Document J3kRa0Q94vLOEzR8Bk22NLyVX
Analytical Report
Fluorochemical Characterization of Aqueous Samples
Decatur Outfall 001 FC Monitoring (E03-0848) Exygen Research Laboratory Report No. L0001265
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
3058 Research Drive State College, PA 16801, USA
PAGE
I : 800.281.3219 F: 814.272.1019
exygen.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 L0001265.
Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/M S/M S) 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/M S/M S for the following list of fluorochemicals:
T able 1: T arget Analysis
Compound Name Perfluorobutanesulfonate Perfluorohexanesulfonate Perfluorooctanesulfonate Perfluorobutvric Acid PerfluoroDentanoic Acid Perfluorohexanoic Acid PerfluoroheDtanoic Acid Perfluorooctanoic Acid Perfluorononanoic Acid Perfluorodecanoic Acid Perfluoroundecanoic Acid Perfluorododecanoic Acid Perfluorobutanesulfonamide Perfluorooctanesulfonamide 2-iN-methvlDerluorobutanesulfonamido)ethvl alcohol
Acronvm C 4 Sulfonate C 6 Sulfonate C 8 Sulfonate C 4A cid C 5 Acid C 6 Acid C 7 Acid C 8A cid C 9A cid C 10 Acid C 11 Acid C12 Acid FBSA FOSA M e-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 C 8 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
}\ v .-
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 11/3/03 and 11/4/03. Samples were received on 11/5/03. Chain-of-custody information is presented in
Attachment C.
PACE2 OFS
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
W ater 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/M S/M S 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 C i8 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/M S 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 H P1100 HPLC system coupled to a Micromass Ultima M S/M S was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM ). Samples were extracted on 11/6/03. Samples were analyzed between 11/12/03 and 11/14/03. 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/M S/M S 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 .9 8 5 (r2 > 0.970).
Calibration standards are prepared using the sam e 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.
PAGE3 OF5
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/M S/M S 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 L C /M S /M S analyses, Milliq w ater w as spiked with all com pounds of interest a t 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 C 5 Acid. The accuracy for the C 5 Acid is given as + 53% . The statement of accuracy is based on recoveries of field and laboratory spikes. Low recoveries were observed in the high laboratory spikes for several compounds. However, field and low laboratory spikes of the samples showed acceptable recoveries.
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
PAGE4 OF5
compounds except M eFBSE-OH and C 4 Acid. The limit of quantitation for these compounds 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
...........
"v" " " ' V '
Other Lab Members Contributing to Data
Emily Decker Karen Smith
Date D a te
PAGE5 OF5
SECTION A
EVgenRESEARCH Precise Research. Proven Results.
Analytical
Report
Summary of Fluorochemlcal Residues in Outfall 001 Effluent
Sam ple ID
Outfall 001 Effluent-Composite. Outfall 001 Effluent-Composite* . Outfall 001 Effluent-Composite Dup
Field Control/Travel Blank Equipment Blank
C4 A cid** Perfluorobutyric Acid
5 .2 4 6.91 5.3 6 ND ND
Analyte Found (ng/m L)
C5 Acid
C6 Acid
Perfluoropentanolc Acid
Perfluorohexanolc Acid
3 .2 5 3 .3 4 3.61 ND ND
1 5 .3 1 4 .6 1 4 .5 ND ND
C7 Acid Perfluoroheptanoic Acid
4 .4 2 4 .3 5 4 .4 9 ND ND
Sam ple ID
Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup
Field Control/Travel Blank Equipment Blank
C8 Acid Perfluorooctanolc Acid
2 6 .9 2 7 ,6 2 7 .3 ND \ ND ,
A nalyte Found (ng/m L)
C9 Acid
C10 Acid
Perfluorononanolc Acid
Parfluorodecanolc Acid
ND ND ND ND
ND ND ND ND ND ND
C11 Acid Perfluoroundecanolc Acid
ND ND ND ND ND
Sam ple ID Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup
Field Control/Travel Blank Equipment Blank
C12 Acid Parfluorododacanolc Acid
ND ' ND ND ND ND
Analyte Found (ng/m L)
C4 Sulfonate
C6 Sulfonate
Perfluorobutanesulfonate Perfluorohexanesulfonate
4 .0 0 3.91
3 .0 0 3 .1 4
4 .0 8
3 .2 3
ND ND
ND ND
C8 Sulfonate Parfluorooctaneaulfonate
5 5 .8 5 4 .4 5 8 .2 ND ND
Sam ple ID Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup
Field Control/Travel Blank Equipment Blank
FBSA 3 4 .0 3 3 .3 3 3 .9 ND ND
\ Analyte Found (ng/m L)
FSA 6 .0 8 5 .9 2 5 .6 9 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 Sum m ary o f Fluorochem ical Residues In O utfall 001 Effluent
Sample Description Outfall 001
Low FM d Splks
Outfall 001
High FMd Splks
C4 Acid*
CSAcId
CSAcId
C7 Acid
Amount Amt Found Amount
Amt Found Amount
Amt Found Amount
Amt Found Amount
Spiked in Sample Recovered Recovery In Sample Recovered Recovery In Sample Recovered Recovery In Sample Recovered Recovery
(ng/mL) (ng/mL) (ng/mL) (%)
(ngAnL) (ngAnL) (%)
(ng/mL) (ng/mL)____ (%)_ (ngAnL) (ngAnL) (%)
1
5.24 ,
8.92
**
3.25
2.18 -107
15.3
15.9
--
4.42 6.15 -
500 5.24 644 128 3.25 239 47 15.3 568 111 4.42 510 101
Outfall 001 SpkC
Low Lab Splks
1
5.24 6:66 **
325
2.09 -116
15.3
16.2
**
4.42 6.42
Outfall 001 SpkD
High Lab 8pika 500 5.24
215 , 42
3.25
93
18 15.3 247 46 4.42 261 51
Field Blank
Low FMd Splks
1
ND
ND \ -
ND
1.09 109
ND
1.24 124
ND
1.20 120
Field Blank
High FM d Splks
500
ND
441 86
ND
608 122
ND
593 119
ND
613 123
Sample Description
Outfall 001
Low FM d Splks
C8 Acid
CSAcId
C10 Acid
C11 Acid
Amount Amt Found Amount
Atnt Found Amount
Amt Found Amount
Amt Found Amount
Spiked In Sample Recovered Recovery fn$ample Recovered Recovery In Sample Recovered Recovery In Sample Recovered Recovery
(ng/mL) (ngAnL) (ngAnL) (%)
(nd/mL) (ngAnL) (%)
(ng/mL) ("<*" ->__ i*L_ (ngAnL) ("flft"-)____ (%)
1 26.9 27.3 **
n d \ 1.21 121 ND 1.14 114 ND 1.07 107
Outfall 001
High Flsld Splks
500
26.9
517
98
ND
473 95
ND
507 101
ND
566 113
Outfall 001 SpkC
Low Lab Splks
1
26.9 26.8
-
ND
1,01 101
ND
0.923
92
ND
0.732
73
Outfall 001 S p k D
High Lab Splks
500
26.9
303 55
ND
300 \
60
ND
313 63
ND
274 55
Field Blank
Low FM d Splks
1
ND
1.16 116
ND
1.11 111
ND
1.08 108
ND
1.12 112
Field Blank
High FM d Splks
500
ND
556 111
ND
560 112
ND
563 113
ND
502 100
ND = 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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CH
Recovery Sum m ary o f Fluorochem ical Residues in O utfall 001 Effluent Continued
Sample Description Outfall 001
Low FM d S p lln
Outfall 001
High FMd SpUn
C12 Acid___________________C4 Sulfonate_________________ C6 SuHonate_________________ C8 Sulfonate
Amount Amt Found Amount
Amt Found Amount
Amt Found Amount
Amt Found Amount
Spiked In Sample Recovered Recovery In Sample Recovered Recovery In Sample Recovered Recovery In Sample Recovered Recovery
(noAnL) (ng/mL) (ng/mL) (%)
(ng/mL)
(ng/mL) (ng/mL)____ (%)
(noAnL) (ng/mL)____ (%)
1
ND
0.935
94
4.00
3.78
"
3.00 4.86 186 55.8 55.8 **
500 ND 547 109 4.00 358 71 3.00 550 109 55.8 605 110
Outfall 001 SpkC
Low Lab SpHn
1
ND
0699
70
4.00
3.95
"
3.00 4.70 170 55.8 60.6 **
Outfall 001 SpkO
H lg h U b S p lln
500
ND
211 , 42 4.00 277 55 3.00 396 79 55.8 459 81
Field Blank
Low FMd SpUn
1
ND 1.03 103 ND 1.25 125 ND 1.18 118 ND 1.15 115
Field Blank
High FMd SpUn
500
ND
517 103
ND
556 111
ND
626 125
ND
585 117
Sample Description
O u tfa ll 001 Low FMd SpUn
FBSA
FOSA
Me-FBSE-OH*
Amount Amt Found Amount
Amt Found Amount
Amt Found Amount
Spiked In Sample Recovered Recovery In Sample Recovered Recovery In Sample Recovered Recovery
(ngAnL) (ngAnL) (ngAnL) (%)
(ngAnL) (ngAnL) (%)
(noAnL) (ngAnL) (%)
1
3 4 .0
3 2 .9
6 .0 8
6 .9 5
**
ND
ND
-
Outfall 001
High FM d S p lln
500
3 4 .0
553
104
6 .0 8
. 552
109
ND
492 98
Outfall 001 SpkC
Low Lab SpUn
1
3 4 .0
3 5 .2
"
6 .0 8
5 .8 0
**
ND ND -
O u tfa ll 001 S p k D
High Lab SpHn
500
3 4 .0
354 64
6 .0 8
357 70
ND
319 64
Field Blank
Low FM d 8 p ltn
1
ND
1 .1 0
110
ND
1 .0 7
107
ND
ND
-
Field Blank
High FM d 8piks
500
ND
518 104
ND
514 it e
ND 320 64
ND = 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.
JK.30305518 Research Drive j T ^ S tSatate College, PA 16801, USA
VT: 800.281.3219 F: 814.272.1019 exygen.com
SECTION C
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
L o g in # :
L0001265 > 1,375
Project:
P0000430
Project T itle/Type: Fluorochemicals by LC M SM S / R O U TIN E
Project Storage:
Submitted By: D R . W ILLIAM REAGEN
Status:
U n re c e iv e d
Login Type: Started: D ate Start: Due Date:
Im m ediate Receipt of Sam ples T 11/5/2003 3:16:01PM 1 1 /1 9 /2 0 0 3
Received Date: Received By:
1 1 /0 5 /2 0 0 3 AMMERMAN, MARK
Spread Sam ple:
Label:
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Direction / Handled By
RECEIVED AMMERMAN, MARK
C ontainer # C0018516 C0018517 C0018518 C0018519 C0018520 C0018521 C0018522 C0018523
G ross W eight pH
C ontainer Type
618.9 g
500 ml Clear Plastic
607.3 g
500 ml Clear Plastic
267.9 g
500 ml Clear Plastic
284.8 g
500 ml Clear Plastic
262.3 g
500 ml Clear Plastic
244.4 g
500 ml Clear Plastic
251.7 g
500 ml Clear Plastic
615.1 g
500 ml Clear Plastic
M iscellaneous Item Key None
Description
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ICOC
M fg. Lot
Mfg. ID
Sample ID L0001265-0001 L0001265-0002 L0001265-0003 L0001265-0004 L0001265-0005 L0001265-0006 L0001265-0007 L0001265-0008
Matrix LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID
Fraction W ater W ater W ater W ater W ater W ater W ater W ater
Samples
Sample Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite Dup Field Control / Travel Blank Outfall 001 Low Spk (1.0 ppb) Outfall 001 High Spk (500 ppb) Field Blank Low Skp (1.0 ppb) Field Blank High Spk (500 ppb) Equipment Blank
Date Sampled Date Received 11/05/2003 11/05/2003 11/05/2003 11/05/2003 11/05/2003 11/05/2003 11/05/2003 11/05/2003
Date Due 11/19/2003 11/19/2003 11/19/2003 11/19/2003 11/19/2003 11/19/2003 11/19/2003 11/19/2003
11/5/2003 Login.rpt
Report Version: Oct 23 2003 9:55AM Page 1 of 2
Instance:
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L0001265-0001
C o n ta in e r C0018516 / 500 ml Clear Plastic / NONE
L0001265-0002
C o n ta in e r C0018517 / 500 ml Clear Plastic / NONE
L0001265-0003
C o n ta in e r C0018518 / 500 ml Clear Plastic / NONE
L0001265-0004
C o n ta in e r C0018519 / 500 ml Clear Plastic / NONE
L0001265-0005
C o n ta in e r C0018520 / 500 ml Clear Plastic / NONE
L0001265-0006
C o n ta in e r C0018521 / 500 ml Clear Plastic / NONE
L0001265-0007
C o n ta in e r C0018522 / 500 ml Clear Plastic / NONE
L0001265-0008
C o n ta in e r C0018523 / 500 ml Clear Plastic / NONE
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M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod
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.* ?
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4. Sampler should print their name in the space provided,and sign their name followed by the date of
the sampling event.
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sample matrix, no. of containers a n if preservative used.
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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.
\ ^ V. '
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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 satisfyjyour requirements, arrangements must be made prior to samples being submi^e^ to the laboratory. Contact your project manager.
3
Special Project Requirements such as Low"Level Detection Limits or level of Q reported must
be indicated on the chain of custody. (Use Additional Comments Section.)1' ' `
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.\
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s.com
Required Client Information:
Section A
Company
3 /
frjS S ,
Address
CHAIN-OF-CUSTODY / Analytical Request Document
The Chain-of-Custody is a LEGAL DOCUMENT. A ll relevant Helds m ust be com pleted accurately.
Required Client Information:
Section B
ReportTq:
_
/Wt.
S. FMrt'Jme.
Copy To:
'
____________________
Page:
of
Invoice To:
Client Information (Check quote/contract)
Requested Due Date:
*TAT:
639448
To Be Completed by Pace Analytical and Client Quote Reference:
Section C
Project Manager:
Rhone \
Fax
33
P.O.
Project Name:
OtAfa-L o o \ r e ,
Project Number:
Q T C iy
* Tum around times less than 14 days subject to laboratory and contractual obligations and may resuit in s Rush Turnaround Surcharge.
Tum Around Time (TAT) in calendar days.
# Containers | Unpreserved I
date
COLLECTED
S e c tio n D
Required Client Information:
SAM PLE
ID
i One charac^Rpe^box. (A-Z, 0 -9 A - )
Scimple IDs M UST BE UNIQUE
Valid Matrix Codes ----------------
MATRIX
CODE
WATER
W1
SOIL
SL
OIL OL
WIPE AIR
WF AR
J / V
TISSUE
TS
OTHER N OT
tu o o o X CC
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Project #: Profile #:
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SA M PLE CO NDITIO N
Temp in C
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Received on Ice m Sealed Cooler ( K M
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SAMPLE NOTES f "
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SAM PLER NAME AND SIGNATURE
DATE Signed: (MM / DD / YY)
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report will be sent arid contact cap,J?;e j f a i l e j i ^$S$orts arise), b|ig|p(i j^ ^ ^ tjip n ^ jc liffe re n t from
client, PO#, .Reject Name and/or Project Number as it w^appearorLthe report. ^ !
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(.O^'- '2'.N0 `5o'te Rdfrence, Projecf Manager. Projet No. arid Profile! No. Wjll be completed by Pace
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4. Sampler should print thjeir name in th spa&.proyid,dl ^nd sign their narrie followed by the. date of
the sampling event. I i ! ' ;
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sample matrix, no. of containers and"preservative used.
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report; inclucjp tir^ ^ s ^ i^ p lirig ,^ r ,0 7 llv';': ' \.
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6. Analysis Requested: Complete analysis on the lines provided arid place a check in the column for
the samples requiring the analysis. It may be necessary to usej the space provided for additional
comments ofincludeattaphments for extended lists of parameters.
,
:: |
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;:
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7. Submission of samples tb laboratory: Indicate Item Number oflthose samples being transferred;
sign relinquished by, and include your affiliation:
I ' : " ; "" i ';
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* IMPORTANT NOTE:
j
__ Standard Turnarourid Time is:2 weeks. If this does not satisfy!your requirements, arrangements must be made prior to samples being submitted to the ial
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Special Project Requirements such as LowHeg^j Detection Limits or levetof QC repwtedarROTfe
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R equired Client Information:
Section A
Company
rri &
Address
CHAIN-OF-CUSTODY / Analytical Request Document
The Chain-of-Custody Is a LEGAL DOCUMENT. A ll relevant fields m ust be com pleted accurately.
Required Client Information:
Section B
"I f c Tk s r F l4 ,, .< L , I
Copy To:
IfS S :
of
Invoice To;
Client Information (Check quote/contract):
Requested Due Date:
*TAT:
639448
To Be Completed by Pace Analytical and Client Quote Reference:
Section C
Project Manager:
fis ti)
Fax
P.O.
Project Name:
O utfhLU O P I T O
Project Number
& rd y
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.
W F o - Q 8V*
Profile #:
Requested Analysis:
MATRIXCODE^
SS; COLDLAETCETED 33*T -- 3 TIME ,, COLLECTED "O #Containers | Unpreserved NaOH Methanol Other
Section D RequiredClientInformation:
4*
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SAMPLE ID One(cAtt-aZr,ac-ff9cphe~r)^jox.
Siimpie IDs MUSTBE UNIQUE
p j d lA h i e^_DO H t!k J
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VWMaAAliTTdREMRIXatrixCodeCWsO1D--E--- --_
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SHIPMENT METHOD
J AIRBILL NO. | SHIPPING DATE jNO. OF C O O L E R S ^ TM ,! RELINQUISHED BY / AFFILIATION ! DATE i TIME i ACCEPTED BY / AFFILIATION
SAMPLE CONDITION Temp in C
Received on Ice Y/N Sealed Cooler f Y/N
Samples Intact 'Y/N -------------------------- 1 Additional Comments:
*M 0 oz.
ML
SAMPLER NAME AND SIGNATURE
PRINT Name of SAMPLEI
DATE Signed: (MM / DD / YY)
tnemuooQ tssupsfllBoitylfiAX YQQTSUO-^O-MIAHO
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Instructions for completing Chain of Custody (COC)
1^ 7 b<i .www
A noifosS
2* V ^
1. ^>blK0letg.sarsciienf^formationatUSp of sheet: 'M5e,: address, phone, contact (person to whom
report will be sent and contact can bre Made if questions arise),
ji^q^^tit>j1;^|idifferent from
client, RO`#r ProjectName and/or Project Number as it .wjjOappear-'onlhe report.- *
':i JilO L`-`\ l psH 4IhtiM b0 J
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: \
7 7 7^ . NQ5cSte Rfrence, Project
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er, Project No, and,Profile No; will be completed by Pace.
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to enO
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4. Sampler should print ,thelf name in the Spa&pro\4id4 and sign their name followed by thp date of
the sampling eveenrti. ! ! !
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; i r - - ' .(Vi \ <U> - i -* *\ T K i'7
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5. Complete Sample Description as y ^ l appear on tl^p labprpjptry report:; inclucj'p t i f ^ ^ i q m p l i p ^ ^
sa/nple matrix, no. of containers anc^preservative gsved.
o'
7 7l
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6. Analysis Requested: CCnpplete analysis on the lines provided and place a check in the column for the samples requiring trip analysis. It may be necessary to usejthe space provided for additional comments or include attachments for extended lists of parameters.; ,
1 ' ' M : ' : !
: i !
"
'
7. Submission of sampfes to laboratory: Indicate Item Number o f`those samples being transferred;
sign relinquished by, arid include your affiliation!.
IMPORTANT NOTE:
Standard Turnaround Time is 2 weeks. If this does not satisfy your requirements, arrangements
V /!
M\
Special Project Requirements such as Low Le^jl Detection Limits or levetof QC reported?rrasfc
:OITiOM O? 3 .;'5?*Ae_
be indicated pn the chain of custody. (Use AdditionaT Comments S e c tio n ^ T .,v ' '
.
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Required Client Information:
Section A
^,/nCompany TT V ss
Address
Required Client Information: Report Toe
/m t.
Copiwy TTo/v:
5-
.
Invoice To:
CHAIN-OF-CUSTODY / Analytical Request Document
The Chain-of-Custody is a LEGAL DOCUMENT. A ll relevant fields m ust be com pleted accurately.
Section B
Page:
of
r
Client Information (Check quote/contract):
Requested Due Date:
*TAT:
639448
To Be Completed by Pace Analytical and Client Quote Reference:
Section C
Project Manager:
Rhone \
Fax
P .O .
Project Name:
OtSht-L coi T O
Project Number:
* 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.
Project #:
Fq 3 -
Requested Analysis:
Section D
Required Client Information:
SAMPLE ID
. O ne cffera p fe -p er^bo x.
(A -Z , 0 -9 /.-)
S am ple ID s M U S T B E U N IQ U E
o A1
JLh i B______ Q O ... r C T L
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J E T t f r i i L fir * * * 1 * L [& L
r
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Valid Matrix Codes -4 -
MATRIX
CODE
WATER
W1
SOIL
SL
OIL OL
WIPE
WF
AIR AR 3 *
TISSUE
TS
OTHER
OT -
&
fill ;
-
b im y r i t i ~t * i u w , *> r A r W
o LU
do
o
mm / dd / yy
ttfshs
M v/ i
fjf/ p j tth / v s
t2y
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LU
P do
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/v ig
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Preservatives
COCMozm o
XXX
CO
I 0
o CM CO
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11
t
K (5
1i
its rji " .
pSf
fifa 1
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CtK
| rj !
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MATRIX CODE # C ontainers Unpreserved |
M e th a n o l ___ I
Other |
/{A p t*
/ J - t / c y g w s fT / / /
.
/ /
/ /
/ /
/ /
^ // //
// ^/ ^ / /
/ / Remarks / Lab ID
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SHIPMENT METHOD
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AIRBILL NO
SHIPPING DATE |NO. OF C O O L E R S L ^ er| RELINQUISHED BY/AFFILIATIO N I DATE I TIME |
<te.: h '
ACCEPTED BY / AFFILIATION
I DATE I TIME
SAMPLE CONDITION Temp in C
Received on Ice Y^N Sealed Cooler Y/N Samples Intact ,Y/N Additional Comments:
SAMPLE NOTES 4 * -
<
f
* ri'
o oz.
po', W
O
A
T,rA
o .o ^
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7 -------------- -- ----------- i ,
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SAMPLER NAME AND SIGNATURE
PRINT Name of S A M P L E R ^
/-
T- (
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SIGNATURE of MPL3EflT _
Y ry . -o e r--
DATE Signed: (MM / DD / YY)
-
O N r\ h , ` d
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. Qute 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.
1 -;
' : ',
I : :
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4. Sampler should print their name in the space provided and sign their name followed by the date of
the sampling event.
-
;^
i'
,
5. Complete Sample Description as it yviD appear on tl^e laboratory report; include time of sampling,
sample matrix, no. of containers and preservative used.
.''
\'
"
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.
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
exten. ded
lists
of
parameters.
7.' Submission of samples to laboratory: Indicate Item Number of those samples being transferred; sign relinquished by, and include your affiliation.
;;
-3
' -r
. ....
I|J
"'S*
!! /
* IMPORTANT NOTE:
:'
j
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.)
o
.-- s, .-sa^T~Br-
PROJECT INFORM ATION
Client (name & address): 1
CHAIN OF CUfFODY/ANALYSIS REQUEST FORM
Exygen Research Sample Receiving 3 1 17 Research Drive State College, PA 16801, USA 1: 8 1 4 .2 3 1 .8 0 3 2 F: 8 1 4 .2 3 1 .1 5 8 0 fefaygenresearch.com
Page
.i of /
ANALYSES REQUESTED
Project Manager (Name & E-mail Address):
Phone: ( (rSJ ^ Fax:________________________ Sampler: ___________________
Project Name;!
RO. #: Quotation #:]
fM it- >oi
Please fill out this form com pletely to ensure correct analysis anBSroper handling of your samples.
SAMPLE ANALYSIS
C lie n t S am ple Id e n tific a tio n O u f/fti-L 0 0 1 f i( iu r - t C p *p t , ^ L L cot g f f . C a*f tp
fif<P /wjrfrl 11 *
^ T u i'y m u d '
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C o llectio n Tim e
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C om m ents 3 # 7 6? I 3 3 y
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LAB USE ONLY
CHAIN OF CUSTODY
OTHER INFORMATION
C /o le r i f i t m u a a b v 11?
^ ...... . .
.
LAB USE ONLY
b:: ''
C ooler Tem p. (C ) I D ate / Tim e y iir h
-
PROJECT REQUIREMENTS Results Deadline:
Laboratory Report Options: |~1 Sample results only I I Add case narrative I I Add quality control summary l~1 Add calibration summary I~1 Add raw data D O th er___________________
REV. 3-02
I John Q uarrr- D e
- LR pdfpdf
Fige 11
10/21/2003
Project: E03-0848
3M ENVIRONMENTAL UVBORATORY Preliminary/UnauthorizecFeport
Requester; Schnobrich, Dana M (223-lN -08)
Department: 530711
Project Number: 0022674449
Date Received: 10/21/2003
.
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 Resulte/Actlvity Pace Field Sampling Event
3M SampleNumber E03-0848-61834
SampiedDate 11/3/2003
Sample Description Outfall 001 Effluent - Composite
LAB EXYGEN
Analytical Method LCMS
. . ;
' .' ,
.
.
E03-0848-61835 "
`' . ' 11/3/2003
Components
Result
PFOS
PFHS
PFBS
FOSA.
' '
PFBAmide
MeFBSE-OH
C4 acid
C5 acid
C6 acid
C7 acid
PFOA
C9 acid
CIO acid
C ll acid
C12 acid
-- " Outfall 001 Effluent - CompositeDuplicate
LAB EXYGEN
Analytical Method LCMS
:
E03-0848-61836
11/3/2003
Components
PFOS
PFHS
' PFBS
FOSA
'
PFBAmide
MeFBSE-OH
C4 acid
C5 acid
C6 acid
C7 acid
PFOA
C9 acid
CIO acid
C ll acid C12 acid
Field Control/Travel Blank
Result
.
';
RL Qualifier RL Qualifier
I John Q ualtieri - ecatur 4 Q..0. 3 FG - LRpdf.pdf
10/21/2003
3M ENVIRONMENTAL LABORATORY Preliminary/UnauthorizecReport
Project: E03-084S (coni) 3M SampleNumber
E03-0848-61836 (coni)
SampledDate 11/3/2003
Sample Description Field Control/Travel Blank
LAB
EXYGEN
Analytical Method LCMS
E03-0848-61837
11/3/2003
Components PFOS
PFHS
PFBS
FOSA
PFBAmide
MeFBSE-OH
C4 acid
.
C5 acid
C6 acid
C7 acid
PFOA
C9 acid
CIO acid
,
C ll acid
C12 acid
EquipmentBlank
LAB
EXYGEN
Analytical Method LCMS
Components PFOS
PFHS
PFBS
FOSA
PFBAmide
MeFBSE-OH
C4 acid
CS acid
C6acid
C7 acid
PFOA
C9 acid
CIO acid
,
C ll acid
C 12 acid
Result Result
2 of 2 R L Qualifier
RL Qualifier
F jg T j \
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USA A ir b ill FedEx Tracking
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Recipient's
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