCS Lot-Sample#t R7J160000-213
Prep Da t e ..... : 10/16/07
Analysis Date..
Prep Batch #- -.: 7209213
Analysis Time..
Dilution Factor; 1
J82N41AC
10/25/07 13:05
Matrix
PARAMETER PFOA PROS
PERCENT RECOVERY 97 92
RECOVERY LIMITS (70 - 130) (39 - 120)
METHOD______ DEN -LC-0012 DEN -LC-0012
SURROGATE 13C4 PFOA 13C4 PFOS
PERCENT RECOVERY 70 61
RECOVERY LIMITS (50 - 200) (50 - 200)
NOTE(S): ______________________________________ Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters
: WATER
DEP2-SDWB-000250
LABORATORY CONTROL SAMPLE DATA REPORT
HPLC
Client Lot #... LCS Lot-Sample# Prep Date...... Prep Batch #... Dilution Factor
PARAMETER PFOA PFOS
D7J150133
Work Order #...: J82N41AC
Matrix........ .: WATER
R7J160000-213
10/16/07
Analysis Date..: 10/25/07
7289213
Analysis Time..: 13:05
1
/
SPIKE
MEASURED
PERCENT
AMOUNT
AMOUNT
UNITS
RECOVERY METHOD
0.200
0.194
ug/L
97
DEN -LC-0012
0.200
0.183
ug/L
92
DEN -LC-0012
SURROGATE 13C4 PFOA 13C4 PFOS
PERCENT RECOVERY 70 61
RECOVERY LIMITS (50 - 200) (50 - 200)
NOTECS) :
Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters
DEP2-SDWB-000251
LABORATORY CONTROL SAMPLE EVALUATION REPORT
HPLC
Client Lot LCS Lot-Sample#: Prep Da t e..... : Prep Batch #...: Dilution Factor:
D7J250133
Work Order # --
R7J160000-213
10/16/07
Analysis Date..
7289213
Analysis Time..
1
J82N41AD
10/25/07 13:21
Matrix
PARAMETER PFOA PFOS
PERCENT RECOVERY 101 78
RECOVERY LIMITS (70 - 130) (39 - 120)
METHOD_______ DEN -LC-0012 DEN -LC-0012
SURROGATE 13C4 PFOA 13C4 PFOS
PERCENT RECOVERY 69 59
RECOVERY LIMITS (50 - 200) (50 - 200)
NOTE(S):
________________________
Calculations are performed before rounding to avoid round-off errors In calculated results.
Bold print denotes control parameters
; WATER
DEP2-SDWB-000252
LABORATORY CONTROL SAMPLE DATA REPORT
HPLC
Client Lot #...: D7J150133
Work Order
J82N41AD
LCS Lot-Sample#: R7J160000-213
Prep Date..... : 10/16/07
Analysis Date..: 10/25/07
Prep Batch # -- : 7289213
Analysis Time..: 13:21
Dilution Factor: 1
Matrix........ : WATER
PARAMETER PFOA PFOS
SPIKE AMOUNT 0.0200 0.0200
MEASURED AMOUNT 0.0202 0.0157
UNITS ug/L ug/L
PERCENT RECOVERY 101 78
method' DEN -LC-0012 DEN -LC-0012
SURROGATE 13C4 PFOA 13C4 PFOS
PERCENT RECOVERY 69 59
NOTK(S) :_________________________________________________________
Calculations are performed before rounding to avoid round-off errors in calculated results.
Bold print denotes control parameters
RECOVERY LIMITS (50 - 200) (50 - 200)
DEP2-SDWB-000253
DEP2-SDWB-000254
QC Laboratories'
CHAIN OF CUSTODY
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MATRIX CO DES
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SAMPLED BY: (NamelCompany)
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RELINQUISHED BY SAMPLER
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RECEIVED BY
DATE
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