Document xdbRyjaMG2n6Bm71J0wkZN99m
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Centre Analytical Laboratories, Inc.
3048 Research Drive State College, PA 16801
www.centrelab.com
iP h o n e : (814) 231-8032
Fax: (814) 231-1253 or (814) 231-1580
Analytical Report
Fluorochemical Characterization of Drinking Water, Surface Water, Sediment,
POTW Effluent, POTW Sludge and Landfill Leachate Samples Port St. Lucie Resampling (E00-2003)
Centre Analytical Laboratory Report No. 023-014P (Revision 1)
\
Revision Date 3/27/01
Testing Laboratory Centre Analytical Laboratory, Inc.
3048 Research Drive State College, PA 16801
3M Environmental Laboratory Contact Kent R. Lindstrom Bldg. 2-3E-09 P.O. Box 33331
St. Paul, MN 55133-3331 Phone: (651)778-5352
Requester Dale Bacon Ph.D. 3M Environmental Technology & Safety Services
Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331
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1 Introduction
Results are reported for the analysis of a series of water, leachate, sludge, and sediment samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M Environmental Laboratory. The samples were collected from Port St. Lucie, Florida and are part of 3M Project EOO-2003. The Centre study number assigned to the project is 023-014.
Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) and ion chromatography was requested for all samples. A total of 45 samples were received for analysis.
The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals:
Table 1: Target Analysis
Compound Name Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate
Acronvm PFOS PFOSA POAA
The analytical methods used for water samples were validated by Centre. The validation protocol and results are on file with Centre. The methods were modified for the sediment samples, however the procedures have not been fully validated for this matrix. Data presented here is the highest quality data available at this time.
2 Sample Receipt
The samples were submitted in individual plastic containers and were not preserved. Forty-five individual sample containers were received. Samples were received on 7/25/00. The samples were collected between 7/18/00 and 7/19/00. Chain-of-custody information is presented in Attachment C.
3 Holding Times
The analytical method used was validated against a maximum holding time of 14 days. Stability after this time period has not been validated. However, it should be noted that field fortifications in water and other matrices have shown acceptable recoveries at 100 and 1000 ng/L for periods longer than 14 days.
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4 Methods - Analytical and Preparatory
4.1 LC/MS/MS
4.1.1 Sample Preparation for LC/MS/MS Analysis
Water samples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliter portion of sample was transferred to a C18 SPE cartridge. The cartridge was first eluted with 5 mL of 40% methanol in water solution. The luate was discarded and the SPE column was then eluted with 100% methanol. A 5 mL portion of methanol was collected for analysis by LC/MS/MS. This treatment resulted in an eight-fold concentration of the samples prior to analysis.
For the sediment and sludge samples, a representative portion of sample (5 grams) was first extracted into 5 ml of methanol. The extracts were filtered and diluted to a final volume of 40 mL with Type I water. The diluted extracts were then treated in the same manner as the water samples, beginning with the solid phase extraction.
4.1.2 Sample Analysis by LC/MS/MS
In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards.
A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Water samples were extracted between 8/15/00 and 8/17/00 and analyzed by MS/MS between 8/18/00 and 8/23/00. Sediment and sludge samples were extracted on 8/18/00 and were analyzed by MS/MS on 8/21/00. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in Attachments D and E.
5 Analysis
5.1 Calibration
A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined, A calibration curve is acceptable if r >.0.985 (r2 > 0.970).
Calibration standards are prepared using the same SPE procedure used for samples.
Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value.
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For the results reported here, calibration criteria were met.
5.2 Blanks
Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant.
Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant.
5.3 Surrogates
Surrogate spikes are not a component of the LC/MS/MS analytical methods.
5.4 Matrix Spikes
Matrix spikes were prepared for every field sample using all compounds of interest. Matrix spike recoveries are given in Attachment B.
Field spikes were submitted with the water samples. Field spike recoveries are also included in Attachment B. The PSLF Leach-C-FMS sample spiked at 200 ng/L appears to have been spiked in error. Spike results are comparable to the 1000 ng/L spiking level.
5.5 Duplicates
All field samples were analyzed in duplicate. Results are given along with the sample results in Attachment A.
5.6 Laboratory Control Samples
For LC/MS/MS analyses, Milliq water was spiked with all compounds of interest at 25 and 250 ng/L during each extraction set. All recoveries for all compounds were between 70-130% in each LCS. Results are given along with the raw data in Attachments D and E.
5.7 Sam ple RelatedCom m ents There are no other sample related comments for this data set.
6 Data Summary
Please see Attachment A for a detailed listing of the analytical results. Surface water results are reported in parts per trillion (ppt) (ng/L). Sediment and sludge sample results are reported in parts per billion (ppb) (ug/Kg) on both an as-received and dry-weight basis.
7 Data/Sample Retention
Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Centre.
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8 Attachments
8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data (Surface Water Samples) 8.5 Attachment E: LC/MS/MS Raw Analytical Data (Sediment and Sludge Samples)
9 Signatures
Other Lab Members Contributing to Data Karen Smith
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I
jSSSk Centre Analytical Laboratories, Inc.
3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253
3M Sample Identification MDWPIN-R-O-C MDWPIN-Lime-C MDWPOut -C NPWWTPEff -C NPWWTPCC-C PSLF Leach-C TW#2 Fire Dept-C SW#3 SH-C TW#3 Penpark-C SW#1 Penpark-C TW#1 Holiday Inn-C SW#2 MCM-C QSW Palm City-C NPWWTP Sludge-C SED #3 SH-C SED #1 Penpark-C SED #2 MCM-C
Sample Description Municipal Drinking Water Plant Intake - Reverse Osmosis Municipal Drinking Water Plant Intake - LIME Municipal Drinking Water Plant Outflow North Port Wastewater Treatment Plant Effluent North Port Wastewater Treatment Plant Chlorine Contact Chamber Port St. Lucie Landfill Leachate Tap Water Site #2 Fire Department Surface Water Site #3 Stuart Harbor Tap Water Site #3 Pendarvis Park Surface Water Site #1 Pendarvis Park Tap Water Site #1 Holiday Inn Surface Water Site #2 Martin Cty Marina Quiet Surface Water Palm City North Port Wastewater Treatment Plant Sludge Sample Sediment Sample #3 Stuart Harbor Sediment Sample #1 Pendarvis Park Sediment Sample #2 Martin Cty Marina
Please refer to the reverse side for our standard terms and conditions.
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Wf. THANK YOU F u ti THiS r n BE O * SERVICE
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ANALYTICAL REPORT
Centre Analytical Laboratories, Inc.
3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253
Analytical Results E00-2003 Port St. Lucie, FL Resampling (water samples)
3M Sample Identification
PFOS (ng/L)
PFOSA (ng/L)
POAA (ng/L)
MDWPIN-R-O-C MDWPIN-R-O-C dup MDWPIN-Lime-C MDWPIN-Lime-C dup MDWPOut -C MDWPOut-C dup NPWWTPEff -C NPWWTPEff-C dup NPWWTPCC-C NPWWTPCC-C dup PSLF Leach-C PSLF Leach-C dup TW#2 Fire Dept-C TW#2 Fire Dept-C dup SW#3 SH-C SW#3 SH-C dup TW#3 Penpark-C TW#3 Penpark-C dup SW#1 Penpark-C SW#1 Penpark-C dup TW#1 Holiday Inn-C TW#1 Holiday Inn-C dup SW#2 MCM-C SW#2 MCM-C dup QSW Palm City-C QSW Palm City-C dup Blind Dup C1 Blind Dup C1 dup
Blind D up C 2
Blind Dup C2 dup
.
ND ND ND ND ND ND NQ NQ 85.5 78.8 429 425 ND ND NQ NQ ND ND NQ NQ ND ND NQ NQ 2930 2850 ND ND
NQ
NQ
ND ND ND ND ND ND ND ND NQ NQ NQ NQ ND ND ND ND ND ND ND ND ND ND ND ND 30.0 27.5 ND ND
ND
ND
ND ND ND ND ND ND NQ NQ 42.9 40.2 1030 1020 ND ND ND ND ND ND ND ND ND ND ND ND 96.9 97.1 ND ND
ND
ND
Limit of Detection (LOD) for the procedure is appoximately 2.5 n g /l for PFOS and PFOSA and 7.5 ng/L for POAA
Limit of Quantitation (LOQ) for the procedure is 25 ng/L for all compounds
ND - Compound not detected
NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable.
ND < LOD < NQ < LOQ
Please refer to the reverse side for our standard terms and conditions.
BACK TO MAIN ANALYTICAL REPORT
Centre Analytical Laboratories, Inc.
3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253
Analytical Results E00-2003 Port St. Lucie, FL Resampling (solids)
3M Sample Identification
NPWWTP Sludge-C NPWWTP Sludge-C dup SED #3 SH-C SED #3 SH-C dup SED#1 Penpark-C SED#1 Penpark-C dup SED#2 MCM-C SED#2 MCM-C dup
PFOS (ug/Kg) (as received)
1.36 1.30 ND ND ND ND ND ND
PFOSA (ug/Kg) (as received)
ND ND ND ND ND ND ND ND
POAA (ug/Kg) (as received)
ND ND ND ND ND ND ND ND
3M Sample Identification
NPWWTP Sludge-C NPWWTP Sludge-C dup SED #3 SH-C SED #3 SH-C dup SED#1 Penpark-C SED#1 Penpark-C dup SED#2 MCM-C SD#2 MCM-C dup
.
PFOS (ug/Kg) (dry weight)
62.9 60.2 ND ND ND ND ND ND
PFOSA (ug/Kg) (dry weight)
ND ND ND ND ND ND ND ND
POAA (ug/Kg) (dry weight)
ND ND ND ND ND ND ND ND
Limit of Detection (LOD) for the procedure is appoximately 0.08 ug/Kg for all compounds (as received) Limit of Quantitation (LOQ) for the procedure is 0.20 ug/Kg for all compounds (as received) ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ
% Solids
2.16 2.16 76.68 76.68 76.10 76.10 65.74 65.74
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
MDWPIN-RO C 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
90.3 105 117
Matrix Spike Result
(% Recovery)
90.3 105.0 117.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
MDWPIN-Lime C
Spiked Amount (ng/L):
100
IPFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
101 98.8 111
Matrix Spike Result
(% Recovery)
101.0 98.8 111.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
MDWPIN-Out C 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
102 103 103
Matrix Spike Result
(% Recovery)
102.0 103.0 103.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample 10: Spiked Amount (ng/L):
NPWWTP Eff-C 100
PFOS PFOSA POAA
Sample Concentration
(ng/L)
14.7 0
15.1
Matrix Spike Result (ng/L)
112 85.0 127
Matrix Spike Result
(% Recovery)
97.3 85.0 111.9
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
NPWWTPCC-C 100
PFOS PFOSA POAA
Sample Concentration
' (ng/L)
85.5 4.4 42.9
Matrix Spike Result (ng/L)
187 88.5 149
Matrix Spike Result
(% Recovery)
101.5 84.1 106.1
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
PSLF Leach-C
Spiked Amount (ng/L): 1
10
PFOS PFOSA POAA
Sample Concentration
(ng/L)
429 7.0 1030
Matrix Spike Result (ng/L)
554 102 1125
Matrix Spike Result
(% Recovery)
125.0 95.0 95.0
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
TW#2 Fire Dept-C
Spiked Amount (ng/L):
100
PROS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
101 102 110
Matrix Spike Result
(% Recovery)
101.0 102.0 110.0
Criteria (Pass / Fail)
PASS PASS PASS
Bk T MAIN
Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
SW#3 SH-C
Spiked Amount (ng/L): |
100
PFOS PFOSA POAA
Sample Concentration
(ng/L)
7.8 0 0
Matrix Spike Result (ng/L)
103 98.5 117
Matrix Spike Result
(% Recovery)
95.2 98.5 117.0
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
TW#3 Penpark-C
Spiked Amount (ng/L):
100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
96.0 107 110
Matrix Spike Result
(% Recovery)
96.0 107.0 110.0
Criteria (Pass / Fail)
PASS PASS PASS
g pccr r m w A iw
Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
SW#1 Penpark-C
Spiked Amount (ng/L):
100
PFOS PFOSA POAA
Sample Concentration
(ng/L)
5.2 0 0
Matrix Spike Result (ng/L)
114 109 126
Matrix Spike Result
(% Recovery)
108.8 109.0 126.0
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
BKCK U n U IAIN
Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
TW#1 Holiday Inn-C
Spiked Amount (ng/L):
100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
108 119 117
Matrix Spike Result
(% Recovery)
108.0 119.0 117.0
Criteria (Pass / Fail)
PASS PASS PASS
W A L K I U IVIA IN
Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
SW#2 MCM-C 100
PFOS PFOSA POAA
Sample Concentration
(ng/L)
7.7 0 0
Matrix Spike Result (ng/L)
125 119 135
Matrix Spike Result
(% Recovery)
117.3 119.0 135.0
Criteria (Pass / Fail)
PASS PASS FAIL
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
QSW Palm City-C
Spiked Amount (ng/L):
100
PFOS PFOSA POAA
Sample Concentration
(ng/L)
2930 30.0 96.9
Matrix Spike Result (ng/L)
3260 160 249
Matrix Spike Result
(% Recovery)
330.0 130.0 152.1
Lower Recovery Limit:
70
Upper Recovery Limit:
130
PFOS sample concentration exceeds spiking concentration by greater than 10X
Criteria (Pass / Fail)
FAIL PASS FAIL
B M K T O MAIN
Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
Blind Pup 1 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
101 93.5 99.4
Matrix Spike Result
(% Recovery)
101.0 93.5 99.4
Criteria (Pass / Fail)
PASS PASS PASS
ByCK'T MAIN
Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
Blind Pup 2 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 8.0 0 0
70
130
Matrix Spike Result (ng/L)
109 103 112
Matrix Spike Result
(% Recovery)
101.0 103.0 112.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID:
NPWWTP Sludge-C
Spiked Amount (ng/L):
250
PFOS PFOSA POAA
Sample Concentration
(ng/L)
170 16.7 12.3
Matrix Spike Result (ng/L)
377 193 256
Matrix Spike Result
(% Recovery)
82.8 70.5 97.5
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Concentrations indicate amount of material in the sample extract
Note: Sample results less than 25 ng/L are reported as NQ In the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
Sed#3 SH-C 250
PFOS PFOSA POAA
Sample Concentration
(ng/L)
0 0 0
Matrix Spike Result (ng/L)
227 210 237
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Concentrations indicate amount of material in the sample extract
Matrix Spike Result
(% Recovery)
90.8 84.0 . 94.8
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
Sed#1 Penpark-C 250
PFOS PFOSA POAA
Sample Concentration
(ng/L)
3.3 0 0
Matrix Spike Result (ng/L)
215 216 236
Matrix Spike Result
(% Recovery)
84.7 86.4 94.4
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
Concentrations indicate amount of material in the sample extract
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
Sed#2 MCM-C 250
PFOS PFOSA POAA
Sample Concentration
(ng/L)
2.9 0 0
Matrix Spike Result (ng/L)
240 220 246
Matrix Spike Result
(% Recovery)
94.8 88.0 98.4
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
Concentrations indicate amount of material in the sample extract
m xrm m m --
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
MDWPIN-RO-C FMS
Spiked Amount (ng/L): (
200
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
197 177 173
Matrix Spike Result
(% Recovery)
98.5 88.5 86.5
Criteria (Pass / Fail)
PASS PASS PASS
ra n rTOIviAin
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
MDWPIN-RO-C FMS
Spiked Amount (ng/L): |
1000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
954 857 768
Matrix Spike Result
(% Recovery)
95.4 85.7 76.8
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
MDWPIN-Lime-C FMS
Sipiked Amount (ng/L):
200
F3FOS F3FOSA F3OAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
179 173 189
Matrix Spike Result
(% Recovery)
89.5 86.5 94.5
Criteria (Pass / Fail)
PASS PASS PASS
UUk IU MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
MDWPIN-Lime-C FMS
Spiked Amount (ng/L): |
1000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
844 844 793
Matrix Spike Result
(% Recovery)
84.4 84.4 79.3
Criteria (Pass / Fail)
PASS PASS PASS
BACKTMAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
MDWP Out-C FMS
Spiked Amount (ng/L): |
200
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
201 190 172
Matrix Spike Result
(% Recovery)
100.5 95.0 86.0
Criteria (Pass / Fail)
PASS PASS PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
MDWP Out-C FMS 1000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
831 787 708
Matrix Spike Result
(% Recovery)
83.1 78.7 70.8
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
NPWWTP Eff-C FMS
Spiked Amount (ng/L):
200
PFOS PFOSA POAA
Sample Concentration
(ng/L)
14.7 0
15.1
Matrix Spike Result (ng/L)
203 106 223
Matrix Spike Result
(% Recovery)
94.2 53.0 104.0
Criteria (Pass / Fail)
PASS FAIL PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
" " B T T T O IT O W
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
NPWWTP Eff-C FMS
Spiked Amount (ng/L):
1000
PFOS PFOSA POAA
Sample Concentration
(ng/L)
14.7 0
15.1
Matrix Spike Result (ng/L)
816 538 1290
Matrix Spike Result
(% Recovery)
80.1 53.8 127.5
Criteria (Pass / Fail)
PASS FAIL PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
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Attachment B: LC/MS/MS Field Spike Recovery
Sample 10:
NPWWTPCC-C FMS
Spiked Amount (ng/L):
200
PFOS PFOSA POAA
Sample Concentration
(ng/L)
85.5 4.4 42.9
Matrix Spike Result (ng/L)
302 162 252
Matrix Spike Result
(% Recovery)
108.3 78.8 104.6
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
Uilk I U MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
NPWWTPCC-C FMS
1000
PFOS PFOSA POAA
Sample Concentration
(ng/L)
85.5 4.4 42.9
Matrix Spike Result (ng/L)
946 775 972
Matrix Spike Result
(% Recovery)
86.1 77.1 92.9
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
PSLF Leach-C FMS
Spiked Amount (ng/L): |
200
PFOS PFOSA POAA
Sample Concentration
(ng/L)
429 7.0 1030
Matrix Spike Result (ng/L)
1066 897 1790
Matrix Spike Result
(% Recovery)
318.5 445.0 380.0
Criteria (Pass / Fail)
FAIL FAIL FAIL
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
Data indicates that this sample was spiked at 1000 ng/L rather than the 200 ng/L given in the field data
Bk t MIKi
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
PSLF Leach-C FMS
1000
PFOS PFOSA POAA
Sample Concentration
(ng/L)
429 7.0 1030
Matrix Spike Result (ng/L)
1100 829 1870
Matrix Spike Result
(% Recovery)
67.1 82.2 84.0
Criteria (Pass / Fail)
FAIL PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
PSLF Leach-C FMS 25000
PFOS PFOSA POAA
Sample Concentration
(ng/L)
429 7.0 1030
Matrix Spike Result (ng/L)
20900 21800 22800
Matrix Spike Result
(% Recovery)
81.9 87.2 87.1
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
PSLF Leach-C FMS B
Spiked Amount (ng/L):
200
PFOS PFOSA POAA
Sample Concentration
(ng/L)
429 7.0 1030
Matrix Spike Result (ng/L)
630 179 1270
Matrix Spike Result
(% Recovery)
100.5 86.0 120.0
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
WUik IU MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
PSLF Leach-C FMS B
Spiked Amount (ng/L):
1000
PFOS PFOSA POAA
Sample Concentration
(ng/L)
429 7.0 1030
Matrix Spike Result (ng/L)
1170 877 1980
Matrix Spike Result
(% Recovery)
74.1 87.0 95.0
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
b a K T MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
PSLF Leach-C FMS B
Spiked Amount (ng/L):
25000
PFOS PFOSA POAA
Sample Concentration
(ng/L)
429 7.0 1030
Matrix Spike Result (ng/L)
21900 19800 20500
Matrix Spike Result
(% Recovery)
85.9 79.2 77.9
Criteria (Pass / Fail)
PASS PASS PASS
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only.
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
Penpark-C FMS 200
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
200 139 194
Matrix Spike Result
(% Recovery)
100.0 69.5 97.0
Criteria (Pass / Fail)
PASS FAIL PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
Penpark-C FMS
Spiked Amount (ng/L): |
1000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
831 678 794
Matrix Spike Result
(% Recovery)
83.1 67.8 79.4
Criteria (Pass / Fail)
PASS FAIL PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
Holiday Inn-C FMS
} /
Spiked Amount (ng/L):
200
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
212 193 200
Matrix Spike Result
(% Recovery)
106.0 96.5 100.0
Criteria (Pass / Fail)
PASS PASS PASS
BOTJTTTTITOW
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
Holiday Inn-C FMS
Spiked Amount (ng/L): |
1000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
1060 865 866
Matrix Spike Result
(% Recovery)
106.0 86.5 86.6
Criteria (Pass / Fail)
PASS PASS PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
QSW Palm City-C FMS
Spiked Amount (ng/L):
200
PFOS PFOSA POAA
Sample Concentration
(ng/L)
2930 30.0 96.9
Matrix Spike Result (ng/L)
3360 248 325
Matrix Spike Result
(% Recovery)
215.0 109.0 114.1
Lower Recovery Limit:
70
Upper Recovery Limit:
130
PFOS sample concentration exceeds the spiking level by greater than 10X
Criteria (Pass / Fail)
FAIL PASS PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
QSW Palm City-C FMS
Spiked Amount (ng/L):
1000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 2930 30.0 96.9
70
130
Matrix Spike Result (ng/L)
3810 761 899
Matrix Spike Result
(% Recovery)
88.0 73.1 80.2
Criteria (Pass / Fail)
PASS PASS PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sampl ID:
QSW Palm City-C FMS
Spiked Amount (ng/L):
25000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 2930 30.0 96.9
70
130
Matrix Spike Result (ng/L)
23300 20700 20900
Matrix Spike Result
(% Recovery)
81.5 82.7 83.2
Criteria (Pass / Fail)
PASS PASS PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
QSW Palm City-C FMS B
Spiked Amount (ng/L):
200
PFOS PFOSA POAA
Sample Concentration
(ng/L)
2930 30.0 96.9
Matrix Spike Result (ng/L)
3590 240 340
Matrix Spike Result
(% Recovery)
330.0 105.0 121.6
Lower Recovery Limit:
70
Upper Recovery Limit:
130
PFOS sample concentration exceeds the spiking amount by greater than 10X
Criteria (Pass / Fail)
FAIL PASS PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
QSW Palm City-C FMS B
Spiked Amount (ng/L):
1000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 2930 30.0 96.9
70
130
Matrix Spike Result (ng/L)
4000 819 955
Matrix Spike Result
(% Recovery)
107.0 78.9 85.8
Criteria (Pass / Fail)
PASS PASS PASS
BACK TO MAIN
Attachment B: LC/MS/MS Field Spike Recovery
Sample ID:
QSW Palm City-C FMS B
Spiked Amount (ng/L):
25000
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample
. Matrix Spike
Concentration
Result
(ng/L)
(ng/L)
2930 30.0 96.9
24500 26200 20100
70
130
Matrix Spike Result
(% Recovery)
86.3 104.7 80.0
Criteria (Pass / Fail)
PASS PASS PASS
BACK TO MAIN
3,11 TMForm 38778 r- PLWOn m e n ta l L illK ) r a t o r y Chain of Custody /Request for Laborato,y Analytical 1 5 0 7 9
Shipping Addra: 3M Bldg 2-3E-09 935 Bush Avenue Si Paul, MN 55106
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3M Environmental Laboratory
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CALIO ~ Client Sample 10 - Received.
0006740
12124
7-25-00 10:30
0006741
12127
7-25-00 10:30
0006742
12128
7-25-00 10:30
0006743
12130
7-25-00 10:30
0006744
12133
7-25-00 10:30
0006745
12134
7-25-00 10:30
0006746
12136
7-25-00 10:30
0006747
12139
7-25-00 10:30
0006748
12140
7-25-00 10:30
0006749
12142
7-25-00 10:30
0006750
12145
7-25-00 10:30
0006751
12146
7-25-00 10:30
0006752
12148
7-25-00 10:30
0006753
12151
7-25-00 10:30
0006754
12152
7-25-0010:30
0006755
12154
7-25-00 10:30
0006756
12156
7-25-00 10:30
0006757
12163
7-25-00 10:30
Centre Analytical Laboratories
Sam ple Login Report
Matrix WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER Sludge WATER WATER
Study Number:
0 2 3 -0 1 4
Submitted By
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Logged in By/Pate
RICK K 7-25-00
RICK K 7-25-00 RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
-
Initial Loc. COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6
Condition of Samples ; C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A
Page 1 of 3 Comments !..
BACK TO
Verified By/Date: ' i P . / f / 7 ~ 2 j r - o o
Printed 7/25/2000
>
CAL to - Client Sample ID J Received
0006758
12164
7-25-00 10:30
0006759
12165
7-25-00 10:30
0006760
12166
7-25-00 10:30
0006761
12167
7-25-00 10:30
0006762
12168
7-25-00 10:30
12170
7-25-00 10:30
0006764
12172
7-25-00 10:30
0006765
12174
7-25-00 10:30
0006766
12186
7-25-00 10:30
0006767
12188
7-25-00 10:30
0006768
12191
7-25-00 10:30
0006769
12192
7-25-00 10:30
0006770
12194
7-25-00 10:30
0006771
12198
7-25-00 10:30
0006772
12202
7-25-00 10:30
0006773
12203
7-25-00 10:30
0006774
12211
7-25-00 10:30
0006775
12214
7-25-00 10:30
Centre Analytical Laboratories
Sam ple Login Report
Page 2 of 3
Matrix WATER WATER WATER WATER WATER WATER WATER SEDIMENT WATER WATER WATER WATER SEDIMENT WATER WATER WATER WATER SEDIMENT
Study Number: 023-014
Submitted By Enaksha
Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Logged In By/Pate RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
Initial Lc/ ' x CondiMw of Samples ; " 'C o r n w a l l
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
BACK TO MAIN
Verified By/Date: / .
/?
Printed 7/25/2000
i , CAL H> : . 7 Client Sample ID
Received
0006776
12216
7-25-00 10:30
0006777
12224
7-25-00 10:30
0006778
12225
7-25-00 10:30
0006779 0006780 0006781
12226 12230 12231
7-25-00 10:30 7-25-00 10:30 7-25-00 10:30
0006782
12232
7-25-00 10:30
0006783
12238
7-25-00 10:30
0006784
12239
7-25-00 10:30
Centre Analytical Laboratories
Sam ple Login Report
Study Number: 023-014
Matrix:: : >. WATER WATER WATER WATER WATER WATER WATER WATER WATER
Submitted By
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Enaksha Wickremesinhe
Logged in By/Date
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
RICK K 7-25-00
Initial Loc. Condition o Samples
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6 ` C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
COOLER 6
C-WET ICE-A
Page 3of 3
Comments . . . t --
--
BACK TO MAIN
/f,/ /Verified By/Date:
7
Printed 7/25/2000
