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ty Proven Results.
Analytical Report
Fluorochemical Characterization of Aqueous Samples Decatur Outfall 001 FC Monitoring (E03-0562)
Exygen Research Laboratory Report No. L34911
Testing Laboratory Exygen Research
3058 Research Drive State College, PA 16801
Project Lead Jess Eldrldge 3M Environmental Technology and Safety Services 935 Bush Avenue Building 0002-03-E-09 PO Box 33331 St. Paul, MN 55133-3331
.3058 Research Drive .State College, PA 16801, USA
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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 L34911.
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: T arget Analysis
Compound Name Perfluorobutanesulfonate Perfluorohexanesulfonate Perfluorooctanesulfonate Perfluorobutvric Acid Perfluorooentanoic Acid Perfluorohexanoic Acid Perfluoroheotanoic Acid Perfluorooctanoic Acid Perfluorononanoic Acid Perfluorodecanoic Acid Perfluoroundecanoic Acid Perfluorododecanoic Acid Perfluorobutanesulfonamide Perfluorooctanesulfonamide 2-fN-methvloerluorobutanesulfonamido)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. All samples were cooled to 4C from time of collection to receipt at the laboratory. Samples were stored at 4C from receipt until analysis. Eight individual containers were received. Field samples were collected on 7/22/03 and 7/23/03. Samples were received on 7/25/03. Chain-of-custody information is presented in Attachment C.
PAGE2 OF5
3 Holding Times
Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of collection.
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 portion of sample was diluted to forty-milliliters with Type I water. The 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 C18 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.
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 8/04/03. Initial analysis showed some quality control failures, therefore re-extractions were performed for the C4 Acid, C12 Acid, C8 Sulfonate, FOSA, and MeFBSE-OH were performed on 8/22/03. Samples were analyzed between 8/12/03 and 8/23/03. Raw analytical data is provided 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) 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.
PAGE3 OF5
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.
All calibration criteria were met for this analysis.
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
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.
5.5 Duplicates
Field and laboratory duplicates were prepared for each field sample. 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 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.
5.7 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 except the C4 Acid, C11 Acid, C12 Acid, and MeFBSE-OH. The accuracy for the C11 Acid, C12 Acid, and MeFBSE-OH are given as + 39%, 65%, and + 45% respectively. No data is being reported for the C4 Acid because of multiple QC failures. The statement of accuracy is based on recoveries of field and laboratory spikes. Low recoveries were observed in the field blank spikes for the C5 Acid and the C4 Sulfonate. However, field and laboratory spikes of the sample showed acceptable recoveries, therefore, the field blank spike results are considered an anomaly and were not used in determining the accuracy for these compounds.
PAGE4 OF5
6 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. The limit of quantitation for this compound is 4.0 ng/mL.
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 Exygen.
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: Raw Analytical Data
9 Signatures
Other Lab Members Contributing to Data Emily Decker Karen Smith
^0
PAGE50F5
SECTION A
Analytical ^
kReport
Summary of Fluorochemical Residues in Outfall 001 Effluent
Sample ID
Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup
Field Control/Travel Blank Equipment Blank
C5 Acid
Perfluoropentanoic Acid
1.13 1.09 1.05 ND ND
Analyte Found (ng/mL)
C6 Acid
C7 Acid
Perfluorohexanoic Acid Perfluoroheptanoic Acid
4.94
2.22
4.84
2.21
4.87
2.20
ND ND
ND ND
Sample ID
Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup
Field Control/Travel Blank Equipment Blank
C8 Acid
Perfluorooctanoic Acid
10.3 10.1 9.99 ND ND
Analyte Found (ng/mL)
C9 Acid
C10 Acid
Perfluorononanoic Acid Perfluorodecanoic Acid
ND ND
ND ND
ND ND ND ND
ND ND
C11 Acid
Perfluoroundecanoic Acid
ND ND ND ND ND
Sample ID
C12 Acid
Perfluorododecanoic Acid
Outfall 001 Effluent-Composite
ND
Outfall 001 Effluent-Composite*
ND
Outfall 001 Effluent-Composite Dup
ND
Field Control/Travel Blank
ND
Equipment Blank
ND
Analyte Found (ng/mL)
C4 Sulfonate
C6 Sulfonate
Perfluorobutanesulfonate Perfluorohexariesulfonate
9.52
2.43
9.91
2.4*
9.32
2.35
ND ND
ND ND
C8 Sulfonate
Perfluorooctanesulfonate
31.4 31.0 30.7 ND ND
Analyte Found (ng/mL)
Sample ID
Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup
Field Control/Travel Blank Equipment Blank
PFBAm ide
21.9 22.2 22.2 ND ND
FOSA
4.11 4.11 4.15 ND ND
M e-F B S E -O H **
ND ND ND ND ND
ND = Not detected = Response between 0 and 1 ng/mL. **ND = Not detected = Response between 0 and 4 ng/mL.
'Laboratory Duplicate
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SECTION B
Proven Results.
Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent
Sample Description Outfall 0 0 1
Low Field Spike
Amount Spiked (ng/mL)
C5 Acid
C6 Acid
C7 Acid
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) (ng/mL)
(%)
10
1.13
8.90
78
4.94
12.3
74
2.22
9.97
78
Outfall 001
H igh Field Spike
500
1.13
357
71
4.94
493
98
2.22
522 104
Outfall 0 0 1 Spk C
Low Lab Spike
10
1.13
12.0.
109
4.94
15.4 105
2.22
12.8
106
Outfall 001 Spk D
H igh Lab Spike
500
1.13
393
78
4.94
534 106 2.22
553 110
Field Blank
Low Field Spike
10
ND
1.42
14
ND
8.96
90
ND
10.0
100
Field Blank
High Field S pike
500
ND
33.7
7
ND 408 82 ND 558 112
Sample Description Outfall 001
Low Field Spike
Amount Spiked fnq/mL)
Amt Found in Sample
(ng/mL)
C8 Acid
Amount
Amt Found
Recovered Recovery in Sample
(ng/mL)
(%)
(ng/mL)
C9 Acid
C10 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 10.3 17.9 76
ND
8.10
81
ND 7.71 77
ND
6.12
61
Outfall 0 0 1
High Field Spike
500
10.3
514 101
ND , 493
99
ND
486 97
ND
443 89
Outfall 0 0 1 Spk C
Low Lab Spike
10
10.3
20.6
103
ND
10.8 108
ND
10.5
105
ND
10.5 105
O u tfa ll 0 0 1 S p k D
High Lab Spike
500
10.3
551 108
ND
568 114
ND
556 111
ND
554 111
Field Blank
Low Field Spike
10
ND
9.52
95
ND
9.96
too
ND
8.82
88
ND
7.66
77
Field Blank
High Field Spike
500
ND
553 111
ND
536 107
ND
532 106
ND
500 100
ND = Not detected = Response between 0 and 1 ng/ml.
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Proven Results.
Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent Continued
Sample Description Outfall 0 0 1
Low Field Spike
Amount Spiked (ng/mL)
C12 Acid
04 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/mL)
(%)
(ng/mL) (ng/mL)
{%)
(ng/mL) (ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
10
ND
3.51 35
9.52
17.7 82
2.43
10.4
80
31.4
26.8
-46
Outfall 0 0 1
High Field Spike
Outfall 001 Spk C
Low Lab Spike
Outfall 001 Spk D
High Lab Spike
Field Blank
Low Field Spike
Field Blank
High Field Spike
500 10 500 10 500
ND ND ND ND ND
434
11.6
87 116
9.52 9.52
598 120 9.52
11.8
118
ND
381
76 ,
ND
467 20.6 483 4.60 176
91 111 97 46 35
2.43 2.43 2.43 ND ND
555 12.9 547 9.97 557
111 105 109 100 111
31.4 31.4 31.4 ND ND
654 47.2 618 12.0 623
125 158 124 120 125
Sample Description Outfall 0 0 1
Low Field Spike
Amount Spiked (nq/mL)
PFBAmide
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
(nq/mL) (ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
10
21.9
29.4
75
4.11
8.55
44
ND
5.67
57
Outfall 0 0 1
High Field Spike
500
21.9
488 93
4.11
501 99
ND
727 145
Outfall 0 0 1 Spk C
Low Lab Spike
10
21.9
33.0
111
4.11
17.0
129
ND
9.17
92
Outfall 0 0 1 Spk D
H igh Lab Spike
500
21.9
531 102 4.11
650 129
ND
669 134
Field Blank
Low Field Spike
10
ND
9.05
91
ND 11.1 111 ND
11.2
112
Field Blank
High Field Spike
500
ND
501 100
ND
495 99
ND
568 114
ND = Not detected = Response between 0 and 1 ng/mL, *ND = Not detected = Response between 0 and 4 ng/mL.
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SHIPMENT METHOD
SAMPLE CONDITION
Temp in C
') L>
Received on Ice y /N
Sealed Cooler /N
Samples Intact Y/N
Additional Comp" ''Is
f
AIRBILL NO. SAMPLE NOTES
~
SHIPPING DATE
NO. OF COOLERS ITEM
NUMBER
RELINQUISHED BY / AFFILIATION
DATE
\,C j..,0 fc -r (
/flis r ' V o
TIME ACCEPTED BY / AFFILIATION
7/ 0 ---------------------
/
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DATE TIME
7j / * 0
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L- Ch t r i *VL T
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SAMPLER NAME AND SIGNATURE
( O*' p O i ,~ti O. I l r*,U
DATE Signed: --'MM / DD / YY)
_____ 4' % / a
DP \d
Instructions for completing Chain of Custody (COC)
1. Complete all Client information at fop of sheet: name, address, phone, contact (person to whom report wiii be sent and contact can be made if questions arise), billing information if different from client, PO/f. Project Name and/or Project Number as h will appear on the report.
to CbK'te Fhawifancm Pmjeci hfanageu Pnveot No. and Profile No. will be completed by Pace.
0. A sepai me COC must be feed out for each day of sample collection.
4 Sampler should print their name in the space provided ana sign their name followed by the date of
the sampling event.
.
- ' '
5. Complete Sample Description as It will appear on the laboratory report; include time of sampling,
sample matrix, no, of containers and preservative used.
'
6. Analysis Requested: Complete analysis on the lines provided and place a check in the column for the samples requiring the analysis. If may be necessary to use the space provided for additional comments or include attachments for extended lists of parameters.
7. Submission of samples to laboratory: Indicate Item Number of those samples being transferred; sign relinquished by, and include your affiliation,
* IMPORTANT NOTE:
Standard Turnaround Time isJ2 weeks. If this does not satisfy your requirements, arrangements must be made prior to samples being submitted to the laboratory. Contact your project manager.
Special Project Requirements such as Low Level Detection Limits or level of QC reported must
be indicated on the chain of custody, (Use Additional Comments Section.)
.-
lI
CHAIN-OF-CUSTODY / Analytical Request Document
raceAnalytical
www.pacelabs.com
Required Client Information: Company .
3 fY\ V \
Section A t ss
The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately.
Required Client inform ation:
ReporLTo:
_?
w iF ss v l d t ^ k
Copy To:
Section B
Page: / V
639393
To Be Com pleted by Pace Analytical and Client Quote Reference:
Section C
Invoice To:
Client Inform ation (Check quote/contract): Requested Due Date:
Project Manager:
._Project^ Name: ()<J^ / a UU -90 f f c
Project Number:
Y0y\ ; `fX*/ '
Turn around tim es less than 14 days subject to laboratory and contractual obligations and may result in z Rush Turnaround Surcharge.
^ Turn Around Time (TAT) in calendar days.
IA
Project #:.
' O Z -
Profile #:
0 ^ 2,
Requested Analysis:
Section D
Required Client Information:
Valid Matrix Codes -
Preservatives
SAMPLE ID Onecharacter per box. (A-Z, 0-9 /.-)
Sample IDs MUSTBEUNIQUE
TSOWAOIIOITSRILPHISLEEURE
Wi
SOLL
awrp
3*1
TS /-`''S OT; tt-
wSbLU ==1
oo hh:mma/p
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km km
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MAT IRXCODE
3
- DATE ^ COLLECT -< #Containers Unpreserved NaOH Methan lo tOher
/ "^ / / / / / / / / R em arks / Lab ID t / -, - -, / r"- "........... " /.L :L y
\" (
Lj
I_ j I____
____
JI 1____
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19 " i
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SAMPLE CONDITION Temp in C
Received on Ice Y/N
Sealed Cooler Y/N
Samples Intact Y/N
TAdditional Com''
SAMPLE NOTES f i ( (' S rX I
L l / Cb jof> "
Vf f f c k t o n --
0 -/A
1
Com posite O. / /
_j 1 !n
\ f L~ i H, n-~
M ,ptKi 'L , /Qi
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SAMPLER NAME AND SIGNATURE
PRINT Name of SAMPLER:
f/
X X U c.
SIGNATURE of SAMPLER):
/ j j __
,
________ A ' /
,:~ X .A X e
^
DATE Signed: i
/ DD / YY) v /c s
Instructions for completing Chain of Custody (COC)
1. Complete ail Client infotnation at top of sheet: name, address, phone, contact (person to whom report will be sent and contact can be made if questions arise), billing information if different from client, PC#. Project Name and/or Project Number as it will appear on the report.
2. Quote Reference, iCojeci Manager, Project No. and Profile No. will be completed by Pace,
-3. A separate COC must be filled out for each day of sample collection.
4. Sampler should prim their name in the space provided and sign their name followed by the date of
the sampling event,
.
-
;
5. Complete Sample Description as it will appear on the laboratory report; include time of sampling,
sample matrix, no, of containers and preservative used,
'
6. Analysis Requested: Complete analysis on the lines provided and place a check in the column for the samples requiring the analysis. It may be necessary to use the space provided for additional comments or include attachments for extended lists of parameters.
7. Submission of samples to laboratory: Indicate Item Number of those samples being transferred; sign relinquished by, and include your affiliation,
* IMPORTANT NOTE:
Standard Turnaround Time is.2_weeks. If this does not satisfy your requirements, arrangements must be made prior to samples being submitted to the laboratory. Contact your project manager.
Special Project Requirements such as Low Level Detection Limits or level of QC reported must
be indicated on the chain of custody. (Use Additional Comments Section.) , .
-
CHAIN-OF-CUSTODY/Analytical Request Document
PaceAnalytical "
www.pacelabs.com
Required Client Inform ation:
Company
Address
XV
Section A
Required Client Information
Report To:
wr
Copy To:
- '/ t o
Invoice To:
The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately.
Section B
__ ______
639393
Page: / of /
Section CTo Be C om pleted by Pace Analytical and C lient
Quote Reference:
Client Inform ation (Check quote/contract):
Requested Due Date:
'TAT:
Project Manager:
P.O .
.m o n e
i' - ') T O ->^ ' Section D
Project Name:
V t, - ii- V T /' / 1- ; u
Project Number:
i f c
o n ? ? I <-/ D N ' j
m e,
Required Client Information:
Valid Matrix Codes -------
* Turn around times less than 14 days subject to laboratory and contractual obligations and may result in a Rush Turnaround Surcharge.
* Turn Around Time (TAT) in calendar days.
. _____
FProject 4 C ' 3 "*
Profile #:
Requested Analysis:
& 2-
Preservatives
M ATR IX C O D E
# Containers Unpreserved 1 HCI Methanol
O ther
S iA M P L E
1D
0 ne character per box. (A-Z, 0-9 / - )
Sampl e IDs MUST BE UNIQUE
W ATtM SOIL OIL W IP E AIR TISSUE OTHER
vv 1 SL OL WP
AR 3 " TS OT M
b Od
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w5 S LU
i= = i o o
mm / dd / yy hh:mm a/p
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SHIPMENT METHOD
i
AIRBILL NO.
SAMPLE CONDITION Temp in C
Received on Ice Y/N Sealed Cooler Y/N Samples Intact Y/N Additional C om r'
SAMPLE NOTES
'v F ou
1
TO
i
Jj1___ 1
j 1 !
i
SHIPPING DATE
NO. OF COOLERS ITEM
NUMBER
RELINQUISHED BY / AFFILIATION
DATE
7 '//.i / if .
TIME / n {'!.
J^
A` I//Oi L - ( 4 /ts ft r'-M T
1 ACCEPTED BY / AFFILIATION
...............
_
DATE TIME
c k t o st r ^ --
CO^ p o <>~t ( I f I f ' .
o. // jU
'A
SAMPLER NAME AND SIGNATURE
PRINT Name of SAMPL.ER: ^- ' 0
A A U r,
SIGNATURE of SAMPLEif r m
,
/
f T^ ' n
;
DATE Signed1 T O ^ M / D D / Y Y )
; IT O ;
L- I
Instructions for completing Chain of Custody (COC)
1. Complete all Client Information at top of sheet: name, address, phone, contact (person to whom report will be sent and contact can be made if questions arise), billing information if different from client, PO#, Project Name and/or Project Number as it will appear on the report.
2. Quote Reference, Project Manager, Project No. and Profile No. will be completed by Pace.
3. A separate COC must be filled out for each day of sample collection.
4. Sampler should print their name in the space provided and sign their name followed by the date of the sampling event.
5. Complete Sample Description as it will appear on the laboratory report; include time of sampling, sample matrix, no. of containers and preservative used.
6. Analysis Requested: Complete analysis on the lines provided and place a check in the column for the samples requiring the analysis. It may be necessary to use the space provided for additional comments or include attachments for extended lists of parameters.
7/ Submission of samples to laboratory: Indicate Item Number of those samples being transferred; sign relinquished by, and include your affiliation.
* IMPORTANT NOTE:
Standard Turnaround Time is 2 weeks. If this does not satisfy your requirements, arrangements must be made prior to samples being submitted to the laboratory. Contact your project manager.
Special Project Requirements such as Low Level Detection Limits or level of QC reported must be indicated on the chain of custody. (Use Additional Comments Section.)
it
6/26/2003
Project: E03-0562
3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report
Requester: Schnobrich, Dana M (223-1N-08) Department: 530711 Project Number: 0022674449 Date Received: 6/26/2003 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
1 of 2
Project Results/Activitv Pace Field Sampling Event
3M Sample Number
Sampled Date
E03-0562-49802
7/2</2fo3
1A>
LAB Analytical Method
EXYGEN
LCMS
E03-0562-49803
7/>f/^()()3
LAB
EXYGEN
Analytical Method
LCMS
E03-0562-49804
7/2/2003
LAB Analytical Method
Sample Description
Outfall 001 Effluent - Composite
Comnonents PFOS PFHS PFBS
Result
FOSA PFBAmide MeFBSE-OH
C4 acid C5 acid C6 acid
C7 acid PFOA
C9 acid
CIO acid Cl 1acid C12 acid
OutfaU 001 Effluent - Composite Duplicate
Comnonents
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
Field Control/Travel Blank
Result
Components
Result
RL Qualifier RL Qualifier RL Qualifier
6/26/2003
3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report
Project: E03-0562 (cont.) 3M Sample Number_______ Sampted Date_______Sample Description_______
E03-0562-49804 (cont.) 7Z24?lo03
LAB Analytical Me7th*od
EXYGEN
LCMS
Field Control/Travel Blank
Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C l acid PFOA C9 acid CIO acid C ll acid C12 acid
E03-0562-49805
7H72003
Equipment Blank
Result
LAB EXYGEN
Analytical Method LCMS
Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA
C9 acid
Result
2 of 2
EL Q ualifier
RL Q ualifier
3058 Research Drive State College, PA 16801
Phone: 800-281-3219 Fax: 814-272-1019
Laboratory Sample Log-in Sheet (Environmental)
Complete upon sample receipt:
Client and/or Project Name
Method of Delivery
Walk-in Trackina#:
Pick-up
UPS
^ 7y/ >'2
^RI^edEx.
Air Borne
. Other fexDlain)
Chain of Custody
Temperature Preservation
Custody Seals: DfesSnt, & intact / broken (explain) ja<absent
Thermometer ID: Cooler ID: Cooler ID: Cooler ID: Cooler ID:
CoolertemD: Cooler temD: Cooler temp: Cooler temD:
Chairjxif Custody Record:
^present
f
absent
Samples Received:
- Q C
P p n ice
C C ` C
* d i n ice melt with ice pack none
Explanation
Completed by Slanature:
Date (Time):
Complete during1 sample log-in:
.
LIMS Log-In #
6 ftv tf
Physical Condition
Samples intact?
No (explain)
Chain of Custody
Samples received agree with COC record?
^ P ^ e s No (explain)
Analysis Request
Analysis request clear?
JP'^es No (explain)
Preservation
Sample containers appropriate? Chemical preservation appropriate? Samples received within holding time? Sample volume/mass adequate?
Yes No (explain) Yes No (explain) Yes No (explain) Yes No (explain)
f /v '
Explanation Completed by Sianature:
/
^ --------'
Complete followina resolution of anv nonconformances:
Client Contacted
Yes Client: No
Resolution
Date:
/
c~ l(
/
^
Date (Time):
'
'
*
Completed by Sianature: Lab Sx Log-in Sheet -Ex
Date:
11-5-01/0
LOGIN CHAIN OF CUSTODY REPORT (InOl) Jul 25 2003, 01:11 pm
Login Number: L34911 Account: 2046 3M ENVIRONMENTAL LABORATORY
Laboratory Sample Number
Client Sample Number
L34911-1
OUTFALL 001 EFFLUENT-COMPOSITE 2 3 -JUL-03 25- JUL- 03
L34911-2
OUTFALL 001 EFFLUENT-COMPOSITE 2 3 -JUL-03 2 5 -JUL-03
COMPLETE ID READS OUTFALL 001 EFFLUENT-COMPOSITE LOW SPK (10 P P B ) .
L34911-3
.C OUTFALL 001 EFFLUENT-COMPOSITE 2 3 -JUL-03 25-JUL-03
COMPLETE ID READS OUTFALL 001 EFFLUENT-COMPOSITE HIGH SPK (500 P P B ) .
L34911-4
OUTFALL 001 EFFLUENT-COMPOSITE 2 3 -JUL-03 25-JUL-03
COMPLETE ID READS OUTFALL 001 E FFLUENT-COMPOSITE D U P .
L34911-5
FIELD CONTROL/TRAVEL BLANK
25-JUL-03
L34911-6 : - 3 :
FIELD CONTROL/TRAVEL BLANK
25-JUL-03
COMPLETE ID READS FIELD CONTROL/TRAVEL BLANK LOW SPK (10 P P B ) .
L34911-7
FIELD CONTROL/TRAVEL BLANK
25-JUL-03
COMPLETE ID READS FIELD CONTROL/TRAVEL BLANK HIGH SPK (500 P P B ) .
L34911-8
EQUIPMENT BLANK
22-JUL-03 25-JUL-03
Page 1 Signature : Date :
P actegfisup;.' i6*
Sendees Name__
f.
4a E x p re Pach 9
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