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Centre Analytical Laboratories, Inc.
3048 Research Drive State College, PA 16801
www.centrelab.com
^P hone: (814) 231 -8032
Fax: (814) 231 -1253 or (814) 231 -1580
Analytical Report
Fluorochemical Characterization of Drinking Water Samples Pensacola, FI (W2176)
Centre Analytical Laboratory Report No. 023-007D (Revision 1)
Revision Date 3/20/01
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 Kris J. Hansen, 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 drinking water samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M Environmental Laboratory. The samples were collected from Pensacola, FI. The Centre study number assigned to the project is 023-007.
Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 16 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 method used was validated by Centre. The validation protocol and results are on file with Centre. 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. Sixteen individual sample containers were received. Samples were received on 02/15/00. The sample collection dates were not supplied. 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. The stability of the analytes of interest for longer periods has not been determined. 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
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 C i8 SPE cartridge. The cartridge was first eluted with 5 mL of 40% methanol in water solution. The eluate 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.
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). Samples were extracted on 2/22/00 and analyzed by MS/MS on 2/23/00. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in attachment D.
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) The response of the quantitation ion 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.
For the results reported here, calibration criteria were met.
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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 method.
5.4 Matrix Spikes
Matrix spikes were prepared for every sample at a concentration of 100 ng/L using all compounds of interest. Matrix spike recoveries are given in Attachment B.
Field spikes were also prepared on several samples at a concentration of 100 ng/L using all compounds of interest. Field spike recoveries are also given in Attachment B. The field spike results for sample MC-329H gave recoveries for all compounds of approximately 1000 %, indicating that this sample was possibly spiked at 1000 ppt instead of 100 ppt.
5.5 Duplicates
All samples were analyzed in duplicate. Results are given along with the sample results in Attachment A.
5.6 Laboratory Control Samples
Milliq water was spiked with all compound of interest at 25 and 250 ng/L. Initial analysis of the 25 ng/L LCS showed low recovery for PFOS. The standard was reinjected and was found to have acceptable recovery (70-130%). All other recoveries for all compounds were between 70 130% in each LCS.
5.7 Sample Related Comments
Field blank samples consisted of empty containers. Forty milliliters of type I water filtered through a hypercarb cartridge was added to the empty container and analyzed in the same manner as the other samples.
6 Data Summary
Please see Attachment A for a detailed listing of the analytical results.
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 (Field and Laboratory Spikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data
9 Signatures
Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith
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Centre Analytical Laboratories, Inc.
3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253
Analytical Results W2171 Pensacola, FI
3M Sample Identification
MC-315H MC-317H MC-320H MC-321H MC-323H MC-326H MC-328H MC-331H NA MC-332H NA MC-333H
Sample Description
Intake-P/N Intake-P/N duplicate Intake-Field Blank Empty Outflow-P/N Outflow-P/N duplicate Site 1 P/N Site 1 P/N duplicate Site 2 P/N Site 2 P/N duplicate Site 3 P/N Site 3 P/N duplicate Field Blank-P/N Empty
PFOS (ng/L)
ND ND ND ND ND ND ND ND ND
46.6 42.3 ND
PF( (ng/L)
ND ND ND ND ND ND ND ND ND ND ND ND
POAA (ng/L)
ND ND ND ND ND ND ND ND ND ND ND ND
Limit of Detection (LOD) for the procedure is appoximately 2.5 ng/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.
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-319H 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
101 112 95.6
Matrix Spike Result
(% Recovery)
101.0 112.0 95.6
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-325H 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
103 124 102
Matrix Spike Result
(% Recovery)
103.0 124.0 102.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-330H 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
115 136 109
Matrix Spike Result
(% Recovery)
115.0 136.0 109.0
Criteria (Pass / Fail)
PASS FAIL PASS
bkT UIETR
Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-331H 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
104 135 105
Matrix Spike Result
(% Recovery)
104.0 135.0 105.0
Criteria (Pass / Fail)
PASS FAIL PASS
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Attachment B: LC/MS/MS Laboratory Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-332H 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 46.6
0 0
70
130
Matrix Spike Result (ng/L)
172 122 112
Matrix Spike Result
(% Recovery)
125.4 122.0 112.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-318H 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
101 102 108
Matrix Spike Result
(% Recovery)
101.0 102.0 108.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-324H 100
PFOS PFOSA POAA
Lower Recovery Limit:
Upper Recovery Limit:
Sample Concentration
(ng/L) 0 0 0
70
130
Matrix Spike Result (ng/L)
104 103 107
Matrix Spike Result
(% Recovery)
104.0 103.0 107.0
Criteria (Pass / Fail)
PASS PASS PASS
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Attachment B: LC/MS/MS Field Spike Recovery
Sample ID: Spiked Amount (ng/L):
MC-329H 100
PFOS PFOSA POAA
Sample Concentration
(ng/L)
0 0 0
Matrix Spike Result (ng/L)
1124 1269 1046
Matrix Spike Result
(% Recovery)
1124.0 1269.0 1046.0
Lower Recovery Limit:
70
Upper Recovery Limit:
130
Note: Results indicate that this sample was spiked at 1000 ng/L instead of 100 ng/L
Criteria (Pass / Fail)
FAIL FAIL FAIL
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3M Envii .mental Laboratory
Form 38778 - PWO
Shipping Address: 3M Bldg. 2-3E-09 935 Bush Avenue St Paul. MN 55106
Telephone: Sample Receiving: (651) 778-4948 Alternate: (651) 778 6753 FAX: (651) 778-6176
Chain of Custody /Reque. j r Laboratory Analytical
17125
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3NI Envil -mental Laboratory
Form 38776 - PWO
Shipping Address: 3M Bldg 2-3E-09 935 Bush Avenue St. Paul, MN 5510
Telephone: Sample Receiving: {651) 770-4948 Alternate: (651)778-6753 FAX: (651) 778-6176
contact Name Company ^ y \
Chain of Custody /Reque. j r Laboratory Analytical
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