Document 4QVDj5BqYwdGa83db7a87axe
Precise Research. Proven Results.
Analytical Report
Fluorochemical Characterization of Aqueous Samples Decatur Outfall 001 FC Monitoring (E04-0388)
Exygen Research Laboratory Report No. L0002749
Testing Laboratory Exygen Research
3058 Research Drive State College, PA 16801
Project Lead Jess Eldridge 3M Environmental Technology and Safety Services 935 Bush Avenue Building 0002-03-E-09 PO Box 33331 St. Paul, MN 55133-3331
lo s s Research Drive ite College, PA 16801, USA
I5 T: 800.281.3219 L F: 814.272.1019 exygen research.com
1 Introduction
Results are reported for the analysis of aqueous samples received by Exygen Research (Exygen) from PACE Analytical. The Exygen study number assigned to the project is L0002749.
Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 8 samples (including field duplicates, blanks, and spikes) 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 Perfluorobutanesulfonate (PFBS) Perfluorohexanesulfonate (PFHS) Perfluorooctanesulfonate (PFOS) Perfluorobutvric Acid PerfluoroDentanoic Acid Perfluorohexanoic Acid Perfluoroheptanoic Acid Perfluorooctanoic Acid Perfluorononanoic Acid Perfluorodecanoic Acid Perfluoroundecanoic Acid Perfluorododecanoic Acid Perfluorobutanesulfonamide PFB Amide) Perfluorooctanesulfonamide 2-(N-methvlDerluorobutanesulfonamido)ethvl alcohol
Acronvm C4 Sulfonate C6 Sulfonate C8 Sulfonate C4 Acid C5 Acid C6 Acid C7 Acid C8 Acid C9 Acid C10 Acid C11 Acid C12 Acid FBSA FOSA Me-FBSE-OH
The analytical methods used were originally developed for groundwater samples and were validated by Exygen. The validation protocol and results are on file with Exygen. Only the C8 Sulfonate, FOSA, and C8 Acid were included in the original method validation. It should be noted that the quality control elements included in this analysis demonstrate the applicability of the method to the additional analytes.
2 Sample Receipt
The water samples were submitted in plastic containers. Samples were received at ambient temperature. Samples were stored at 4C from receipt until analysis. Eight individual containers were received. Field samples were collected between 6/15/04 and 6/17/04. Samples were received on 6/18/04. Chain-of-custody information is presented in Attachment C.
PAGE2 OF5
IM
m
3 Holding Times
iMlll Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 60 days of collection.
II
4 Methods - Analytical and Preparatory
ill
4.1 LC/MS/MS
4.1.1 Sample Preparation for LC/MS/MS Analysis
l 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 portion of sample was diluted to forty-milliliters with Type I water. The
iri dilution was performed prior to extraction in order to lessen the effects of matrix enhancement. This matrix enhancement was observed in earlier samples from this location and from screening runs performed on these samples. The diluted samples were transferred to a Ci8 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to analysis.
ti 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 1 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 ni 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 6/22/04. Samples were analyzed between 6/24/04 and 6/30/04. Raw analytical data is provided in Attachment D. i
5 Analysis
HMl
5.1 Calibration
A 7-level calibration curve was analyzed at the beginning and throughout 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 i 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.
i 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.
i
PAGE3 OF5
ni
All calibration criteria were met for this analysis.
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.
Surrogates
Surrogate spikes are not a component of the LC/MS/MS analytical methods.
Matrix Spikes
Field and laboratory spikes were prepared using all compounds of interest. Field spikes were prepared by adding a measured volume of field sample to a container spiked with the target analytes by the laboratory prior to shipping containers for sample collection. Laboratory spikes consisted of aliquots of un-spiked field samples that were fortified at the laboratory at the time of extraction. Field blank spikes consisted of laboratory water fortified at the laboratory and shipped with the sample containers to the field and back to the laboratory for analysis. Laboratory control spikes (see section 5.6) are samples of laboratory water spiked at the time of extraction. Each type of spike provides information needed to assess analyte stability, extraction efficiency, and matrix effects that may impact analytical results. Matrix spike recoveries are given in Attachment B. Please see Section 5.7 for additional discussion of matrix spike recoveries.
Duplicates
Field and laboratory duplicates were prepared for each field sample. Duplicate results are given along with the sample results in Attachment A.
Laboratory Control Samples
For LC/M S/M S analyses, Milliq water was spiked with all compounds of interest at 100 and 500 ng/mL 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 Attachment D.
Statement of Accuracy
Based on results of field spikes, laboratory fortified field samples, field blank spikes, and laboratory control spikes, the analytical accuracy of all analytes is 30% for all compounds with the following exceptions. No data is being reported for the C4 acid because of multiple QC failures. This compound showed acceptable recoveries for blank spikes, but matrix effects were present in the wastewater samples. Results for the C6 acid should be used as screening data only because of erratic recoveries in the several field and laboratory spikes. The statement of accuracy is based on recoveries of field and laboratory spikes.
Data Summary
Please see Attachment A for a detailed listing of the analytical results. Results are reported in parts per billion (ppb) (ng/mL). Please note that the limit of quantitation is 1.0 ng/mL for all compounds except MeFBSE-OH, which has a quantitation limit of 4.0 ng/mL.
PAGE 4 OF5
6 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 Exygen.
7 Attachments
7.1 Attachment A: Results 7.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: Raw Analytical Data
9 Signatures
Other Lab Members Contributing to Data Karen Smith
PAGE 5 OF5
SECTION A
1 \ \
Summary of Fluorochemical Residues in Outfall 001 Effluent
iM
Analyte Found (ng/m L)
C5 Acid
C6 Acid
C7 Acid
idi
S am p le ID Outfall 001 Effluent-Composite
Perfluoropentanoic Acid ND
Perfluorohexanoic Acid 1.16
Perfluoroheptanoic Acid ND
Outfall 001 Effluent-Composite*
ND
1.94
ND
Outfall 001 Effluent-Composite Dup
ND
1.34
ND
Field Control/Travel Blank
ND
ND
ND
Equipment Blank
ND
ND
ND
Analyte Found (ng/m L)
i
C 8A cid
C9 Acid
C10 Acid
C11 Acid
S am ple ID
Perfluorooctanoic Acid
Perfluorononanoic Acid
Perfluorodecanoic Acid Perfluoroundecanoic Acid
Outfall 001 Effluent-Composite
2.49
ND
ND
ND
i Outfall 001 Effluent-Composite*
2.77
ND
ND
ND
Outfall 001 Effluent-Composite Dup
2.57
ND
ND
ND
Field Control/Travel Blank
ND
ND
ND
ND
Equipment Blank
ND ,
ND
ND
ND
ri
Analyte Found (ng/m L)
C12 Acid
C4 Sulfonate
C6 Sulfonate
C8 Sulfonate
il
S am ple ID
Perfluorododecanoic Acid Perfluorobutanesulfonate Perfluorohexanesulfonate Perfluorooctanesulfonate
Outfall 001 Effluent-Composite
ND
13.3
1.07
13.4
Outfall 001 Effluent-Composite*
ND
15.2
1.07
16.0
Outfall 001 Effluent-Composite Dup
ND
13.8
1.07
14.7
0 Field Control/Travel Blank
ND
ND
ND
ND
Equipment Blank
ND
ND
ND
ND
i
S a m p le ID
Outfall 001 Effluent-Composite m Outfall 001 Effluent-Composite*
Outfall 001 Effluent-Composite Dup Field Control/Travel Blank Equipment Blank
m
FBSA
65.9 73.5 65.9 ND ND
Analyte Found (ng/m L)
FSA
2.94 3.08 3.01 ND ND
M e-FB SE-O H **
20.7 17.6 17.7 ND ND
ND = Not detected = Response between 0 and 1 ng/mL. i **ND = Not detected = Response between 0 and 4 ng/mL.
'Laboratory Duplicate
i
li
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0 exygen.com
SECTION B
CH
Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent
Sample Description
Outfall 001 Low Flaid Spike
Amount Spiked (ng/mL)
Amt Found in Sample
(na/mL)
C5 Acid_________________________ C6 Acid_________________________ C7 Acid
Amount
Amt Found Amount
Amt Found Amount
Recovered Recovery in Sample Recovered Recovery in Sample Recovered Recovery
(ng/mL)_____ (%)___ (ng/mL) (ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
10 ND
5.41
54
1.16
6.71
67
ND
5.48
55
Outfall 001 High Field Spike
250
ND
156 62
1.16
4430
1772
ND
233 93
Outfall 001 Spk C
Low Lab Spike
1
ND
1 29 129
1.16
6.68
552
ND
2.48
248
Outfall 001 Spk D High Lab Spike
Field Blank Low Field Spike
Field Blank High Field Spike
500 10 250
ND ND ND
471 8.76 187
94 88 75
1.16 ND ND
650 7.96 225
130 80 90
ND ND ND
675 12.7 269
135 127 108
Sample Description
Outfall 001 Low Field Spike
Amount Spiked (ng/mL)
C8 Acid
Amt Found Amount
Amt Found
in Sample Recovered Recovery in Sample
(ng/mL) (no/mL)
(%)
(ng/mL)
C9 Acid
CIO Acid
C11 Acid
Amount
Amt Found Amount
Amt Found Amount
Recovered Recovery in Sample Recovered Recovery in Sample Recovered Recovery
(ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
10
2.49
9.72
72
ND
3.16
32
ND
3.98
40
ND
3.36
34
Outfall 001
High Field Spike
250
2.49
223
88
ND
194 78
ND
205 82
ND
196 78
Outfall 001 Spk C Low Lab Spike
Outfall 001 S p k D High Lab Spike
1 500
2.49 2.49
5.98 493
349 98
ND ND
1,01 101 522 104
ND ND
1.10 549
110 110
ND
0.949
95
ND 624 125
Field Blank
Low Field Spike
10
ND
11.2
112
ND
9.62
96
ND
9.51
95
ND
9.09
91
Field Blank
High Field Spike
250
ND
239 96
ND
201 80
ND
215 86
ND
209 84
ND = Not detected = Response between 0 and 1 ng/mL. *ND = Not detected = Response between 0 and 4 ng/mL.
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Proven Results.
Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent Continued
Sample Description Outfall 001 Low Fiald Spika
Outfall 001 High Fiald Spika
Amount Spiked (ng/mL)
C12 Acid
C4 Sulfonate
C6 Sulfonate
C8 Sulfonate
Amt Found Amount
Amt Found Amount
Amt Found Amount
Amt Found Amount
In Sample Recovered Recovery In Sample Recovered Recovery in Sample Recovered Recovery In Sample Recovered Recovery
(ng/mL) (ng/m U
(%)
(ng/mL) (ng/mL)
(*/)
(ng/mL) (ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
10
ND
2.02
20
13.3
20.3
70
1.07
7.92
69
13.4
20.9
75
250 ND
133 53 13.3 238 90 1.07 229 91
13.4
264 100
Outfall 001 Spk C Low Lab Spika
1
ND
0.969
97
13.3
14.0
70
1.07
2.52
145
13.4
14.8 **
Outfall 001 Spk D High Lab Spika
500
ND
649 . 130
13.3
522 102 1.07
501 100 13.4
506 99
Field Blank
Low Flaid Spika
10
ND
9.16
92
ND
9.79
98
ND
10.1 101
ND
9.74
97
Field Blank
High Fiald Spika
250
ND
209 84
ND
230 92
ND
236 94
ND
231 92
Sample Description
Outfall 001 Low Fiald Spika
Amount Spiked (ng/mL)
FBSA
FOSA
Me-FBSE-OH*
Amt Found Amount
Amt Found Amount
Amt Found Amount
in Sample Recovered Recovery in Sample Recovered Recovery in Sample Recovered Recovery
(ng/mL) (ng/mL)
(%)
(ng/mL)
_____(%)..... (ng/mL) (ng/mL)
(/.)
10
65.9
72.8
**
2.94
8.83
59
20.7
26.1
54
Outfall 001 High Fiald Spika
250
65.9
298 93
2.94
206 81
20.7
312 125
Outfall 001 Spk C Low Lab Spika
Outfall 001 S p k D High Lab Spika
1 500
65.9 65.9
66.9 ** 2.94
582 103 2.94
4:20
126
20.7
542 108 20.7
18.9
659 128
Field Blank
Low Fiald Spika
10
ND
10.2
102
ND
8.78
88
ND
7.87
79
Field Blank
87High Fiaid Spika
250
ND
230 92
ND
217
ND 253 101
NO = Not detected - Response between 0 and 1 ng/mL. *ND = Not detected = Response between 0 and 4 ng/mL. "Sam ple residue exceeded the spiking level by more than 4 times; therefore an accurate recovery cannot be calculated.
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SECTION C
#
A n a ly tic a l
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CHAIN-OF-CUSTODY / Analytical Request Document
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Required C lie n t Inform ation:
Valid Matrix Codes
Preservatives
SB
DATE COLLECT
SAMPLE ID
One character per box. (A-Z, 0 - 9 / . - )
Sample IDs MUST BE UNIQUE
WATER SOIL OIL WIPE AIR TISSUE OTHER
W1
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MATRIX CODE
3 S; 5
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NC SC G A O ther_______
NPDES GROUND WATER
UST
RCRA
SAMPLE CONDITION
SAMPLE NOTES
Temp in C
c'\. U l o / t A t r
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Required C lien t Inform ation:
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One character per box. (A-Z, 0-9 / .- )
Sample IDs MUST BE UNIQUE
Valid Matrix Codes -
MATRIX
CODE
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5/ 25/2004 Project: E04-0388
3M ENVIRONMENTAL LABORATORY Prelim inary/Unauthorized Report
Page 1 o f2
Requester: Schnobrich, Dana M (223-1N-08) Department: 530711 Project Number: 0022674449 Date Received: 5/25/2004 Project Description: Decatur Outfall 001 FC Monitoring Quarterly Comments:
Completion Date:
Project Lead: Jess S. Eldridge Phone Number: 651-778-5233 Email Address: jseldridge@mmm.com
Project Results/Activitv Pace Field Sampling Event
3M Sample Number
Sampled Date
E04-0388-70331
6/8/2004
LAB EXYGEN
Analytical Method LCMS
E04-0388-70332
6/8/2004
LAB EXYGEN
Analytical Method LCMS
E04-0388-70333
6/8/2004
Sample Description______________________________________________
Outfall 001 Effluent - Composite
Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid Cl 1 acid C12 acid
Result
RL Qualifier
Outfall 001 Effluent - Composite Duplicate
Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid Cl 1 acid Cl 2 acid
Result
RL Qualifier
.
Field Control/Travel Blank
5/ 25/2004
3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report
Page 2 of 2
Project: E04-0388 (cont.) 3M Sample Number_____ Sampled Date______Sample Description______________________________________________
E04-0388-70333 (cont.) 6/8/2004
Field Control/Travel Blank
LAB EXYGEN
Analytical Method LCMS
E04-0388-70334
6/8/2004
Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid Cl 1 acid C12 acid
Equipm ent Blank
Result
RL Qualifier
'
LAB EXYGEN
Analytical Method LCMS
Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid Cl 1 acid C12 acid
Result
RL Qualifier
USAirbill
Express
From
Date ( a } ) ? } O V
64701.7043323
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State
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DeptTFloor/Suite/Room
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0200
4a Express Package Service
{N /F e d E x P rio rity Overnight Nextbiisiness morning'
P 1 FedEx Standard Overnight I-- - Next business afternoon*
Packages up to 150lbs. 'To mostlocations
I | FedEx First Overnight -- I EEaarlrileiesst tnneexxttbbuussinineessssmmoomrnminag
deliveryto seiect locations*
f ~ j FedEx 2Day
I-- J Second business day*
1 FedEx Express Saver --I Third business day*
FedEx Envelope rate notavailable- Minimum charge: One-pound rate
4b Express Freight Service
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I I FedEx 2Day Freight
Call for Confirmation: .
-- 1 Second business day**
Packages over 150lbs. "TmffjiKnMP Htkitweaato
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5 Packaging
FedEx E nv e lo p e *
f j FedEx Pak*
j FedEx
Includes FedEx Small Pak,
" Box
FedExLarge Pak, and FedEx Sturdy Pak
* Declared value limit $500
FedEx Tube
6 Special Handling
SATURDAY D efo/ay Available ONLYfor FedEx Priority Overnight FedEx 2Day, FedEx IDsy Freight and FedEx 2Day Freightto select ZIP codes
tochide FedExaddress in Secte* 3.
'1
r--] HOLD W eekday
i-- i HOLD S aturday
I - 1 a t FedEx Location
1__ 1 a t FedEx Location
Notavailablefor
Available ONLYfor FedEx Priority
FedEx First Overnight
Overnight and FedEx 2Day
to select locations
Does th is shipment contain dangerous goods?
n Oneboxmustbe checked. j Yes
I----- 1 As per attached
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Shipper's Declaration
not required
tiding Dry feei cannot be shipped in FfJEx packaging.
J 0%Ory Ice. 9, UN 1845 _________ x ______
Cargo A ircraft Only
Payment BUjta.
Enter FedEx Acct No. or Credit Card No. b elo w .------------ 1
j Recipient
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Total P ackages
T otal W eig h t
T otal D eclared Value?
S .00
?Our liability is limited to $100 unless you declare a higher value. See back fo r details.
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Total Charges
