-------
Table A: PFAC-MXJ: Components and Concentrations (uq/mL:
± 5% in methanol)
Compound
Acronym
Concentration
(pg/mL)
Peak
Assignment
in Figure 1
3-Perfluoropropyl propanoic acid
FPrPA
4.00
A
3-PerfluoropentyI propanoic acid
FPbPA
20.0
B
3-Perfluorohepty! propanoic acid
FHpPA
20..0
C
Certified By: Date: 09/23/2021
^ni m.'rtn ''y/yy<
B.G. Chittim, Genera! Manager
futmH 11, *'u04-f MU
fTACMXJ0921 ,lof 5
Tt-^O
-------
Figure 1: PFAC-MXJ; LC/MS Data (SIR)
14sept2021 _PFAC MXJ_008 14-Sep-2021 12:22:41
PFACMXJ0921 1/50 dil
100
2: SIR of 7 Channels ES-
TIC
4.13e5
0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50
100
5.00 5.50 6.00
2: SIR of 7 Channels ES-
TIC
4.19e6
>H"|~ i "I * II rl-t 1 | , f-TTTl M • | • I ¦ | 1 ' r i 1 ~ • J ¦ ~1 1 i ¦ I ' < | ' i ' - i ' 1 ' | 1 ¦ i ' • 'I f v f-r.-r '"",f " 'THTi 'i '| p ' rtT' ]' ' ] '• ' * i : --1 " • | ¦ J ¦
0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00
100
2: SIR of 7 Channels ES-
TIC
4.89e6
0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4,50
5.00 5.5D
6.00
Time
Conditions for Fiqurel:
Waters Acquity Uttra Perforrnance LC
Waters Xevo TQ-S micro MS
Chromatoaraohic Conditions:
Column: Acquity UPLC BEH Shield RP,a
1.7 pm, 2.1 x 100 mm
WIS Parameters:
Experiment: SIR
Mobile phase: Gradient
Start: 50% H O / 50% (80:20 MeOH:ACN)
(both with 10 mM NH.OAc buffer)
Ramp to 90% organic over 9 min and hold for
2 min before returning to initial conditions in 1 min.
Time: 15 min
Source: Electrospray (negative)
Capillary Voltage (kV) = 2.50
Cone Voltage (V) = variable (2-74)
Desolvation Temperature (°C) = 350
Desolvation Gas Flow (L/hr) = 1000
Flow: 300 pL/min
Form#: 13, Issued 2004-11-10
Re vision Revised 2020-12-23
PFACMXJ0921 (4 of 5)
revO
-------
Figure 2: PFAC-MXJ; LC/MS/MS Data (Selected MRM Transitions)
14sept2021_PFACMXJ_001 14-Sep-2021 09:45:06
PFACMXJ0921 1/50 dil
100
241>177
2.56e4
FPrPA
[C6H4F702]- — tC5H3F6]-
0.50 1.00 1.50 2.00 2.50 3.00
3.50
100
FPePA
0.50
1.00
1.50
2.00
2.50
3.00
3.50
100
FHpPA
4.00 4.50 5.00 5.50
6.00
341 > 237
4.24e5
[C8H
4^1 lOz]
[C7HF8]-
4.00
4.50
5.00 5.50
6.00
[C10H4F15OJ- — tc9F„]-
441> 317
1.52e5
Time
0.50 1.00
1.50
2.00
2.50
3.00
3.50
4.00
4.50 5.00
5.50
6.00
Conditions for Flaure 2:
injection: On-column (PFAC-MXJ)
MS Parameters:
Collision Gas (mbar) = 3.31 e-3
Mobile phase: Same as Figure 1
Collision Energy (eV) = 6-60 (variable)
Flow: 300 jjL/min
Form#: 13, Issued 2004-11-10
Re vision Revised 2020-12-23
PFACMXJ0921 (5 of 5)
revO
-------
Attachment 7
ERA Cooler Study Report in Support of the HGL/DoD PFAS
Multi-Laboratory Method Validation Study - January 2022
(Dated January 2022)
-------
ERA Cooler Study Report in Support of the HGL/DoD PFAS Multi-
Laboratory Method Validation Study- January 2022
Table of Contents
Purpose...
Objective.
Procedure
1
1
1
Study Evaluation and Results
Conclusion
5
2
Appendix
7
1. Purpose:
¦ To assess the ability of the aqueous matrix samples to retain a temperature of < 6°C during the scheduled 24 hr.
shipping process and to measure/document sample temperatures out to 120 hours under ambient external
temperature conditions.
2. Objective:
¦ To assess if pre-frozen aqueous samples will be able to maintain a < 6°C temperature under ambient shipping
conditions when packed per normal ERA protocol and shipped in ERA coolers to participating laboratories.
3. Procedure:
1. (7) large shipping coolers (25" x 15.5" x 17" Styrofoam cooler in a cardboard shipping box) were assembled for
2. (108) 1L HDPE bottles were filled with approximately 500 mL of tap water to represent study samples. Bottles
were stored at < 0 deg C for a minimum of 16 hrs. or until frozen.
3. Each cooler was packed according to ERA Work Instruction 730002425 Whole Volume Cooler Shipping.
• A minimum of 26 freezer packs (blue ice type) were used per cooler.
• A layer of freezer packs was placed in the bottom and top of the cooler.
• Each cooler was filled with 13 pre-frozen 1L Amber HDPE bottles containing tap water and packed per
this protocol for shipping.
• Any remaining space around and on top of the bottles was filled with additional insulating material
(foam sheets, bubble wrap or packing paper) or ice packs.
4. Each cooler was labeled 1-7 corresponding to the different time interval of 12, 24, 36, 48, 72, 96 & 120 hours.
5. Initial sample temperatures for each of the seven coolers was taken with an IR temperature gun prior to cooler
sealing. Sample #1 was checked for this temperature.
6. The (7) coolers were placed at ambient temperature in a central location of ERA's lab under four large work
benches for this project.
• This location is environmentally controlled and is suggested to best represent temperature conditions
during shipment (according to the planned schedule).
• A thermometer was placed adjacent to but outside of the coolers to monitor ambient room
temperature.
the study.
Page 1 of 7
-------
7. One cooler was opened, and the temperature was checked at each time intervals: 12, 24, 36, 48, 72, 96 & 120
hours (± 30 minutes). At each interval, the time was recorded, and the following performed:
• The temperature for the 3 samples from across the cooler was checked with an IR temperature gun and
the results were recorded.
• The ambient room temperature was checked and recorded
8. Results were compiled in an Excel spreadsheet which is included at the end of this document.
4. Study Evaluation/Results;
The 1L Amber bottles exhibited either a very slight or no apparent bulge in the side of the bottle after the water
became frozen. If the bulge was noticed it was located at the top of the frozen water level from the expansion of the
ice (see photo below). None of the 108 frozen bottles broke and all bulges that were observed were insignificant
and would have no impact on the structural integrity of the bottle.
I
The first five (of seven) coolers were packed on 1/10/2022 and three samples in each cooler were randomly labeled
1-3. The Ambient temperature and the temperature of a single bottle from each cooler was recorded at the time of
the initial cooler packing. See photos of packing configurations within the coolers below.
Page 2 of 7
-------
Page 3 of 7
-------
At each time interval the temperature of the three bottles, the ambient temperature and the thermometer IDs were
recorded. All data for the cooler study were recorded and entered in a spread sheet (which is included at the end of
this document). Samples for the 12 and 24 hr. check remained completely frozen. A small amount of thawed water
(~ 10 mL) was noticeable in the bottles at the 36 hr. check. At the 72 hr. check, bottles were about % frozen and Va
thawed. It was decided to extend the cooler study to 96 hr. and 120 hr. checks to anticipate any delays that may
occur with the delivery carrier for the planned overnight deliveries. At the 96 hr. check, bottles 1 and 3 (which were
located along the outside of the cooler) were % frozen and % thawed. Bottle 1 (located in the middle of the cooler)
Page 4 of 7
-------
had only ~ 20 ml of thawed water. At 120 hrs., all sample temperatures were below 0°C and the volumes of thawed
water can be seen in the following two pictures below.
Pictures Representing Volume(s) of Thawed Water After 120 hrs.:
Bottle #1 - 60 mL Bottle #2-180 mL Bottle #3 - -300 mL
5. Conclusion:
The current cooler packing design will keep all samples in the coolers frozen for the planned shipping duration of 24
hrs. and if the samples are shipped within the originally scheduled proposed timeline. The coolers will keep the
samples at least half frozen and below 0°C for a duration of 120 hrs. (under the conditions of test). If it is decided
Page 5 of 7
-------
that the samples need to be received completely frozen and/or additional shipping conditions or if the distribution
schedule is adjusted to a time when the ambient temperature may be significantly higher, further testing may be
needed.
Page 6 of 7
-------
Appendix:
HGL/DOD PFAS Cooler Temperature Study Log
A Wstsrs Contpurty
Cooler ID
Temp.
Check
Start Date/Time
of Cooler Study
Initial
Temp.
Check*
Scheduled
Date/Time
to be Checked
Bottle
#1
Temp.
Bottle
#2
Temp.
Bottle
#3
Temp.
IR
Thermometer
ID
Ambient
Temp.
Ambient
Thermometer
ID
Initials
Date/Time
Checked
Comment
Cooler #1
12 hr.
1/10/202216:40
-19°C
1/11/2022 5:30
-1.9°C
-3.1°C
-2.6°C
TH-118
2i. rc
TH-65
ES
1/11/2020 5:30
Samples completely frozen.
Cooler #2
24 hr.
1/10/202216:40
-14°C
1/11/202217:30
-1.6°C
-1.8°C
-1.6°C
TH-118
2i. re
TH-65
AJC
1/11/2022 16:40
Samples completely frozen.
Cooler #3
36 hr.
1/10/202216:50
-18°C
1/12/2022 5:30
-1.4°C
-2.3°C
-2.4°C
TH-118
20.8°C
TH-65
ES
1/12/2022 5:30
Little thawed water noticeable ~10 mL.
Cooler #4
48 hr.
1/10/202217:00
-19°C
1/12/202217:30
-1.4°C
-1.8°C
-1.9°C
TH-118
21.3°C
TH-65
MG
1/12/2022 16:50
N/A
Cooler #5
72 hr.
1/10/202217:00
-19°C
1/13/202217:30
-1.0°C
-1.6°C
-1.1°C
TH-118
21.1°C
TH-65
AJC
1/13/2022 16:35
Samples 3/4frozen, l/4thawed.
Cooler #6
96 hr.
1/14/202210:30
-16°C
1/18/202210:30
-0.9°C
-1.6°C
-0.5°C
TH-118
2i. rc
TH-65
BPM
1/18/2022 10:32
Bottle #2 middle cooler location
~20mL thawed, outside bottle 1&3
~3/4frozen, ~l/4thawed.
Cooler #7
120 hr.
1/14/202210:30
-17°C
1/19/202210:30
-0.9°C
-0.6°C
-0.4°C
TH-118
20.0°C
TH-65
BPM
1/19/2022 10:35
Bottle #1 middle cooler location 60mL
thawed, thawed. Bottle #2 outside
location 180 mL thawed and bottle #3
outside location ~300mL thawed.
Mark bottles, randomize marked bottles in coolers.
All coolers stored under micro benches in the lab.
* Initial Temperature Check performed using IRThermometer ID : TH-118. All on Bottle #1
Initial ambientTemp = 20.9°C
Page 7 of 7
-------
PFAS Multi-Laboratory Validation Study Report
Aqueous Media: Wastewater, Surface Water, and Groundwater
SERDP
Appendix B
Preparation of PFAS-
Spiked Samples
Date: July 25, 2023
-------
Waters
THE SCIENCE OF WHAT'S POSSIBLE."
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 1of14
Content Table
1 PURPOSE 1
2 SCOPE 1
3 DEFINITIONS AND ABBREVIATIONS 3
4 ROLES AND RESPONSIBILITIES 3
5 REFERENCES / RELATED DOCUMENTS 4
6 FORMS 5
6.1 Records 5
7 HEALTH & SAFETY 5
8 EQUIPMENT/MATERIALS 5
9 PROCEDURE/INSTRUCTION 6
9.1 Matrix Check-in & Preparation Process 6
9.2 Matrix Characteristics Testing 9
9.3 PFAS Spiking Concentrate Manufacturing & Verification Process 9
9.4 Sample PFAS Spiking Process 10
9.5 Sample Shipping Process 10
9.6 Certificate of Analysis and Sample Instructions Generation 11
10 APPENDICES /ATTACHMENTS 12
1 PURPOSE
1.1 The purpose of this procedure/work instruction is to supply samples for a characterization determination
and a Multi-Laboratory Validation Study for per-and polyfluoroalkyl substances (PFAS).
2 SCOPE
2.1 The scope of this procedure is to prepare the defined sample matrices for characterization testing and
then spiking the prepared matrices with known amounts of PFAS analytes for a Multi-Laboratory
Validation Study for analytical Method 1633 - October 2021.
2.1.1 Matrix Characterization for PFAS and Chemical Characteristics:
Sample Chart 1 - PFAS Characterization Samples
Matrix
Matrix
Type
Number
Matrix
Types
Number of
Unspiked
Samples
Total Number
of Samples
Shipping/
Matrix Type
Volume/Mass
to be provided
for each
Sample
Water
Wastewater
9 1
3
27
550 mL
Groundwater
3
3
9
550 mL
Surface Water
4 2
3
12
500 mL
Landfill Leachate
3
3
9
125 mL
Soil/Sediment
Soil
83
3
24
10.0 g
Sediment
3
3
9
10.0 g
Biosolids
3
3
9
1.00 g
Tissue
Fish/Clams4
3
3
9
10.0 g
Total Number
108
Footnotes:
1 Eight wastewaters were received by ERA and ERA will manufacture one substitute wastewater following ASTM method
Template 730000483 V08
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HARD COPY UNCONTROLLED UNLESS STAMPED, SIGNED AND DATED BY AUTHORISED PERSONNEL
-------
Waters
THE SCIENCE OF WHAT'S POSSIBLE."
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 2 of 14
D5905-98 (Reapproved 2018).
2 Four different surface water lots were received by ERA.
3 Eight different soil lots were received by ERA. One received soil lot does not contain enough sample to supply all samples for the study.
4 Two fish filets (salmon and walleye) with skin were received and un-shucked clams.
Sample Chart 2 - Chemical Characteristics Testing
Analyte
Analytical
Method
Container
Preservation
Minimum Sample
Volume/Mass
Number
of Lots 1
Number of
Unspiked
Samples per Lot
Holding
Time
Aqueous Samples
Alkalinity (total, carbonate and bicarbonate)
SM 2320B
250 mL HDPE
< 6°C
100 ml
19
1
14 days
Ammonia
EPA 350.1
250 mL Amber
Glass
< 6°C, H2S04
250 ml
19
1
28 days
Calcium, sodium
SW 6010C
250 mL HDPE
< 6°C, HNO3
50 ml
19
1
6 months
Chloride, sulfate
SW 9056A
250 mL HDPE
< 6°C
100 ml
19
1
28 days
Conductivity
SW 9050A
250 mL HDPE
< 6°C
50 ml
19
1
28 days
Oil and grease
EPA 1664B
1000 mL Amber
Glass
< 6°C, H2SO4
1 L
19
1
28 days
pH
SW 9040C
250 mL HDPE
< 6°C
100 ml
19
1
Immediately
Total dissolved solids
SM 2540C
250 mL HDPE
< 6°C
100 ml
19
1
7 days
Total suspended solids
SM 2540D
250 mL HDPE
< 6°C
100 ml
19
1
7 days
Soil and Sediment Samples
Grain Size
ASTM D422
16 oz Plastic or
Glass Jar
None
500 g
11
1
Not defined
Moisture
ASTM
D2216
4oz Glass Jars
< 6°C
20 g
11
1
1 year
pH
SW 9045D
4 oz Glass Jars
< 6°C
50 g
11
1
Immediately
Salinity (sediment only)
SM 2520B
4 oz Glass Jars
< 6°C
50 g
3
1
6 months
Total Organic Carbon
SW 9060A
4 oz Glass Jars
< 6°C
10 g
11
1
28 days
Tissue
Lipids
SM 2540B
4 oz Glass Jar
< 6°C
20 g
3
1
1 year
Biosolids
pH
SW 9045D
4 oz Glass Jar
< 6°C
50 g
3
1
Immediately
Total Number of Samples Shipping: 188
Notes:
EPA Methods - USEPA Methods for Chemical Analysis of Water and Wastes (MCAWW) USEPA/600/4-79-020, Revised March
1983.
SW Methods - USEPA Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, SW-846, Third Edition, 1998.
SM Methods - Standards Methods for the Examination of Water and Wastewater, Revised 2018
ASTM Methods - ASTM International, Revised 2019
Footnotes:
1 Refer to Sample Chart 1 for further information regarding Matrix Type.
2.1.1.1 Samples listed in Sample Chart 1 will be sent to SGS AXYS for PFAS characterization
testing and samples listed in Sample Chart 2 will be sent to Eurofins TestAmerica
Denver for sample chemical characteristics testing.
2.1.2 Multiple Laboratory Validation Study Samples:
2.1.2.1 The chart below lists the matrix types, spiking levels and sample quantities required for
the Multiple Laboratory Validation testing.
Template 730000483 V08
It is the responsibility of the user to verify they are using the current released version.
HARD COPY UNCONTROLLED UNLESS STAMPED, SIGNED AND DATED BY AUTHORISED PERSONNEL
-------
Waters
THE SCIENCE OF WHAT'S POSSIBLE."
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 3 of 14
Multiple Laboratory Validation Study Sample Chart
Matrix
Matrix
Type
Number
Matrix
Types
Number of
Unspiked
Samples/
Matrix Type
Number of
Replicates
Spiked at
Low Level1/
Matrix Type
Number of
Replicates
Spiked at
High Level1,2/
Matrix Type
Total
Number of
Samples
Shipping/
Matrix Type
Spiked
Volume/Mass to
be provided for
each Sample
Water
Wastewater
7
1
3
3
49
500 mL3
Groundwater
3
1
3
3
21
500 mL3
Surface Water
3
1
3
3
21
500 mL3
Landfill Leachate
3
1
3
3
21
100 mL3
3
21
5.00 g3
Sediment
3
1
3
3
21
5.00 g3
Biosolids
3
1
3
3
21
0.500 g3
Tissue
Fish/Clams
3
1
3
3
21
2.00 g3
Total Number
205
Footnotes:
1 Low and High levels for spiking defined in analytical method "Analysis of Per-and Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue
Samples by LC-MS/MS", October 2021.
2 Except for FTSs spiked at 1.5 times low level.
3 Labs will be instructed to use the entire sample contents for analysis and assume the volume or mass listed.
2.1.2.2 Samples listed in the Multiple Laboratory Validation Study Sample Chart will be sent to
the labs that were selected for the Multiple Laboratory Validation Study.
2.1.2.3 ERA will prepare 5 extra sets of prepped samples for use as: replacement samples,
future testing, and/or other use by the client.
2.1.3 Analyte lists as determined from the analytical Method 1633 - October 2021 (as referenced
above) will be confirmed by the SERDP/ESTCP team. New analyte addition(s) to be reviewed
and approved by ERA Technical department.
2.1.4 Final product concentrations as determined from the analytical Method 1633 - October 2021 (as
referenced above) will be confirmed by the SERDP/ESTCP team.
3 DEFINITIONS AND ABBREVIATIONS
3.1 PFAS - Per-and Polyfluoroalkyl Substances
3.2 GHS - Globally Harmonized System
3.3 HDPE - High Density Polyethylene
3.4 PWS - Performance Work Statement
3.5 NIST - National Institute of Standards & Technology
3.6 CofA - Certificate of Analysis
3.7 DWBSS - Dry Weight Basis Sample Size is the state of the soil without the presence of water.
4 ROLES AND RESPONSIBILITIES
4.1 Technical Manager
4.1.1 Responsible for the project evaluation and project scope feasibility.
4.1.2 Documentation review.
Template 730000483 V08
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HARD COPY UNCONTROLLED UNLESS STAMPED, SIGNED AND DATED BY AUTHORISED PERSONNEL
-------
Waters
THE SCIENCE OF WHAT'S POSSIBLE,"
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 4 of 14
4.1.3 Providing technical assistants for the steps described in this Work Procedure.
4.2 Product Line Manager
4.2.1 Responsible for the overall project management and task scheduling of the project.
4.2.2 Documentation review.
4.2.3 Overseeing project progress for the steps described in this Work Procedure.
4.3 Chemist/Chemistry Technician
4.3.1 Responsible for performing the sample homogenizing and packaging.
4.3.2 Manufacturing PFAS concentrates and verification analysis of concentrates.
4.3.3 Perform sample spiking.
4.3.4 Preparing samples and coolers for shipping.
4.4 Production Technician
4.4.1 Responsible for performing the sample homogenizing and packaging.
4.4.2 Preparing samples and coolers for shipping.
5 REFERENCES/RELATED DOCUMENTS
5.1 The listed ERA ISO 17025 Accredited Work Procedures in the table below are associated with this
procedure.
Doc No:
Document Title
730002414
Environmental Product Packaging and Labeling
730002350
Organic Liquid Standards Preparation
730002570
Semi-volatile Analytical Verification by High Performance Liquid Chromatography
730002497
Analytical Verification of Grease and Oil in Water Samples
730002520
Analytical Verification by ICP-OES
730002523
Analytical Verification of Anions, Perchlorate and DBPs by Dionex Ion
Chromatography
730002515
Analytical Verification of Total Alkalinity in Water Samples
730002510
Analytical Verification of Ammonia in Water and Soil Samples
730002501
Analytical Verification of pH in Water and Soil Samples
730002508
Analytical Verification of Specific Conductance in Water and Soil Samples
730002492
Analytical Verification of Total Dissolved Solids in Water Samples
730002493
Analytical Verification of Total Suspended Solids (TSS) in Water Samples
730002434
Reagents Manufacturing
730002412
Environmental Product Manual Certificate of Analysis Generation
Template 730000483 V08
It is the responsibility of the user to verify they are using the current released version.
HARD COPY UNCONTROLLED UNLESS STAMPED, SIGNED AND DATED BY AUTHORISED PERSONNEL
-------
Waters
THE SCIENCE OF WHAT'S POSSIBLE,"
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 5 of 14
730002425
Whole Volume Cooler Shipping
730002254
Control of Quality Records
6 FORMS
8.1 Records
8,1.1 All records associated with this procedure will be retained by Quality according to OP
730002254 Control of Quality Records.
7 HEALTH & SAFETY
7.1 GHS Evaluation
7.1.1 ERA will perform GHS (Globally Harmonized System) evaluation as needed for product
shipments.
8 EQUIPMENT /MATERIALS
8.1 Mixing Equipment:
8.1.1 30-gal Blue HDPE Open Top Drum
8.1.2 Stainless Steel Mixer
8.1.3 Rotational Mixer
8.1.4 Food Processor
8.1.5 Mixing Bins - for solids/tissues
8.2 ERA will procure other required (non-chemical) materials. Quantities will be based upon number of
laboratories and samples. Items will include but are not limited to:
8.2.1 1000 mL amber HDPE Narrow Mouth Bottles - Thermo Scientific Part# 03-313-8F
8.2.2 1000 mL Amber Glass Bottles - ESS Part# 1000-0150-PC
8.2.3 250 mL HDPE Narrow Mouth Bottles - Thermo Scientific Part# 312002-0016
8.2.4 250 mL Amber Glass Bottles - ESS Part# 0250-0150-PC
8.2.5 125 mL HDPE Narrow Mouth Bottles - Thermo Scientific Part# 312089-0004
8.2.6 4 oz Glass Jars - Berlin Part# - GLA-00869
8.2.7 24 mL clear glass screw top vial - Berlin Packaging Part# 293339, Cap Part# CAP-00145
8.2.8 12 oz Blue Gel Ice Packs - Katzke Paper Part# MM-PP12
8.2.9 Large Styrofoam Coolers - Katzke Paper Part# CP211312C
8.2.10 Medium Coolers - Katzke Paper Part# CP121213
8.2.11 Reusable Matrix Coolers
8.2.12 Packaging Material
Template 730000483 V08
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HARD COPY UNCONTROLLED UNLESS STAMPED, SIGNED AND DATED BY AUTHORISED PERSONNEL
-------
Waters
THE SCIENCE OF WHAT'S POSSIBLE,"
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 6 of 14
8.3 ERA will work with Client to source high level PFAS starting materials from an ERA approved vendor.
ERA will consult Client with any availability or lead time concerns for vendor supplied starting materials.
8.4 ERA will procure PFAS starting materials. Lead time will be determined by vendor.
8.5 Client Supplied Matrices for preparation of PFAS spiking:
8.5.1 8 - Client supplied Wastewater Matrix Lots, 1 ASTM manufactured by ERA, 7 lots will be chosen
for the study
8.5.2 3 - Client supplied Leachate matrix lots all 3 will used for the study.
8.5.3 4 - Client supplied Surface Water matrix lots, 3 will be chosen for the study.
8.5.4 3 - Client supplied Ground Water matrix lots all 3 will used for the study.
8.5.5 8 - Client supplied Soil lots, 3 will be chosen for the study.
8.5.6 3 - Client supplied Sediment lots all 3 will used for the study.
8.5.7 3 - Client supplied Biosolids lots all 3 will used for the study.
8.5.8 3 - Client supplied Fish/Clam Tissue lots all 3 will used for the study.
9 PROCEDURE I INSTRUCTION
9.1 Matrix Check-in & Preparation Process:
9.1.1 Check-In - When each matrix is received containers will be:
9.1.1.1 Labelled:
9.1.1.1.1 With matrix type
9.1.1.1.2 Source ID from clients Chain of Custody (When Provided)
9.1 1.1.3 Container#
9.1.1.2 Login all matrices into an electronic matrix log for record keeping & organization. File is
available to client. File Location - K:Customs-WholeVolumes\Hydrogeologic PFAS
Round Robin 2020\Matrix Log.
9.1.1.3 Store labelled and logged in matrices in a walk-in refrigerator. Fish/clam tissues are
stored in a freezer until needed for preparation.
9.1.1.4 Client will be notified when each matrix has been received.
9.1.2 Matrix Preparation & Homogenizing:
9.1.2.1 Prior to the homogenization and final packaging of the matrices, composite samples
will be prepared for each matrix lot by taking subsamples from each homogenized
container and combining.
9.1.2.1.1 The unspiked composite samples of each matrix lot will be sent to SGS
Axys (PFAS) and Eurofins TestAmerica Denver (characteristic
parameters) for background analysis.
9.1.2.1.1.1 HGL will advise ERA of any dilutions or adjustments
required to any of the matrices.
9.1.2.1.1.2 Any required dilutions will be made using approximate
volumes.
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Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 7 of 14
9.1 2.1.2 Any matrix adjustment (to inorganic background parameters) will be
verified in ERA's laboratory.
9 1.2.2 Aqueous Matrices:
9.1.2.2.1 All samples for each individual aqueous matrix will be combined and
homogenized in a pre-cleaned and sealable 30-gal blue HDPE open top
drum with a powered stainless-steel mixer.
9.1.2.2.2 Each aqueous matrix will mix for 1 hr and be stored in a labeled 30-gal blue
HDPE sealable container until the specific aqueous matrices for the study
have been selected by the SERDP/ESTCP team.
9.1.2.2.3 Once the specific aqueous matrices are selected, they will be packaged in
1000 ml_ amber HDPE bottles for the Waste, Surface & Ground waters,
125 ml_ HDPE bottles for the Leachate, while mixing.
9.1.2.2.4 Wastewater, Surface Water & Ground Water bottles will be filled to a
nominal fill of 500 ml_ in a 1000 ml_ amber HDPE bottle and Leachate
bottles will be filled to a nominal fill of 100 ml_ in a 125 ml_ HDPE bottle.
9.1.2.2.5 The labs will be directed in the sample instructions to use the entire
contents of the sample and assume 500 ml_ for Waste, Surface & Ground
waters and 100 ml_ for Leachate Waters.
9.1.2.2.6 The packaging sequence for each lot will be recorded for reference.
9.1.2.2.7 Label each bottle with an adhesive label listing matrix type and lot number,
that is listed in the Appendices section under the Sample Labeling
Scheme.
9.1.2.2.8 Filled bottles will then be stored in a walk-in refrigerator until the spiking
event.
9.1.2.2.9 The steps above will be repeated for each aqueous matrix.
9.1.2.3 Soil/Sediment/Biosolids:
9.1.2.3.1 All sample containers for each Soil, Sediment and Biosolid matrix will be
combined and homogenized in pre-cleaned sealable containers. Sediment
samples containing standing liquid will be decanted prior to homogenizing.
9.1.2.3.2 Each solid matrix in the bulk container will be mixed until thoroughly
homogenized for at least 1 hr in a rotational mixer.
9.1.2.3.3 All soil matrices will be tested for the percent moisture content and
recorded.
9.1.2.3.4 Each soil matrix will be stored in a bulk labeled sealable container until the
specific matrices for the study have been selected by the SERDP/ESTCP
team.
9.1.2.3.5 The labs will be directed in the sample instructions for the soil, sediment
and biosolid matrices to use the entire contents of the sample and rinse
the vial out to remove any PFAS material that may adhere to the vial walls.
The labs will also be directed in the instructions to assume 5.0 g dry
weight basis for soil/sediment samples and 0.5 g dry weight basis for the
biosolids is packaging in the vial. Instructions will also include that
moisture content and moisture correction will not be necessary by the labs.
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THE SCIENCE OF WHAT'S POSSIBLE,"
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 8 of 14
9.1.2.3.6 When the specific matrices are chosen, 5 g dry weight basis ± 0.5 g soil
and sediment sample sizes will be packaged in 24 ml_ clear glass screw
top vials. The dry weight basis sample size is the state of the soil without
the presence of water.
9.1.2.3.7 0.5 g dry weight basis ± 0.05 g sample size for each biosolid matrix will be
packaged in 24 ml_ clear glass screw top vials.
9.1.2.3.8 Percent Moisture Content (MC) and Dry Weight Basis Sample Size
(DWBSS) will be calculated by ERA as follows.
% Moisture Content:
M- D
MC
D
x 100
MC = % Moisture Content
M = Weight of Moist Soil
D = Weight of Dry Soil
Dry Weight Basis Sample Size:
DWBSS
s~
'mc^
Dx
.100„
J
+ D
DWBSS = Dry Weight Sample Size
MC = % Moisture Content
D = Weight of Dry Soil
9.1.2.3.9 The packaging sequence for each lot will be recorded for reference.
9.1.2.3.10 Label each vial with an adhesive label listing matrix type and lot number,
that is listed in the Appendices section under the Sample Labeling
Scheme.
9.1.2.3 11 Filled vials will then be stored in a walk-in refrigerator until spiking and
shipping.
9.1,2.3.12 Steps above will be repeated for each solid matrix.
9.1.2.4 Fish/Clam Tissue:
9.1.2.4.1 Each tissue will be homogenized separately in a pre-cleaned bin.
9.1.2.4.2 Fish tissue including skin and shucked clams will be processed with a food
processer until a smooth paste consistency is achieved. Due to the
amount of the tissue and capacity of the food processor, the tissue may
need to be processed in separate batches and combined in the pre-
cleaned bin.
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Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 9 of 14
9.1.2.4.3 After the paste consistency is achieved each tissue will be mixed until
thoroughly homogenized for at least 1 hr in a pre-cleaned bin. 2 g ± 0.5 g
fish/clam tissue sample size will be packaged in 24 ml_ clear glass screw
top vials.
9.1.2.4.4 The packaging sequence for each lot will be recorded for reference.
9.1.2.4.5 Label each vial with an adhesive label listing matrix type and lot number,
that is listed in the Appendices section under the Sample Labeling
Scheme.
9.1.2.4.6 Filled vials will then be stored in a freezer until spiking and shipping.
9.1.2.4.7 Labs will be directed in the tissue sample instructions to use the entire
contents of the sample and rinse the vial out to remove any PFAS material
that may adhere to the vial walls. The labs will also be directed in the
sample instructions to assume 2.0 g for each tissue sample is packaging
in the vial.
9.1.2.4.8 Steps above will be repeated for each fish/clam tissue matrix.
9.2 Matrix Characteristics Testing:
9.2.1 All aqueous, soil, sediments, and tissue matrices will be sent to Eurofins TestAmerica Denver for
sample chemical characteristics testing.
9.2.2 Reference Sample Chart 2 in section 2.1.1 for a summary of sample requirements for the
chemical characteristic analysis for each matrix. Detailed are the testing parameters, testing
method, packaging container, sample preservative, volume/mass and holding times.
9.2.3 After external characteristic testing is completed, data will be reviewed by the Method Validation
Team and they will determine if any adjustments are needed to any of the sample matrices.
9.2.4 If any adjusting is required, ERA will adjust the determined lot to meet any outstanding criteria.
Adjustments will be analytically verified by ERA using the ERA work procedures listed in section
5.1 of this work procedure.
9.3 PFAS Spiking Concentrate Manufacturing & Verification Process:
9.3.1 ERA will manufacture an estimate of 4 unique mixed PFAS spiking concentrates, depending on
analyte concentrations using gravimetric balances and volumetric glassware traced to NIST
weights following ERA ISO 17025 Accredited Work Instruction 730002350 (Organic Liquid
Standards Preparation).
9.3.2 The 4 mixed spiking concentrates will consist of 2 mixed spiking concentrate solutions for the
aqueous matrices and 2 mixed spiking concentrate solutions for the solid matrices will be used
to manufacture all final products. See "MARTIX SPIKING LEVELS" in Appendices section of this
procedure for spiking levels.
9.3.3 New analyte addition(s) may affect the total number of spiking concentrates and/or the originally
planned concentrations. PFAS analytes, concentrations, and levels will be approved by the
client prior to manufacturing commencement. Depending on background PFAS levels more
spiking concentrates maybe be required.
9.3.4 ERA will analytically verify the 4 PFAS spiking concentrates by LC/MS/MS following ERA ISO
17025 Accredited Work Procedure 730002570 (Semi-volatile Analytical Verification by High
Performance Liquid Chromatography). A minimum of n=5 for each concentration will be verified.
9.3.5 Method development will be performed as needed for any new analyte addition(s).
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y^Q|ers WORK INSTRUCTION
THE science of what's possible.- jjtie: Hydrogeologic PFAS Validation Study Procedure
Document No: 73000PFAS Version No: 13 Page 10 of 14
9.4 Sample PFAS Spiking Process:
9.4.1 Sample Spiking Organization:
9.4.1.1 Sample spiking, freezing and packing timeline will be determined by the
SERDP/ESTCP team and communicated to ERA.
9.4.1.2 Whole volume spiking bench sheets will be created and reviewed prior to shipment.
9.4.1.2.1 Two spiking concentrates will be used to spike all aqueous final whole
volume products at varying levels.
9.4.1.2.2 Two spiking concentrates will be used to spike all solid/tissue final whole
volume products at varying levels.
9.4.1.3 Sample Organization:
9.4.1.3.1 The designated samples for each week will be pulled from
refrigeration/freezer on the day the of the spiking.
9.4.1.3.2 Samples will be organized according to the spiking levels.
9.4 1.3.3 Spiking concentrations will be pulled from refrigeration storage and
allowed to reach ambient temperature prior to spiking samples.
9.4.1.4 Sample Spiking:
9.4.1.4.1 Once samples and spiking concentrates reach room temperature they will
be mixed/vortexed prior to being opened and aliquots withdrawn. They will
be organized on physically separated work benches according to spiking
levels.
9.4 1.4.2 A validated repeating pi petto r delivery system will be used to deliver the
aliquots on to the samples.
9.4.1.4.3 Bench sheets will list the amount of each spiking concentrate to deliver to
the specific sample. Spiking aliquots will be determined upon
determination of final concentrations.
9.4 1.4.4 Detailed records of the spiking events will be recorded and a peer witness
review of samples, spiking concentrates and pipettor will be performed
prior to and during actual spiking event.
9.4.1.4.5 Once the designated aliquot of spiking concentrate has been delivered,
each sample will be sealed and placed in a designated completed area to
avoid double spiking.
9.4.1.4.6 A peer witness review of samples, spiking concentrates and pipettor will
be performed during the actual spiking event and documented.
9.4.1.4.7 Aqueous sample bottles will be inverted to homogenize and stored in the
walk-in freezer until they are scheduled to ship. Soil/Sediments/Biosolids
and fish tissue will be stored in a walk-in refrigerator until they are
scheduled to ship.
9.4.1.4.8 Samples will be spiked in advanced by the Friday prior to the scheduled
shipping week and then ship overnight by Wednesday to give ample time
for samples to freeze.
9.5 Sample Shipping Process:
9.5.1 Order confirmations for shipments will be setup by ERA in consultation with client.
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W0t©rS WORK INSTRUCTION
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Document No: 73000PFAS Version No: 13 Page 11 of 14
9.5.2 Sample shipping will follow the determined schedule by the SERDP/ESTCP team and will be
communicated to ERA.
9.5.3 Frozen Blue Ice Gel packs and packing material will be used with each shipment to chill and
protect samples.
9.5.4 Shipment Preparation:
9.5.4.1 Cooler shipments will be prepared following ERA work instruction 730002425 (Whole
Volume Cooler Shipping). Each order will include the following listed below.
9.5.4.1.1 A set number of coolers will be determined by matrix type.
9.5.4.1.2 The samples that are prescheduled for each shipping event.
9.5.4.1.3 Temperature Blank
9.5.4.1.4 Completed chain of custody form.
9.5.4.1.5 Sample Preparation Instructions
9.5 4.1.6 Blue Gel Ice Packs
9.5.4.1.7 A 4x4 label applied to outside of cooler box stating, "Upon arrival, contact
(LAB POC) immediately."
9.5 4.2 Laboratory contacts and client personnel will be notified by email of shipment and
supplied with shipment tracking numbers.
9.6 Certificate of Analysis and Sample Instruction Generation:
9.6.1 CofA's for each spiked level matrix will be created using ERA ISO 17025 Accredited Work
Instruction 730002412 (Environmental Product Manual Certificate of Analysis Generation).
9.6 2 Sample instructions for each matrix type will generated.
9.6.3 CofA's & Sample instructions content will be discussed and mutually agreed upon with client.
9.6.4 CofA's & Sample instructions will be distributed to personnel designated by the client.
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YYq|0 WORK INSTRUCTION
the science of what's possiBLEr Title: Hydrogeologic PFAS Validation Study Procedure
Document No: 73000PFAS Version No: 13 Page 12 of 14
10 APPENDICES/ATTACHMENTS
SAMPLE LABELING SCHEME
Matrix
Type
Requested
Name
Description
Matrix
Code
Sample
Identifier
Characterization
Sample Lot#
Spiked Study Sample Lot Numbers
Unspiked
Low
Replicate
Low
Replicate
2
Low
Replicate
3
High
Replicate
High
Replicate
2
High
Replicate
3
Ground
Water
USACE
GW#1, Midwest
GW
A
GWA0
GWA1
GWA2
GWA3
GWA4
GWA5
GWA6
GWA7
Ground
Water
LRPCD
GW #2,
Southwest
GW
B
GWB0
GWB1
GWB2
GWB3
GWB4
GWB5
GWB6
GWB7
Ground
Water
USACE
GW#13
GW
C
GWC0
GWC1
GWC2
GWC3
GWC4
GWC5
GWC6
GWC7
Surface
Water
Lake Harsha, OH
SWOH 9/10
SW
D
SWD0
SWD1
SWD2
SWD3
SWD4
SWD5
SWD6
SWD7
Surface
Water
Norwell, MA
SW MA 9/24
SW
E
SWE0
SWE1
SWE2
SWE3
SWE4
SWE5
SWE6
SWE7
Surface
Water
Burley Creek,
WA
Burley Creek
SW
F
SWF0
SWF1
SWF2
SWF3
SWF4
SWF5
SWF6
SWF7
Surface
Water
Sequim Bay, WA
Sequim
Seawater
SW
G
SWG0
SWG1
SWG2
SWG3
SWG4
SWG5
SWG6
SWG7
Waste
Water
Metal Finisher
Metal Finisher
WW
H
WWH0
WWH1
WWH2
WWH3
WWH4
WWH5
WWH6
WWH7
Waste
Water
Hospital
Hospital
WW
I
WWI0
WWI1
WWI2
WWI3
WWI4
WWI5
WWI6
WWI7
Waste
Water
POTW Influent
POTW Influent
WW
J
WWJ0
WWJ1
WWJ2
WWJ3
WWJ4
WWJ5
WWJ6
WWJ7
Waste
Water
ASTM Substitute
ASTM Substitute
WW
K
WWK0
WWK1
WWK2
WWK3
WWK4
WWK5
WWK6
WWK7
Waste
Water
WW Bus
Washinq Station
WW Bus Wash
WW
L
WWL0
WWL1
WWL2
WWL3
WWL4
WWL5
WWL6
WWL7
Waste
Water
Playa Del Ray,
CA
Plant Effluent
WW
M
WWM0
WWM1
WWM2
WWM3
WWM4
WWM5
WWM6
WWM7
Waste
Water
P&P WW
#1-28
WW
N
WWN0
WWN1
WWN2
WWN3
WWN4
WWN5
WWN6
WWN7
Waste
Water
POTW Effluent
POTW Effluent
WW
O
WWOO
WW01
WW02
WW03
WW04
WW05
WW06
WW07
Waste
Water1
Dairy
Wastewater1
Dairy
Wastewater
WW
P
WWP01
WWP1
WWP2
WWP3
WWP4
WWP5
WWP6
WWP7
Soil
Musselshell,
Clark Co. MT
AA (2016-106),
L32547-2
ss
R
SSR0
SSR1
SSR2
SSR3
SSR4
SSR5
SSR6
SSR7
Soil
Ivy, Cashe Co.
UT
BB (2017-111),
L32547-3
ss
S
SSSO
SSS1
SSS2
SSS3
SSS4
SSS5
SSS6
SSS7
Soil
Fruitland, San
Juan Co. NM
CC (2018-105),
L32547-4
ss
T
SST0
SST1
SST2
SST3
SST4
SST5
SST6
SST7
Soil
Armijo, Dona
Ana Co. NM
DD (2018-116),
L32547-5
ss
U
SSUO
SSU1
SSU2
SSU3
SSU4
SSU5
SSU6
SSU7
Soil
Drummer,
Dekalb Co. IL
EE (2019-107),
L32547-6
ss
V
ssvo
SSV1
SSV2
SSV3
SSV4
SSV5
SSV6
SSV7
Soil
Brock, Wheatley
Co. TN
FF (2019-110),
L32547-7
ss
w
sswo
SSW1
SSW2
SSW3
SSW4
SSW5
SSW6
SSW7
Soil
Delhi, Fresno
County. CA
2014-107
ss
X
ssxo
SSX1
SSX2
SSX3
SSX4
SSX5
SSX6
SSX7
Sediment
Burley 1 Sed.
Burley Creek,
WA
Burley 1 Sed.
SD
Y
SDY0
SDY1
SDY2
SDY3
SDY4
SDY5
SDY6
SDY7
Sediment
Burley 2 Sed.
Burley Creek,
WA
Burley 2 Sed.
SD
z
SDZ0
SDZ1
SDZ2
SDZ3
SDZ4
SDZ5
SDZ6
SDZ7
Sediment
Sequim Bay
Sediment
Sequim Bay
Sediment
SD
AA
SDAA0
SDAA1
SDAA2
SDAA3
SDAA4
SDAA5
SDAA6
SDAA7
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YYq|0 WORK INSTRUCTION
the science of what's possiBLEr Title: Hydrogeologic PFAS Validation Study Procedure
Document No: 73000PFAS Version No: 13 Page 13 of 14
Fish
Tissue
Walleye (low lipid
fish)
Walleye
TS
AB
TSABO
TSAB1
TSAB2
TSAB3
TSAB4
TSAB5
TSAB6
TSAB7
Fish
Tissue
Salmon (high
lipid fish)
Salmon
TS
AC
TSACO
TSAC1
TSAC2
TSAC3
TSAC4
TSAC5
TSAC6
TSAC7
Fish
Tissue
Clams
Clams
TS
AD
TSADO
TSAD1
TSAD2
TSAD3
TSAD4
TSAD5
TSAD6
TSAD7
Leachate
MSWLF
Leachate
Sample
MSWLF
Leachate
Sample
LC
AE
LCAEO
LCAE1
LCAE2
LCAE3
LCAE4
LCAE5
LCAE6
LCAE7
Leachate
CDD Landfill
CDD
LC
AF
LCAFO
LCAF1
LCAF2
LCAF3
LCAF4
LCAF5
LCAF6
LCAF7
Leachate
Ash leachate
Ash leachate
LC
AG
LCAGO
LCAG1
LCAG2
LCAG3
LCAG4
LCAG5
LCAG6
LCAG7
Biosolids
Playa Del Ray,
CA
Wetcake
BS
AH
BSAHO
BSAH1
BSAH2
BSAH3
BSAH4
BSAH5
BSAH6
BSAH7
Biosolids
Biosolids #1 East
Biosolids #1
East
BS
Al
BSAI0
BSAI1
BSAI2
BSAI3
BSAI4
BSAI5
BSAI6
BSAI7
Biosolids
South Plant
Biosolids
South Plant
Biosolids
BS
AJ
BSAJO
BSAJ1
BSAJ2
BSAJ3
BSAJ4
BSAJ5
BSAJ6
BSAJ7
1 Dairy Wastewater determined to not be fit for the study and will not be used.
Matrices highlighted in yellow above are to be excluded from MLV study.
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THE SCIENCE OF WHAT'S POSSIBLE."
Document No: 73000PFAS
WORK INSTRUCTION
Title: Hydrogeologic PFAS Validation Study Procedure
Version No: 13 Page 14 of 14
MATRIX SPIKING LEVELS
Wastewater, Ground Waterand Surface Water
Leac hates
Soils, Sediments, Biosolidsand Tissues
Low Spike1
High Spike1
Low Spike1
High Spike1
High Spike1
PFAS Compound
(ng/L)
(ng/L)
(ng/L)
(ng/L)
Low Spike1 (ng/Kg)
(ng/Kg)
PFBA
80
400
PFPEA
40
200
PFHXA
20
100
PFHPA
20
100
PFOA
20
100
PFNA
20
100
PFDA
20
100
PFUNA
20
100
PFDOA
20
100
PFTRDA
20
100
PFTEDA
20
100
PFBS
20
100
PFPES
20
100
PFHXS
20
100
PFHPS
20
100
PFOS
20
100
PFNS
20
100
PFDS
20
100
PFDOS
20
100
4:2 FTS
80
240
6:2 FTS
80
240
8:2FTS
80
240
PFOSA
20
100
NMeFOSA
20
100
NEtFOSA
20
100
NMeFOSAA
20
100
NEtFOSAA
20
100
NMeFOSE
160
400
NEtFOSE
160
400
HFPO-DA
80
240
ADONA
80
240
9CL-PF30NS
80
240
11CL-PF30UDS
80
240
3:3FTCA
80
400
5:3FTCA
120
2000
7:3FTCA
120
2000
PFEESA
40
200
PFMPA
40
200
PFMBA
40
200
NFDHA
40
200
All spike concentrations are presented as acid concentrations; not salts
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PFAS Method Validation Study:
Wastewater Sample Preparation Guidelines
Shipment Contents
(4) 25"xl5.5"xl7" Styrofoam box coolers
(7) Wastewaters Lots
(49) 1L amber HDPE bottles
Temperature blank
Sample Preparation Guidelines
Sample Chain of Custody (COC)
Sample Description
Samples are packaged in a 1L amber HDPE bottle containing approximately 500 mL of spiked sample.
Samples will be received at < 6°C.
Samples are not preserved.
Samples must be stored immediately at <-20°C until sample preparation.
Each sample will contain the PFAS analytes as defined in "MLV Study Method Analysis of Per- and
Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS",
October 2021.
Before You Begin
• Prior to preparation, samples should be allowed to equilibrate to room temperature and then analyzed as
soon as possible.
Sample Instructions
1. The sample preparation procedure found in the MLV Study Method is to be followed, with one exception.
Do not measure the volume of the container as required by Section 11.2.2 of the MLV Study Method.
Instead, record 500 mL as the volume of sample prepared. This is the volume to be used when calculating
PFAS concentrations in each sample. The container is to be rinsed as required by the MLV Study Method."
2. Report your results as ng/L and report the sample lot number that is provided on the sample container
and on the COC, without any modifications, as the Sample Number (Sample NO. on the EDD).
Page 1 of 1
Version: 04
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PFAS Method Validation Study:
Surface & Ground Water Sample Preparation Guidelines
Shipment Contents
(4) 25"xl5.5"xl7" Styrofoam box coolers
(3) Surface Waters Lots
(3) Ground Water Lots
(42) 1L amber HDPE bottles
Temperature blank
Sample Preparation Guidelines
Sample Chain of Custody (COC)
Sample Description
Samples are packaged in a 1L amber HDPE bottle containing approximately 500 mL of spiked sample.
Samples will be received at < 6°C.
Samples are not preserved.
Samples must be stored immediately at <-20°C until sample preparation.
Each sample will contain the PFAS analytes as defined in "MLV Study Method Analysis of Per- and
Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS",
October 2021.
Before You Begin
• Prior to preparation, samples should be allowed to equilibrate to room temperature and then analyzed as
soon as possible.
Sample Instructions
The sample preparation procedure found in the MLV Study Method is to be followed, with one exception.
Do not measure the volume of the container as required by Section 11.2.2 of the MLV Study Method.
Instead, record 500 mL as the volume of sample prepared. This is the volume to be used when calculating
PFAS concentrations in each sample. The container is to be rinsed as required by the MLV Study Method."
Report your results as ng/L and report the sample lot number that is provided on the sample container
and on the COC, without any modifications, as the Sample Number (Sample NO. on the EDD).
Page 1 of 1
Version: 01
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PFAS Multi-Laboratory Validation Study Report
Aqueous Media: Wastewater, Surface Water, and Groundwater
SERDP
Appendix C
Data Management Report
(Exa Data and Mapping
Services Inc.)
Date: July 25, 2023
-------
Data Management Summary Report
for the
Multi-Laboratory Validation Draft EPA Method 1633 - PFAS in Aqueous, Solid, Biosolids,
and Tissue Samples by LC-MS/MS
DRAFT
Prepared for:
SERDP/ESTCP PFAS Method Validation Study Team
Strategic Environmental Research and Development Program (SERDP)
4800 Mark Center Drive, Suite 16F16
Alexandria, VA 22350-3605
Prepared by:
Exa Data & Mapping Services, Inc.
19530 23rd Ave NE
Poulsbo, WA 98370
And
HydroGeoLogic, Inc.
11107 Sunset Hills Road, Suite 400
Reston, Virginia 20190-5375
July 19, 2023
-------
TABLE OF CONTENTS
LIST OF TABLES ii
LIST OF FIGURES ii
LIST OF APPENDICES ii
LIST OF ACRONYMS AND ABBREVIATIONS iii
1.0 INTRODUCTION 1
1.1 Background 1
1.2 Phase s of Data Management 2
1.3 Data Management System Objectives 3
2.0 ROLES AND RESPONSIBILITIES 4
3.0 DATA SHARING PLAN AND FILE TRACKING 6
3.1 ExaBlue SharePoint: Host and Software 6
3.1.1 Folder Structure 8
3.1.2 Access and Permissions 13
3.2 File Tracking System 14
3.2.1 Exa Internal Tracking 15
3.2.2 MLVReview Status 16
3.2.3 EPA NA VSEA Review Tracker 18
3.3 File-Naming Protocols 18
4.0 DATA MANAGEMENT PROCESSES AND PROCEDURES 19
4.1 Workflow 19
4.1.1 Receipt of Data Sets 19
4.1.2 Review Laboratory Data Package/EDD Submissions 22
4.1.4 Statistical Analyses 23
4.1.5 Data Archiving 24
4.1.6 Rejection and Resubmission Process 25
4.2 EDD QA/QC Procedures 26
4.2.1 QA/QC Checks at Import 26
4.2.2 Detailed EDD QA/QC and Reporting 28
4.2.3 Final Processing Steps 34
4.3 Database and Tools 36
4.3.1 Database Structure 36
4.3.2 Populating Final Result and Final Qualifier 39
4.3.3 QA/QC Checks on Master EDD Database 39
4.3.4 Matrix Spike Percent Recovery Calculation Procedures 40
4.3.5 Import and Export File Structures 40
5.0 REFERENCES 42
i
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LIST OF TABLES
Table 1. MLV Study Data Management Team Member Roles and Responsibilities
Table 2. MLV Study General Data Types
Table 3. Project Participants with Access to the ExaBlue SharePoint
Table 4. Example Review Status Table
Table 5. Laboratory Data File-Naming Protocol Examples
Table 6. List of Required Fields
Table 7. Detailed List of EDD QA/QC Checks
Table 8. Fields with Range Checks
Table 9. Allowed Code Combinations for Sample No, Matrix, and SampleType fields
Table 10. Additional Fields Included in the Amended EDD
Table 11. Data Rules for Calculating Percent Matrix Spike Recoveries
LIST OF FIGURES
Figure 1. Organization of the Multi-Laboratory Validation Study Teams Relative to their Roles
in Managing Data
Figure 2. Folder Structure for the ExaBlue SharePoint
Figure 3a. Workflow for the PFAS Multi-Lab oratory Validation Study
Figure 3b. Workflow for the PFAS Multi-Lab oratory Validation Study (continued)
Figure 4. Opening Form of the MLV Study EDD QA/QC Tool
Figure 5. EDD Checking Routines and Reporting Form
Figure 6. QA/QC Report and Detailed QA/QC Queries Form
Figure 7. Append to Master EDD Database and Generate Amended EDD Form
Figure 8. Entity-Relationship Diagram (ERD) for the Project Database
LIST OF APPENDICES
Appendix A - Description of the File Tracking System
Appendix B - File Tracking System Valid Values
Appendix C - Project Database - Database Dictionary
Appendix D - Supplemental Guidance for Correctly Populating the EDD Template
Appendix E - Project Database - Valid Value Codes and Descriptions
Appendix F - Project Database - Valid Value Codes and Descriptions for Compounds
ii
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LIST OF ACRONYMS AND ABBREVIATIONS
AFFF Aqueous Film-Forming Foams
ASTM American Society for Testing and Materials
DoD US Department of Defense
DFARS Defense Federal Acquisition Regulations Supplement
DMP Data Management Plan
DP Data Package
DVR Data Validation Report
GDIT General Dynamics Information Technology
EDD electronic data deliverable
EIS extracted internal standard
EPA US Environmental Protection Agency
ESTCP Environmental Security Technology Certification Program
GCC Government Community Cloud
HGL HydroGeoLogic, Inc.
IDA Institute for Defense Analysis
IDC initial demonstrations of capability
IPR initial precision and recovery
ITAR International Traffic in Arms Regulations
LC-MS/MS Liquid Chromatography/Tandem Mass Spectrometry
MLV Multi-Laboratory Validation
MVS Team Method Validation Study Team
NAVSEA Naval Sea Systems Command
NIS Non-extracted internal standard
PFAS per- and polyfluoroalkyl substances
QA quality assurance
QC quality control
SDG sample delivery group
SEE Science and Engineering for the Environment
SERDP Strategic Environmental Research and Development Program
SLV Single-Laboratory Validation
SOP Standard Operating Procedures
US ACE US Army Corps of Engineers
VBA Visual Basic for Applications
-------
1.0 INTRODUCTION
This document describes data management processes and procedures for the Multi-Laboratory
Validation of Draft EPA Method 1633 - PFAS in Aqueous, Solid, Biosolids, and Tissue Samples
by LC-MS/MS. EPA Method 1633 is an interim draft method for analyzing per- and
polyfluoroalkyl substances (PFAS), and now requires a Multiple-Laboratory Validation (MLV)
Study. A Data Management Plan (DMP; SERDP/ESCTP 2023, Attachment 4) was generated at
the outset of the project to describe the design of the data management system which outlined the
processes and procedures intended to be used for the transmission, tracking, verification, review,
storage, and delivery of laboratory data and associated validation and analyses data collected in
support of the MLV Study. During the course of the project, the intended design of certain elements
of the data management system were adjusted; the processes and procedures actually used during
the project are documented in this report.
To meet study requirements for the acquisition of technically sound and legally admissible data, a
traceable audit trail was established from the shipment of sample matrices to each participating
laboratory through the archiving of information and data. Each step was conducted in accordance
with the MLV Study Work Plan (SERDP/ESTCP 2023). All potential variations in the analytical
and reporting process were documented and retained with other laboratory data and digital
information generated during the MLV Study.
1.1 Background
The MLV Study was conducted by the US Department of Defense's (DoD) Strategic
Environmental Research and Development Program (SERDP) in cooperation with the US
Environmental Protection Agency (EPA), the US Navy (Navy), the US Air Force (Air Force), and
the US Army Corps of Engineers (USACE). Members from each of these agencies comprise the
advisory Method Validation Study (MVS) Team. The study is being conducted as SERDP Project
ER19-1409. The end goal of the MLV Study is to use the findings to revise, as necessary, draft
Method 1633, and to submit the supporting data packages to the EPA Office of Water for
consideration as a final method under the Clean Water Act.
As part of the method validation, the MVS Team worked with Federal, municipal, state, and
regional contacts to obtain sufficient volumes/masses of samples from eight different
environmental matrices, including wastewater, landfill leachate, groundwater, surface water, fish
tissue/clams, biosolids, sediment, and soil. Sample matrices were collected and transferred under
chain of custody between September and December 2020. A replacement biosolids sample was
collected in October 2021 and an ASTM substitute wastewater sample was developed in December
2021.
1
-------
Specific steps of the MLV Study are to (a) develop the analytical method, (b) conduct single and
multi-laboratory validation studies, and (c) perform statistical analyses of the resultant analytical
data to develop appropriate Quality Assurance (QA) and Quality Control (QC) criteria for the
method. The draft EPA Office of Water Method 1633 for PFAS has been demonstrated in the
Single-Laboratory Validation (SLV) Study conducted under ER19-1409 (Willey etal. 2021). The
Method was evaluated and determined to be sufficiently robust to proceed to the Multi-Lab oratory
Validation Study. AFinalEPA Office ofWater Method 1633 for PFAS is critical to DoD Remedial
Project Managers working at aqueous film-forming foams (AFFF)-impacted sites. The method is
also of critical importance nationally to wastewater permit writers, ecological and human health
risk assessments.
1.2 Phases of Data Management
The data management processes and procedures described herein are applicable to Phases 3-6 of
the MLV Study Work Plan (SERDP/ESTCP 2023). The six phases of the plan include:
• Phase 1 - Soliciting Laboratories: This phase involved soliciting proposals and awarding
subcontracts to laboratories and suppliers to participate in the Study.
• Phase 2 - Procuring Standards and Study Samples: This phase involved procuring the
standards, acquiring and characterizing sample media, and creating the Study Samples.
• Phase 3 - Calibration and Demonstration of Capability: involves using the Study Method
(SERDP/ESTCP 2023, Attachment 1), which includes MLV Study-specific requirements
and guidance to (1) perform the initial steps (calibration, initial demonstrations of
capability [IDCs], initial precision and recovery [IPR], MDLs, and verify limits of
quantitation [LOQs]), (2) demonstrate laboratory capability with standards and clean
matrices, and (3) generate an applicable standard operating procedure (SOP).
Data/information for this phase includes laboratory-specific SOPs, calibration data, and
results from the IDC as well as records related to document reviews, corrections, and
approvals.
• Phase 4 - Analyses of Study Samples: This phase involves all participant laboratories using
the Study Method to analyze the Study Samples. Data/information for this phase includes
laboratory-specific data for each Study Sample (electronic data deliverables [EDDs] and
Data Packages).
• Phase 5.1- Data Verification: This phase involves data verification of all study results by
the HydroGeoLogic (HGL) Project Chemist and automated checks of the EDDs by Exa.
HGL's Project Chemist performed an initial evaluation of the data from each phase of the
study with the MVS Team before authorization is given to proceed with the next phase of
the study. Data/information for this phase includes the data package completeness review
checklist and EDD Error Summary reports.
2
-------
• Phase 5.2 - Data Validation: An independent third-party conducted data validation for all
study results. Data/information for this phase includes data reviews, updated/corrected
EDDs and Data Packages, correspondence related to corrections, and approvals.
• Phase 6 - Development of QC Acceptance Criteria: Data/information for this phase
includes results from the statistical analysis of data from the MLV Study, quality control
(QC) acceptance criteria, recommendations for revisions to draft Method 1633, and a MLV
Study Report submitted to the EPA.
1.3 Data Management System Objectives
The primary objective of the data management system (DMS) is to provide an efficient and
organized method of data management to streamline data flow and ensure the highest quality data
are compiled. Specific objectives are:
• To facilitate and coordinate with the MVS Team members to ensure that the data
management system meets overall project objectives;
• To ensure high quality data that provides an accurate representation of all data produced
during the study;
• To standardize and store the data in a structured format to allow for accurate querying
and statistical analyses;
• To ensure efficient and timely data processing;
• To store the data produced during the MLV Study in a secure location that restricts
access to team members with appropriate credentials;
• To allow easy access to the data by project stakeholders; and,
• To implement documentation procedures that ensure the data is technically defensible
and legally admissible.
The data management methodology is critical to ensure that laboratory analytical data, validation
information, and final statistical calculations are of the highest quality to support and defend the
publication of the final method.
3
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2.0 ROLES AND RESPONSIBILITIES
Under the leadership and guidance of the MVS Team, the Data Management Team developed the
data management system and ensured that the project objectives and scope were achieved. The
Data Management Team consists of Exa Data & Management, Inc. (Exa) and HydroGeoLogic,
Inc. (HGL; Figure 1). The Data Management Team coordinated with the MVS Team and data
providers, including the analytical laboratories, the validator team, and the statistics and analysis
team (Institute for Defense Analysis [IDA]). HGL was responsible for managing the laboratories
and reviewing the data packages submitted by the laboratories to ensure contractual compliance
and coordinating communication between data validators and laboratories. Exa was responsible
for maintaining the project database, reviewing EDDs submitted by the laboratories, and assisting
with coordinating the multi-level review process (described in Section 4.0).
Method
Validation Study
Team
1
Data Management
Team
Legend
—~ Primary communication
Ancillary communication
Figure 1. Organization of the Multi-Laboratory Validation Study Teams Relative to their
Roles in Managing Data
Specific roles of individual team members are provided in Table 1. Ms. Dawn Smorong, Exa's
Project/Database Manager, has overall responsibility for ensuring the data are managed in
accordance with the approved MLV Study Work Plan (SERDP/ESTCP 2023) and other related
documents. Other Exa team roles include that of Ms. Peggy Myre, who served an oversight role to
-------
ensure that project data management goals and target schedule milestones were met. Dr. Michael
Tweiten of Exa had primary responsibility for management of the centralized file sharing system
discussed in Section 3.0. Mr. Glenn Sutula assisted with data management processes.
The HGL data management role will be to coordinate incoming data from the laboratories, and to
perform initial checks of data acceptability as described in Section 4.1.2.
Table 1. MLV Study Data Management
Team Member Roles and Responsibilities
Organization
Team Member
Role
Data Management
Responsibility
Exa Data & Mapping
Dawn Smorong
Exa PM; Data
Manager
Exa project completion and
database management
Peggy Myre
Exa Data
Quality Officer
Ensure compliance with
project goals and the DMP
Michael Tweiten
Exa Data
Library Manager
Setup and manage MLV
Study Library storage and
users
Glenn Sutula
Data Manager
Database management
HvdroGco Logic
Joe Skibinski
HGL Project
Manager
HGL project completion, lab
coordination
John Powell
HGL Program
Chemist
Laboratory coordination,
chemistrv review
Denise Rivers
HGL Project
Chemist
Laboratory coordination,
laboratory data compliance,
chemistry review
Ken Rapuano
HGL Project
Chemist
Laboratory data compliance,
chemistry review
Joe Vilain
HGL Project
Chemist
Laboratory data compliance,
chemistry review
Andrea Fletcher
HGL Data
Manager
Laboratory EDD and data
package tracking and
coordination
5
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3.0
DATA SHARING PLAN AND FILE TRACKING
A critical element to ensure proper organization of the data collected for the MLV Study is
managing the files generated to support the project. A file storage server was deployed to serve as
a repository for all documents and data for the project, termed the ExaBlue SharePoint (Section
3.1). As part of the file organization strategy, a File Tracking System was developed (Section 3.2),
including strict rules for file-naming (Section 3.3).
3.1 ExaBlue SharePoint: Host and Software
All project data and information were stored on a centralized, secure server managed by the Exa
team. Table 2 provides a listing of the general data types stored on the server, as well as the MVS
Team member responsible for upload and maintenance of the associated files.
Access is strictly controlled to ensure the protection of all proprietary data. The selected platform
was Microsoft® (MS) Office 365 Enterprise software; the SharePoint application was used for the
central storage and accessing of documents, data, and other information related to the MLV Study.
This section details server specifications, the folder structure, as well as the list of users and their
access level (permissions).
The ExaBlue SharePoint is hosted on the Microsoft Azure Government Community Cloud (GCC)
High and DoD environments to ensure cloud-service compliance, including Federal Risk and
Authorization Management Program (FedRAMP) High, Department of Defense Security
Requirements Guidelines, Defense Federal Acquisition Regulations Supplement (DFARS), and
International Traffic in Arms Regulations (ITAR). The ExaBlue SharePoint utilizes a Microsoft
Office 365 El Enterprise environment, including Microsoft Office 365 software tools to enable
file sharing, editing, team communications and identity/access management.
The ExaBlue SharePoint employs access restrictions with requirements for authentication and user
credentials to gain access. Exa's Michael Tweiten was responsible for setting up the system,
assigning users and user privileges based on assigned project roles and responsibilities, and making
required adjustments as the project progressed. The laboratory and data validator participants are
only allowed to upload/view their own data. Additional details regarding users and defined
privileges are provided in Section 3.1.2.
The ExaBlue SharePoint was set up to automatically send email notifications to Team members
when files were posted in certain folders.
6
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Table 2. MLV Study General Data Types
Team Member
Data Type
Example Data
Responsible for
I Jnlo ad/M ainte nance
Project Documents
Background Documents - UFP-QAPP and
HGL/Exa
PMP, Study Work Plan, Background
Analytical Data (SGS AXYS), conventional
analyses
Correspondence
All
Final DVR and Data - final versions of the
Exa
laboratory data package, HGL data package
review checklist, data validation reports,
validated EDDs, EPA/NAVSEA review
documents.
Meetings and Schedules - Schedule, Contact
HGL, SEE
list, Meeting Minutes
Project Reports
Working and final versions of reports
MVS Team
(generated for the MLV Study: Aqueous.
i Biosolids/Lnndfill Leacliate. Soil/Sediment.
i Tissue
Laboratory Data
EDDs (csv)
Individual labs
Data packages (pdf)
Individual labs
Sample receipts - Sample acknowledgment
HGL
forms, chain-of-custody records
Standard Operating Procedures (SOP)
Individual labs
Corrective action reports
HGL
ERA laboratory instructions
HGL
Spike Levels and Wellington Certificates of
HGL
Analysis
Data package completenes review checklists
HGL
Validator Data
To validator:
i Amended EDDs (xlsx). Lab Data Packages
Exa/HGL
(pdf)
\From validator:
1 DV Report (pdf)
Individual valid;)tors
Amended EDDs with valid;)lor fields
Individual validators
populated (xlsx)
Evidence of 10% verification (xlsx)
Individual validators
Data validation checklist (doc)
Individual validators
Statistics Data
To IDA:
Database exports (xlsx)
Exa
From IDA:
Report with appendices (pdf) and supporting
IDA
calculations (xlsx)
Database
Database (accdb). documentation (pdf)
Exa
Tracking
MLVS Review Status (xlsx); Exa internal
Exa/SEE/NAVSEA
tracking (xlsx); EPA/NAVSEA Review
Tracker (xlsx)
7
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3.1.1 Folder Structure
The ExaBlue SharePoint employs a strict, hierarchical folder structure, and displays a list of files
and key information about the files, such as who was the last person to modify the file. The folder
and sub-folder structure supported access permissions as described in Section 3.1.2. The top-level
folders indicate the type of data and other content available in the folder (Figure 2).
8
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Appendix A - Description of the File Tracking System
TRACKING
WORKSHEET
TRACKING FIELD
W Field
TRACKING FIELD DESCRIPTION
GENERAL
Tracking ID
Root file name
Project Phase
Project Phase. See 'ValidValues'
EDD File Name
EDD File name
Data Package File Name
Data Package File Name
Laboratory Name
Yes
Laboratory Name. See 'ValidValues'
Matrix
Yes
Matrix. See 'ValidValues'
Notes
Notes regarding submitted files
Log Date
Date the reciept of files was logged into the Tracking System
LABORATORY
EDD/DP Due Date
Due date for the Lab EDD/Data Package (mm/dd/yyyy)
EDD/DP Date Received
Date Lab EDD/Data Package received (mm/dd/yyyy; uploaded to
Sharepoint)
HGL Reviewer
Initials of HGL staff conducting the Data Package review
Date HGL Review Complete
Date HGL review complete (mm/dd/yyyy)
EDD Rejected or Approved -
HGL
Yes
Indicate whether EDD/Data Package was rejected by HGL. See
'ValidValues'
Summary of Errors - HGL
Brief summary of issues found during HGL Data Package review
Exa Reviewer
Initials of Exa staff conducting the automated EDD review
Date Exa Review Complete
Date Exa review complete (mm/dd/yyyy)
EDD Rejected or Approved - Exa
Yes
Indicate whether EDD/Data Package was rejected by Exa. See
'ValidValues'
Summary of Errors - Exa
Brief summary of issues found during Exa EDD review
Date Data Package to DV
Date the Data Package was posted to the Validator folder
(mm/dd/yyyy).
Date Amended EDD to DV
Date the Amended EDD was posted to the Validator folder
(mm/dd/yyyy).
VALIDATOR
Data Validator
Yes
Data Validator. See 'ValidValues'.
DP version reviewed
Current version number of the Data Package provided to the data
validator for review.
Amended EDD version reviewed
Current version number of the Amended EDD provided to the data
validator for review.
Date DV Report/Files Received
Date of receipt for the current data validator report/files (mm/dd/yyyy).
DV Amended EDD version
Current version number of the Amended EDD with validator fields
populated (posted by the data validator).
DV Report version
Current version number of the data validator report (posted by the data
validator).
DV Verification version
Current version number of the Verification file (posted by the data
validator).
DV Checklist version
Current version number of the Checklist (posted by the data validator).
EDD Rejected or Approved - DV
Yes
Indicate whether EDD/Data Package was rejected by the Data Validator.
See 'ValidValues'
Notes
Notes regarding submitted files
Date EPA/NAVY Files Received
Date of receipt for the current review files posted by EPA/NAVY
reviewers (mm/dd/yyyy).
Acronyms: DB - Project Database
DP - Data Package
DV - Data Validator
EDD - Electronic Data Deliverable
27
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Appendix B - File Tracking System Valid Values List
WorksluTl
Held
Y;ili(l Y.due
('ode
\';ili(l Y;due ( ode Description
GENERAL
Laboratory Name
AI.l'IIA
Alpha Analytical
GENERAL
Laboratory Name
BATTELLE
Battelle
GENERAL
Laboratory Name
CALEPA
CalEPA DTSC
GENERAL
Laboratory Name
ELLET
Eurofins Lancaster Labs
GENERAL
Laboratory Name
ETA
ETA, Sacramento
GENERAL
Laboratory Name
GEL
GEL Laboratories
GENERAL
Laboratory Name
MDH
Maryland Department of Health
GENERAL
Laboratory Name
PACE
GCAL/Pace
GENERAL
Laboratory Name
SGSNA
SGS North America
GENERAL
Laboratory Name
VISTA
Vista Analytical
GENERAL
Matrix
GW
Groundwater
GENERAL
Matrix
SW
Surface water
GENERAL
Matrix
SD
Sediment
GENERAL
Matrix
ss
Soil
GENERAL
Matrix
TS
Tissue
GENERAL
Matrix
WW
Wastewater
GENERAL
Matrix
LC
Landfill Leachate
GENERAL
Matrix
BS
Biosolids
GENERAL
Project Phase
Phase 3 - ICAL
Initial Calibration
GENERAL
Project Phase
Phase 3 - IDC
Initial Demonstration of Capabilities (IDC)
GENERAL
Project Phase
Phase 4.4.1
GW, SW, and WW matrices
GENERAL
Project Phase
Phase 4.4.2
SS and SD matrices
GENERAL
Project Phase
Phase 4.4.3
Tissue matrices
GENERAL
Project Phase
Phase 4.4.4
LC and BS matrices
LABORATORY
EDD Rejected or Approved - HGL
Approved
Passed review
LABORATORY
EDD Rejected or Approved - HGL
Rejected
Did not pass review
LABORATORY
EDD Rejected or Approved - HGL
NA
Not applicable (not reviewed)
LABORATORY
EDD Rejected or Approved - HGL
To Validator
Bypassed review and went straight to validator.
LABORATORY
EDD Rejected or Approved - HGL
Re-submitting
Re-submission from the lab expected
LABORATORY
EDD Rejected or Approved - HGL
Pending
Lab has submitted a data package and it's
pending review
LABORATORY
EDD Rejected or Approved - HGL
Not Submitted
Lab hasn't submitted
LABORATORY
EDD Rejected or Approved - Exa
Approved
Passed review
LABORATORY
EDD Rejected or Approved - Exa
Rejected
Did not pass review
LABORATORY
EDD Rejected or Approved - Exa
NA
Not applicable (not reviewed)
LABORATORY
EDD Rejected or Approved - Exa
Re-submitting
Re-submission from the lab expected
LABORATORY
EDD Rejected or Approved - Exa
Pending
Lab has submitted an EDD and it's pending
review
LABORATORY
EDD Rejected or Approved - Exa
Not submitted
Lab hasn't submitted
VALIDATOR
Data Validator
CHEMVAL
ChemVal
VALIDATOR
Data Validator
PYRON
Pyron Environmental
VALIDATOR
Data Validator
JACOBS
Jacobs Engineering
VALIDATOR
EDD Rejected or Approved - DV
Approved
Approved as is (no DV input)
VALIDATOR
EDD Rejected or Approved - DV
Revised
Approved with DV input added
VALIDATOR
EDD Rejected or Approved - DV
Rejected
Did not pass review
VALIDATOR
EDD Rejected or Approved - DV
NA
Not applicable (not reviewed)
28
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Appendix C - Project Database - Database Dictionary
1 :i lilt-
Data l\lu-
Definition anil ( 'ommeiit>>
Di nil
Innii
I.DI)
\ aliil
Value
Iit-Id
Uci|iiiml
ll.ld
Default
\ .iliit-
I'liina n
Ur\
Inclihli- in
Amended
I I)|) lor
HHNI
Ini'luile in
|-'.\porl* lor
IDA
Lab
EDD
Results
TrackingID
text
Tracking ID from Tracking System; incorporated during ETL
procedures
No
No
Yes
X
Yes
No
Lab
EDD
Results
Lab ID Reported
text
LAB ID reported by the laboratories in the EDD
Yes
No
Yes
No
No
Lab
EDD
Results
I.AIS ID
text
^Laboratory Name. See Valid Value list.
No ]
Yes
Yes
X
Yes
No
Lab
EDD
Results
lab num
number
Lab ID code, to keep laboratories anonymous. See Valid Value list.
No |
Yes
Yes
No
Yes
Lab
EDD
Results
:sdg num
text
SDG number; incorporated during ETL procedures; extracted from
Lab Sample ID
No
No
No
Yes
Yes
Lab
EDD
Results
SAMPLENO
text
For samples, these are the sample identification names (IDs) from the
Chain of Custody. The Sample No is the same, regardless of whether
or not the sample is diluted or reanalyzed. For preparation batch QC,
these are "MB" for the Method Blank, "OPR" for the OPR, and
"LLOPR" for the LLOPR. For IDOC samples, "IPR" for the IPR
samples, "MDLB" for the MDLb samples "MDLS" for the MDLs
samples, and "LOQVER" for the LOQVER samples.
Yes
No
Yes
X
Yes
Yes
Lab
EDD
Results
[LAB S AMPLE ID
text
The ID the laboratory assigns to the sample (which identifies the
sample on the associated data files and reports).
IFor samples that need to be re-analyzed for issues other than dilution,
; attach the following identifiers to the end of the lab sample identifier
^without a space between them (e.g., 02082022-01R):
;"R" for analytes, EISs & NISs reported from first re-analysis not due to
! dilution
;"R1" for analytes, EISs & NISs reported from second re-analysis not
:due to dilution
;"R2" for analytes, EISs & NISs reported from second re-analysis not
Idue to dilution
;If more re-analyses not due to dilution are needed to be reported
:beyond three for a sample, continue on with the numbering (e.g., R3,
R l. R5. etc.).
Yes
No
f Yes
X
Yes
Yes
Lab
EDD
Results
ANALYSISDATE
short date;
; mm/dd/yyyy
[Use format mm/dd/yyyy (e.g. 11/20/2019) - do not include time stamp.
Yes
No
Yes
Yes
No
Lab
EDD
Results
ANALYSIS
text
Fill in "PFAS". See Valid Value list.
Yes
Yes
Yes
PFAS
Yes
No
Lab
EDD
Results
PFAS_ ACRONYM
text
Use acronyms included in the example EDD. See Valid Value list.
Yes
Yes
Yes
X
Yes
Yes
Lab
EDD
Results
lab rep
text
l ab replicate identifier
" No j
No
Yes
1
Yes
Yes
15
-------
Appendix C - Project Database - Database Dictionary
1 :i lilt-
Data l\lu-
Definition anil ( 'oniuicut>>
Di nil
hum
I.DI)
\ aliil
Value
Iit-Id
Uci|iiiml Default
Ill-Id Value
I'liina n
Ur\
Include ill
Amended
COD for
Include in
|-'.\porl* lor
IDA
Lab
EDD
Results
DILUTION
number
Dilution made post extraction (e.g., extract diluted 1:10 is entered as
"10"). If analyzed without dilution, enter "1".
Yes
No
Yes 1
X
Yes
Yes
Lab
EDD
Results
LABFLAG
text
Laboratory qualifiers. See Valid Value list.
Yes
Yes
No
Yes
No
Lab
EDD
Results
CONCFOUND
number
Enter numeric quantitative result value only. Report to three significant
figures. Do NOT enter any text string strings or symbols (e.g., "ND",
For analytes that are not detected, the laboratory's sample
specific MDL (i.e. with extract dilution factor, sample volume/weight
and final volume taken into account) is entered. Solids are reported on
a dry-weight basis. Tissues are reported on a wet-weight basis. Report
result units in "Unit" field, consistent for all sample fields.
Yes
No
Yes
Yes
No
Lab
EDD
Results
CONCSPIKE
number
For unspiked samples enter "0" for method analytes. For spiked
samples, enter the spike concentration representing the estimated
concentration in the final extract (i.e. with extract dilution factor,
sample volume/weight and final volume taken into account). Solids are
reported on a dry-weight basis. Tissues are reported on a wet-weight
basis. For EIS and NIS, enter the spike concentration representing the
concentration in the final extract in units consistent with sample result
units. The reporting units for this project are parts per trillion (ppt) or
nanograms per liter (ng/L) for aqueous samples and parts per billion
micrograms per kilogram (jig/kg) for solid samples. Report to 3
significant figures.
Yes
No
Yes
Yes
Yes
Lab
EDD
Results
PERCENTREC
number
For unspiked samples, leave blank. No text should be included in this
field (e.g. N/A). For spiked samples (OPR. LLOPR, MDLs and
LOQVER), enter the spike percentage recovery as a whole number
(e.g., 95 versus 0.95). Do NOT include "%" symbol. For EIS and NIS
recoveries, enter the spike % recovery as a whole number (e.g., 95
versus 0.95). Report to 3 significant figures. Do NOT include
Yes
No
No
Yes
Yes
Lab
EDD
Results
MDL
number
Method Detection Limit. Enter the sample specific MDL (i.e. with
extract dilution factor, sample volume/weight and final volume taken
into account). The reporting units for this project are parts per trillion
(ppt) or nanograms per liter (ng/L) for aqueous samples and parts per
billion micrograms per kilogram (jig/kg) for solid samples. Report to 3
significant figures.
Yes
No
No -9
Yes
Yes
15
-------
Appendix C - Project Database - Database Dictionary
Table
Field
Data type
Definition and Comments
Direct
from
EDD
Valid
Value
Field
Required
field
Default
Value
Primary
Key
Include in
Amended
EDD for
DV
Include in
Exports for
IDA
Lab EDD
Results
LOQ
number
Limit of Quantitation. Enter the sample specific LOQ (i.e. with extract
dilution factor, sample volume/weight and final volume taken into
account). Report to 3 significant figures. The reporting units for this
project are parts per trillion (ppt) or nanograms per liter (ng/L) for
aqueous samples and parts per billion micrograms per kilogram ((.ig/kg)
for solid samples. Report to 3 significant figures.
Yes
No
No
-9
Yes
Yes
Lab EDD
Results
UNIT
text
The reporting units must be consistent for the sample record including
Cone Found, MDL, LOQ etc. The reporting units for this project are
parts per trillion (ppt) or nanograms per liter (ng/L) for aqueous
samples and parts per billion micrograms per kilogram ((.ig/kg) for solid
samples. Ensure that all values for the sample record are reported in the
same units. See Valid Value list.
Yes
Yes
Yes
No
No
Lab EDD
Results
unit final
text
The reporting unit, standardized
No
Yes
Yes
Yes
Yes
Lab EDD
Results
SAMPLE_
TRAN SITIONRATIO
text
Enter the calculated Transition Ratio (Quant Ion Area/Conf Ion Area)
for each analyte in the sample. Report to 3 significant figures. For
analytes this does not apply to (PFBA, PFPeA, NMeFOSE, NEtFOSE,
PFMPA, and PFMBA), leave this field blank. No text should be
included in this field (e.g. N/A).
Yes
No
No
Yes
No
Lab EDD
Results
EXPECTED_
TRAN SITIONRATIO
text
Enter the expected Transition Ratio (Quant Ion Area/Conf Ion Area)
for each analyte per the method. Report to three significant figures. For
analytes this does not apply to (PFBA, PFPeA, NMeFOSE, NEtFOSE,
PFMPA, and PFMBA), leave this field blank. No text should be
included in this field (e.g., N/A).
Yes
No
No
Yes
No
Lab EDD
Results
RRT
text
Enter relative retention time
Yes
No
No
Yes
No
Lab EDD
Results
SAMPLESIZE
number
Enter volume (aqueous samples) or weight (solid samples) of sample
extracted (in liters for aqueous samples, in kilograms for solids).
Yes
No
Yes
Yes
No
Lab EDD
Results
SAMPLESIZEUNIT
text
Will be liters (L) for aqueous samples or kilograms (Kg) for solid
samples
Yes
No
Yes
Yes
No
Lab EDD
Results
EXTRACTIONDATE
short date;
mm/dd/yyyy
Use format mm/dd/yyyy (e.g. 11/20/2019) - do not include time stamp.
Yes
No
Yes
Yes
No
Lab EDD
Results
PERCMOISTURE
number
Percent moisture in solid samples only. Enter the percent moisture as a
whole number (e.g., 73 versus 0.73). Do NOT include "%" symbol.
Yes
No
No
Yes
No
Lab EDD
Results
MATRIX
text
Matrix analyzed. See Valid values list.
Yes
Yes
Yes
Yes
Yes
15
-------
Appendix C - Project Database - Database Dictionary
1 :i lilt-
Data l\lu-
Definition anil ( 'oniuicut>>
Di nil
Innii
I.DI)
\ aliil
Value
Iit-Id
Uci|iiiml Default
Ill-Id Value
I'liina n
Ur\
Include ill
Amended
COD for
HHNI
Include
|-'.\porl*
IDA
Lab
EDD
Results
METHOD
text
Laboratory SOP Name in format of "name(space)revision number"
Yes
No
Yes
Yes
No
Lab
EDD
Results
jSTUDYPHASE
text
(Multi-Lab Validation Study Phase. See Valid Value list.
Yes
Yes
Yes
Yes
No
Lab
EDD
Results
] SAMPLE TYPE
text
(See Valid Value list.
Yes
Yes
Yes
X
Yes
Yes
Lab
EDD
Results
(result type
text
(Code for Result Type. See Valid Value list.
' No
Yes
Yes
Yes
Yes
Lab
EDD
Results
spike cat
text
(Code for Spike Category. See Valid Value list.
" No
Yes
Yes
Yes
Yes
Lab
EDD
Results
validation level
text
Stores information on the level of data validation that has been
completed for the chemistry data.
No ]
No
Yes ( Level 4
Yes
No
Lab
EDD
Results
(validator
text
(Code for Data Validator. See Valid Value list.
No
Yes
Yes
Yes
No
Lab
EDD
Results
(dv qualifier
text
(Code for Data Validator qualifiers. See Valid Value list.
No
Yes
r No r
Yes
No
Lab
EDD
Results
dv qualifier reason
text
Data validation qualifier reason codes.
" No (
No
No
Yes
No
Lab
EDD
Results
dv notes 1
text
(Include comments to distinguish the meaning of the dv qualifier
(assignment (e.g., distinguishing the -J qualifier)
"" No
No
No r
Yes
No
Lab
EDD
Results
dv notes2
text
(Additional information provided by validator deemed pertinent to their
(dv qualifier assignment.
" No (
No
I" No
Yes
No
Lab
EDD
Results
d\ result
number
( Validator recommended result for concentration. If this is provided,
(entries must be made in the dv ResultChange yn field and
(dv ResultChange desc fields.
No j
No
No
Yes
No
Lab
EDD
Results
(dv ResultChange yn
Logical
(Enter Y or N. Indicates whether the validator made a recommendation
(to change the result for concentration.
No ;
No
Yes
Yes
No
Lab
EDD
Results
(dv ResultChange desc
text
Description of the reasons for validator recommending a change to the
result for concentration.
No !
No
r No r
Yes
No
Lab
EDD
Results
Reviewer qualifier
text
Code for qualifiers applied by NAVY/EPA reviewers of data
validation results. See Valid Value list.
No j
Yes
r No
Yes
No
Lab
EDD
Results
(Reviewer notes
text
Notes from NAVY/EPA reviewers of data validation results.
No
No
f No
Yes
No
Lab
EDD
Results
( final qualifier
text
iCode for Final Qualifier. See Valid Value list.
No |
Yes
r No r
No
Yes
Lab
EDD
Results
final result
number
(Final result for concentration. Combines CONC FOUND and
(validator result fields.
No
No
Yes
No
Yes
Lab
EDD
Results
lab rep
text
Data manager assigned. Laboratory replicate number; to assist with
completeness and duplicate checks.
No ;
No
Yes
Yes
No
Lab
EDD
Results
(sample rep
text
(Data manager assigned. From lu MatrixType.Rep field; to assist with
(spike percent rec calculation
" No
No
r No r
No
No
Lab
EDD
Results
(sample root
text
Data manager assigned. Sample NO without the Reg suffix; to assist
with spike percent rec calculation
No !
No
No
No
No
Lab
EDD
Results
(spike level
number
Data manager assigned. From lu SpikeLevel table; to assist with
spike percent rec calculation
No
No
r No r
No
Yes
15
-------
Appendix C - Project Database - Database Dictionary
Direct Valid Include in jncju(je jn
Table Field Datatype Definition and Comments from Value Re?Z le''Ult P™y Exports for
EDO Field fidd Value Key EDDDvf°r IDA
Lab EDD Results
cone minus native
spike percent rec
spk pet rec DNC
CONCFOUNDval
LOQ val
MDL val
LABSAMPLEIDclean
qaqc dup
DM notes
DM notes2
EditDate
number
Data manager calculated. Interim value in spike percent rec
calculation
No
No
No
No
Yes
Lab EDD Results
number
Data manager calculated. Matrix spike percent recovery.
No
No
No
No
Yes
Lab EDD Results
text
Data manager assigned. Determination of Calculate/DNC (do not
calculate)for spike percent rec calculation
No
No
No
No
Yes
Lab EDD Results
text
Data manager assigned. CONC FOUND as a value; to assist with
database-wide QAQC checks.
No
No
No
No
No
Lab EDD Results
text
Data manager assigned. LOQ as a value; to assist with database-wide
QAQC checks.
No
No
No
No
No
Lab EDD Results
text
Data manager assigned. MDL as a value; to assist with database-wide
QAQC checks.
No
No
No
No
No
Lab EDD Results
text
Data manager assigned. Standardized LAB SAMPLE ID to remove re-
analysis suffixes; to assist with completeness and duplicate checks.
No
No
Yes
No
Yes
Lab EDD Results
text
Data manager assigned. Identifies LLOPR OPR and MB double-duty
samples and exclude one of the results for the 'all in' database exports.
No
No
No
No
No
Lab EDD Results
text
Data manager notes.
No
No
No
No
No
Lab EDD Results
text
Data manager notes - 2.
No
No
No
No
No
Lab EDD Results
text
Date of append to Lab EDD Results table.
No
No
Yes
No
No
dicValidValues
Table
text
Valid value table name.
No
No
Yes
No
No
dicValidValues
Field
text
Valid value field name.
No
No
Yes
No
No
dicValidValues
Value
text
Acceptable valid value codes.
No
No
Yes
No
No
dicValidValues
Description
text
Description of valid value codes, if necessary
No
No
Yes
No
No
dicValidValues
VVL match alt field
text
Related valid value field name.
No
No
No
No
No
dicValidValues
VVL match alt code
text
Matching valid value code.
No
No
No
No
No
dicValidValues
Validator
text
Data validator assoicated with each LAB ID CODE
No
No
No
No
No
LU Compound
SORT ORDER
number
Sort order to apply to data summary tables.
No
No
Yes
No
No
LU Compound
PFAS_ ACRONYM
text
Use acronyms included in the example EDD. See Valid Value list.
No
Yes
Yes
X
No
No
LU Compound
COMPOUND
text
Use the names included in the example EDD. Method analytes, and EIS
and NIS compounds must be reported for each sample. See Valid Value
list.
Yes
Yes
Yes
Yes
Yes
LU Compound
CAS NO
text
Chemical Abstract Service Registration Number
Yes
Yes
Yes
Yes
Yes
LU Compound
result type
text
Code for Result Type. See Valid Value list.
No
Yes
Yes
No
No
LU Spike Levels
PFAS_ ACRONYM
text
Use acronyms included in the example EDD. See Valid Value list.
No
Yes
Yes
X
No
No
LU Spike Levels
Matrix
text
Name of the matrix. See Valid Value list.
No
Yes
Yes
X
No
No
LU Spike Levels
Low Spike
number
Low spike concentration
No
No
Yes
No
No
LU Spike Levels
High Spike
number
High spike concentration
No
No
Yes
No
No
15
-------
Appendix C - Project Database - Database Dictionary
1 able
Data l\lu-
Definition anil ( 'oniuicut>>
Di reel
Innii
inn
\ aliil
Value
Held
Uci|iiiml
ll.ld
Default
\ .iliie
I'liina n
l\e\
Include ill
Amended
COD for
HHNI
Include in
lAporl* lor
IDA
LU Spike Levels
Unit
text
Unit of spike concentration
No
No
Yes
No
No
lu MatrixKey
Matrix Type
text
Matrix (full name)
No !
No
Yes
No
No
lu MatrixKey
¦ Requested Name
text
Descriptive name of sample
: No
No
Yes
No
No
lu MatrixKey
: Description
text
¦Description of sample
No '
No
Yes
No
No
lu MatrixKey
Matrix Code
text
Matrix (code)
: No
No
Yes
No
No
lu MatrixKey
Sample Identifier
text
Sample identifier (middle component of SamplelD)
No '
No
Yes
No
No
lu MatrixKey
SamplelD
text
SamplelD (EDD SAMPLE NO must match to this code)
No
No
Yes
No
No
lu MatrixKey
spike cat
text
Spike category (low, high, etc)
No
No
Yes
No
No
lu MatrixKey
¦ Rep
text
Sample replicate number (last component of SamplelD)
No
No
Yes
No
No
lu MatrixKey
: Selected
text
Indicates if sample was selected for use in the study
No
No
Yes
No
No
Note: The Required Fields may be revised during database development; maximum field lengths will be incorporated into the database structure during development.
15
-------
ADDendix D - Supplemental guidance for correctly DODulatine the EDD Template
Item
Guidance
1
If possible, include all results in one worksheet.
2
We will be running QA/QC routines on the EDDs to ensure they are populated correctly. These will be delivered to you in an Excel file (e.g.,
L ABN AME_RW_verO_EDD_Error_Summary. xlsx).
If you have questions/issues regarding the Error Summary report, please incorporate comments directly into the Excel file and send it back to us for review
(via SharePoint).
3
Instructions for reporting CONCFOUND for NIS compounds:
1. Option 1: Report NIS Mass in CONC FOUND, and in the accompanying report provide example calculation and point to where the data in the
numerator (e.g., field sample) and the denominator (e.g. CCV) are found.
2. Option2: Complete the EDDs with the NIS percent recoveries based on areas (i.e., no mass reported). CONC FOUND does not need to be populated.
a. If Option 2 is selected then
i. In the report provide the formula and example calculations for one sample per batch
ii. Point to where those areas values are found in their data packages (i.e., ensure they have reported the NIS area for the field (target) sample and
the comparative area from either the mid-point of the ICAL, CCV, or equivalent.
4
Instructions for populating EDD when a single sample is serving the purpose of the MDLB and MB samples:
1. Copy the results and code the SAMPLE NO field as 'MDLB' for one set of results, and 'MB' for the other set of results.
2. Ensure that the case narrative clearly identifies that the blank sample was used for multiple purposes.
5
Ensure that B flags are applied as indicated by the instructions:
"For analytes that were detected in the associated MB of a sample that exceeded Vi LOQ or is at a concentration greater than 1/1 Oth the concentration in
the sample, whichever is greatest. The MB must also be flagged with a "B" for all concentrations greater than 'A the LOQ."
If the CONC FOUND is between the MDL and LOO AND it is at a concentration greater than 1/2 LOO. the flag should be BJ or JB.
6
Although the instructions for the CONC FOUND field indicate "For analytes that are not detected, the laboratory's sample specific MDL", the exceptions
are for the following sample types, where CONC FOUND can be less than the MDL:
MDLS
LOQVER
Blanks (MB and MDLB)
7
For instances where there are re-analysis not due to dilution, all results must be reported in the EDD (i.e., the original analysis and all subseqent re-analysis).
35
-------
ADDendix D - SuDDlemental guidance for correctly DODulatine the EDD Template
8
The Sample Coding spreadsheet lists the mandatory batch QC samples that are required for Phase 3 and Phase 4 submittals. All mandatory batch QC
samples must be present in the EDD submittals.
9
Do not add suffixes to SAMPLE NO (e.g., IPR1, MLDB 2) - LAB SAMPLE ID will differentiate samples.
10
Fields that must be reported to 3 significant figures:
CONC FOUND
CONC SPIKE
PERCENT REC (DOES need to be reported to 3 sig figs; report as a whole number (95.1), not a fraction (0.951)
MDL
LOQ
SAMPLE TRANSITION RATIO
EXPECTED TRANSITION RATIO
Note that the results in these fields must be rounded appropriately to 3 significant figures. Changing the display for the number of decimal places is not
sufficient.
11
Solids are reported on a dry-weight basis. Tissues are reported on a wet-weight basis.
12
UNIT field must be consistent across all samples.
13
The reporting units for this project are parts per trillion (ppt) or nanograms per liter (ng/L) for aqueous samples and parts per billion micrograms per
kilogram (ng/kg) for solid samples.
14
Do not include text in number fiels (e.g. N/A, %, ND, <).
15
Percent recovery must be reported in the EDD for IPR samples.
36
-------
Appendix E - Project Database - Valid Value Codes and Descriptions
YYI.Iuld
YalidYalue
YY l)i'v(i i|>linii
YYI. mahli
all Ik-Id
YYI.
inalcli all
code
Yalidalor
LAB ID CODE
ALPHA
Alpha Analytical
lab num
3
JACOBS
LAB ID CODE
BATTELLE
Battelle
lab num
6
JACOBS
LAB ID CODE
CALEPA
CalEPA DTSC
lab num
2
PYRON
LAB ID CODE
ELLET
Eurofins Lancaster Labs
lab num
10
JACOBS
LAB ID CODE
ETA
ETA, Sacramento
lab num
1
PYRON
LAB ID CODE
GEL
GEL Laboratories
lab num
8
JACOBS
LAB ID CODE
MDH
Maryland Department of Health
lab num
5
JACOBS
LAB ID CODE
PACE
GCAL/Pace
lab num
9
JACOBS
LAB ID CODE
SGSNA
SGS North America
lab num
7
PYRON
LAB ID CODE
VISTA
Vista Analytical
lab num
4
PYRON
MATRIX
BS
Biosolids
MATRIX
GW
Groundwater
MATRIX
LC
Landfill Leachate
MATRIX
OS
Ottawa sand for all soil, sediment, and biosolid MBs
MATRIX
QC
Quality Control Sample
MATRIX
RT
Reference Tissue for tissue MBs
MATRIX
RW
Reagent water for all aqueous MBs
MATRIX
SD
Sediment
MATRIX
ss
Soil
MATRIX
sw
Surface water
MATRIX
TS
Tissue
MATRIX
WW
Wastewater
result type
EIS
Extracted Internal Standard
result type
NIS
Non-Extracted Internal Standard
result type
TRG
Target analyte
SAMPLE TYPE
BLANK
method analytes in MBs
SAMPLE TYPE
EIS
EIS in all samples
SAMPLE TYPE
IPR
method analytes in IPR IDC samples
SAMPLE TYPE
LLOPR
method analytes in LLOPRs
SAMPLETYPE
LOQVER
Method analytes in MDL LOQVER IDC samples
SAMPLE TYPE
MDLB
Method analytes in MDL Blank IDC samples
SAMPLE TYPE
MDLS
Method analytes in MDL Spike IDC samples
SAMPLE TYPE
NIS
NIS in all samples
SAMPLE TYPE
NORMAL
method analytes in field samples
SAMPLE TYPE
OPR
method analytes in OPRs
spike cat
HIGH
High
spike cat
LOW
Low
STUDYPHASE
Phase 3 - ICAL
Initial Calibration
STUDY PHASE
Phase 3 - IDC
Initial Demonstration of Capabilities (IDC)
STUDY PHASE
Phase 4.4.1
GW, SW, and WW matrices
STUDY PHASE
Phase 4.4.2
SS and SD matrices
STUDY PHASE
Phase 4.4.3
Tissue matrices
STUDY PHASE
Phase 4.4.4
LC and BS matrices
validator
CHEMVAL
ChemVal
validator
JACOBS
Jacobs Engineering
validator
PYRON
Pyron Environmental
Analysis
PFAS
NULL
Lab Flag
B
Detected in the associated MB of a sample that
exceeded lA LOQ or is at a concentration greater
than l/10th the concentration in the sample,
whichever is greatest.
37
-------
Appendix E - Project Database - Valid Value Codes and Descriptions
YYI. I-kid
YalidYalue
YY l)i'v(i i|>linii
YYI. mahli
all Held
YYI.
inalcli all
code
Yalidalor
Lab Flag
D
When the reported result is from a dilution
Lab Flag
I
Fail to meet ion ratio criteria
Lab Flag
J
At a concentration between the MDL and LOQ
Lab Flag
U
Not detected or were detected at a concentration less
than the MDL
UNIT
ng/L
nanograms per liter
MATRIX
GW
UNIT
ng/L
nanograms per liter
MATRIX
LC
UNIT
ng/L
nanograms per liter
MATRIX
SW
UNIT
ng/L
nanograms per liter
MATRIX
WW
UNIT
ug/kg
micrograms per kilogram
MATRIX
BS
UNIT
ug/kg
micrograms per kilogram
MATRIX
SD
UNIT
ug/kg
micrograms per kilogram
MATRIX
ss
UNIT
ug/kg
micrograms per kilogram
MATRIX
TS
dv qualifier
I
Suspect
dv qualifier
J
Estimated
dv qualifier
J-
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J- when the %D is below acceptance
criteria
dv qualifier
J-
If branched isomers were not included in the
summed result reported, qualify associated detects
as J-
dv qualifier
J+
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J+ when the %D is higher than acceptance
criteria
dv qualifier
U
Values below the MDL are considered non-detects
and are qualified as U at the stated MDL.
dv qualifier
UJ
Verify that the %Ds are within the acceptance
criteria. Non-detects are qualified as UJ in all
associated samples for %D outside of acceptance
criteria.
dv qualifier
UJ
Estimated non-detect
dv qualifier
X
Exclusion of data is recommended
Reviewer qualifier
I
Suspect
Reviewer qualifier
J
Estimated
Reviewer qualifier
J-
If branched isomers were not included in the
summed result reported, qualify associated detects
as J-
Reviewer qualifier
J-
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J- when the %D is below acceptance
criteria
Reviewer qualifier
J+
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J+ when the %D is higher than acceptance
criteria
38
-------
Appendix E - Project Database - Valid Value Codes and Descriptions
YYI. I-kid
\ ulid\ ahu-
YY l)i'v(i i|>linii
YYI. maUli
all Held
YYI.
inalcli all
code
Yalidalor
Reviewer qualifier
ll
Values below the MDL are considered noil-delects
and are qualified as U at the stated MDL.
Reviewer qualifier
UJ
Verify that the %Ds are within the acceptance
criteria. Non-detects are qualified as UJ in all
associated samples for %D outside of acceptance
criteria.
Reviewer qualifier
UJ
Estimated non-detect
Reviewer qualifier
X
Exclusion of data is recommended
39
-------
Appendix F - Project Database - Valid Value Codes and Descriptions for Compounds
PIWS At RON Y\1
Compound
( AS NO
Kesul(_ 1 >pe |
13C2-4:2FTS
| lH,lH,2H,2H-Perfluoro-l-[l,2-13C2]hexanesulfonic acid
NA
EIS
13C2-6:2FTS
111.111.211.21 l-IVi 1 Iiioio- 1 -| 1.2-1 '( 2|iiclaiicsiiirniiic acid
NA
EIS
13C2-8:2FTS
lH.lH.2H.2H-Pcrfluoro-l-| 1.2-13C2|dccancsulfonic acid
NA
EIS
13C2-PFDoA
Pcrfluoro-n-l 1.2-13C2|dodccanoic acid
NA
EIS
13C2-PFTcDA
Pcrfluoro-n-| 1.2-13C2|lclradccanoic acid
\ \
EIS
13C3-HFPO-DA
Tclrafluoro-2-hcplafluoropropoxy-13C3-propanoic acid
\ \
EIS
13C3-PFBS
Pcrfluoro-1 -|2.3.4-13C3 |bulancsulfonic acid
\ \
EIS
13C3-PFH.\S
Pcrflnoro-1 -| 1.2.3-13C3|hcxancsulfonic acid
\ \
EIS
13C4-PFBA
Pcrfluoro-n-l 13C4|bulanoic acid
\ \
EIS
13C4-PFHpA
Pcrfluoro-n-[l,2,3,4-13C4]heptanoic acid
\ \
EIS
13C5-PFH.\A
Pcrfluoro-n-[l,2,3,4,6-13C5]hexanoic acid
\ \
EIS
13C5-PFPcA
Pcrlluoro-n-l 13C5"|pcnlanoic acid
\ \
EIS
13C6-PFDA
Pcrfluoro-n-l 1.2.3.4.5.6-13C6|dccanoic acid
\ \
EIS
13C7-PFUnA
Pcrfluoro-n-| 1.2.3.4.5.6.7-13C7|undccanoic acid
NA
EIS
13C8-PFOA
Pcrfluoro-n-[13C8]octanoic acid
NA
EIS
13C8-PFOS
Pcrfluoro-l-[13C81oclancsulfonic acid
\ \
EIS
13C8-PFOSA
Pcrfluoro-1 -| 13C8 |oclancsulfonamidc
\ \
EIS
13C9-PFNA
Pcrfluoro-n-[13C9]nonanoic acid
\ \
EIS
D3-NMcFOSA
N-mcthyl-d3 -perfluoro- 1-octanesulfonamide
\ \
EIS
D3-NMcFOSAA
:N-mclhyl-d3-pcrfluoro-1-oclancsulfonamidoacclic acid
NA
EIS
D5-NEIFOSA
N-clhv l-d5-pcrfluoro-1 -oclancsulfonamidc
\ \
EIS
D5-NEIFOSAA
N-clhv l-d5-pcrfluoro-1 -oclancsulfonamidoacclic acid
\ \
EIS
D7-NMcFOSE
N-mcthyl-d7 -perfluorooctanesulfonamidoethanol
\ \
EIS
D9-NEIFOSE
N-clhy l-d9-pcrfluorooclancsulfonamidoclhanol
\ \
EIS
13C2-PFDA
Pcrfluoro-n-| 1.2-13C2|dccanoic acid
\ \
NIS
13C2-PFH.\A
Pcrfluoro-n-[l,2-13C2]hexanoic acid
\ \
NIS
13C3-PFBA
¦Pcrfluoro-n-l2.3.4-13C3|bulanoic acid
\ \
NIS
13C4-PFOA
Pcrfluoro-n-[ 1.2.3.4-13C4]oclanoic acid
\ \
NIS
13C4-PFOS
Pcrfluoro-n-| 1.2.3.4-13C4|oclancsulfonic acid
NA
NIS
13C5-PFNA
Pcrfluoro-n-[l,2,3,4,5-13C5]nonanoic acid
NA
NIS
1802-PFHxS
Pcrfluoro-l-hexane[1802]sulfonic acid
\ \
NIS
1 lCl-PF30UdS
1 l-chlorocicosafluoro-3-oxaundccanc-l-sulfonic acid
TRG
3:3 FTC A
3-Pcrfluoropropyl propanoic acid
i5(>-i>2-5
TRG
4:2FTS
1H. lH.2H.2H-Pcrfluorohcxanc sulfonic acid
757124-72-4
TRG
5:3 FTC A
211.211. '11. '1 l-IVi'l'liKii\KiclaiKnc acid
914637-49-3
TRG
6:2FTS
1H. lH.2H.2H-Pcrfluorooclanc sulfonic acid
27619-97-2
TRG
7:3 FTC A
3-Pcrfluorohcplyl propanoic acid
812-70-4
TRG
8:2FTS
1H. lH.2H.2H-Pcrfluorodccanc sulfonic acid
39108-34-4
TRG
9C1-PF30NS
9-chlorohexadecafluoro-3-oxanonane-l-sulfonic acid
756426-58-1
TRG
ADONA
4.8-dio.\a-3H-pcrfluorononanoic acid
919005-14-4
TRG
HFPO-DA
Hcxafluoropropylcnc oxide dimcr acid
13252-13-6
TRG
NElFOSA
N -cl hy 1 pc rfl uo roocla ncsul fo na midc
415 I-5U-2
TRG
NElFOSAA
N-clhyl perfluorooctanesulfonamidoacetic acid
2991-50-6
TRG
NElFOSE
N-clhy 1 pcrfluorooclancsulfonamidoclhanol
1691-99-2
TRG
NFDHA
Nonafluoro-3.6-dioxahcplanoic acid
151772-58-6
TRG
NMcFOSA
N-mclhvl pcrfluorooclancsulfonamidc
TRG
NMcFOSAA
jN-methyl perfluorooctanesulfonamidoacetic acid
2355-31 -9
TRG
NMcFOSE
N-mclhvl pcrfluorooclancsulfonamidoclhanol
24448-09-7
TRG
PFBA
Pcrfluorobulanoic acid
375-22-4
TRG
PFBS
(Perfluorobutanesulfonic acid
375-73-5
TRG
40
-------
Appendix F - Project Database - Valid Value Codes and Descriptions for Compounds
PIWS At RON Y\1
Compound
( AS NO
Resull T\pe
PI 1) \
Pcrfluorodccanoic acid
>35-76-2
TRG
PI \ )o\
Pcrfluorododecanoic acid
>07-55-1
TRG
Pll)^
Pcrfluorododecanesulfonic acid
-35-77-3
TRG
PI IIS \
Pcrriiioro(2-clho.\> clhanc)siiironic acid
1 1 ^507-82-7
TRG
PI 1 Ip \
Pcrfluorohcplanoic acid
'"5-S5-1'
TRG
PI 1 lp-
Pcrfluoroheptanesulfonic acid
:"5-'J:-S
TRG
PI 1 K \
Pcifluorohcxanoic acid
TRG
PI 1 K-
Pcrfliiorohcxancsuironic acid
;55-4i-4
TRG
PI All! \
Pcrniioro-4-mclho.\\bulanoic acid
S(..()'J()-S'J-5
TRG
PIMP \
Pcifliinrn-'-iiiclhn\\ propanoic acid
TRG
Pl \ \
Pcrfluorononanoic acid
;"5-.)5-|
TRG
PI\S
Pcrfluorononancsulfonic acid
i.s:5'j-i:-i
TRG
PI () \
Pcrfluorooclanoic acid
:'5-(>"-l
TRG
PR >S
PcifliinriKiclMiicMiirniiic acid
n.-:-i
TRG
PI ()S\
Pcrfliiorooclancsuironamidc
"54-'H-(.
TRG
PI IV \
Pcrfluoropcnlanoic acid
TRG
Pi ivs
Pcrfluoropcnlancsulfonic acid
:"()(,-•) 1-4
TRG
PI 1 cl) \
IViriiininicliadccaiinic acid
TRG
PI III) \
Pcrfluorolridccanoic acid
TRG
PFUnA
(Pcrlluoroundecanoic acid
,2058-94-8
TRG
41
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Figure 2. Folder Structure for the ExaBlue SharePoint
9
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Each top-level folder contains sub-folders for different types of data, from different sources:
Project Documents
• Background Documents - This folder includes reports and documentation that guide the
MLV Study (e.g., Study Work Plan, UFP-QAPP, Background Analytical Data from SGS
AXYS, conventional analyses).
• Correspondence - MVS Team members ensured that project communication (including
email) is backed up. Correspondence included on the ExaBlue SharePoint are: any
written communication (including emails) that document major decisions and
information regarding study status and/or problems; a log documenting verbal
communication with team participants regarding study status or issues.
• Final DVR and Data - When the review processes for a matrix were completed, the
final versions of key documents were moved into this folder to provide efficient access
for MVS Team members tasked with preparing the MLV Study reports. This included:
final versions of the laboratory data package, HGL data package review checklist, data
validation reports (DVR), validated EDDs, EPA and Naval Sea Systems Command
(NAVSEA) review documents.
• Meetings and Schedules - This folder is a repository for meeting notes and status
reports.
Project Reports - MVS Team members with appropriate permissions (Section 3.1.2) maintain
working and final versions of the following reports generated during the MLV Study:
• Aqueous
• Biosolids/Landfill Leachate
• Soil/Sediment
• Tissue
Laboratory Data
• Lab Name - Each laboratory has their own folder including the same structure of sub-
folders.
o Phase 3 IDC - This folder includes the Phase 3 Initial Demonstration of
Capability (IDC) EDDs and Data Packages for aqueous, solid and tissue matrices.
o Phase 3 ICAL - This folder includes the Phase 3 Initial Calibration (ICAL) Data
Package.
o Matrix - There is one sub-folder for each of eight matrices (e.g, wastewater,
surface water, groundwater, soil, sediment, biosolids, landfill leachate, tissue),
and includes the current version of the EDDs and Data Packages. There are
additional directories for:
10
-------
¦ Communications - This folder is used to store documents provided to the
laboratories (e.g., EDDs with comments incorporated, resubmission
requests).
¦ Archive - This folder includes versions of the EDDs and Data Packages
that have been replaced with re-submissions.
o SOP - This folder stores each laboratory's Standard Operating Procedures.
• Other Lab Data - This folder includes sub-directories to store files for:
o Corrective Actions
o ERA Laboratory Instructions
o Spike Levels
o Wellington Certificates of Analysis
• PFAS Compound Names - The folder includes the file listing the Compound Name,
CAS_NO, and PFAS_Acronyms to be used by the laboratory.
• Shared - This folder includes miscellaneous files providing instruction to the
laboratories.
Each sub-folder in the Laboratory sub-directory includes an Archive folder to store versions of
database exports and files with statistical results that have been replaced with revised file
versions.
Validator Data
• Validator Name - Each validator has their own folder including the same structure of
sub-folders.
o Phase 3 IDC- This folder includes sub-directories for each of the three IDC
matrices (aqueous, solid and tissue).
¦ To Validator - Phase 3 IDC data packages and Amended EDDs are
uploaded to this folder (by HGL and Exa, respectively) for each laboratory
(not shown on Figure 2).
¦ From Validator - Phase 3 IDC results provided by the data validator are
posted to this folder (data validation report, Amended EDD with validator
fields populated, evidence of 10% verification, checklist) for each
laboratory (not shown on Figure 2).
o Matrix - There is one sub-folder for each of eight matrices.
¦ To Validator - data packages and Amended EDDs are uploaded to this
folder (by HGL and Exa, respectively), for each laboratory.
¦ From Validator - results provided by the data validator are posted to this
folder (data validation report, Amended EDD with validator fields
populated, evidence of 10% verification and checklist), for each
laboratory.
• Shared - This folder includes miscellaneous files providing directions to the validators.
11
-------
Each sub-folder in the Validator Data sub-directory includes an Archive folder to store versions
of Amended EDDs, Data Packages and data validator submissions that have been replaced with
re-submissions.
Statistics
• Phase 3 - There is one folder for each of the three IDC matrices and the ICAL data.
o Phase 3 IDC - There is one folder for each of the three IDC matrices (aqueous,
solid and tissue).
¦ To IDA - Database Exports are posted to this folder (from Exa; not shown
on Figure 2).
¦ From IDA - IDA posts the statistical report with appendices (pdf), along
with supporting calculations (csv; not shown on Figure 2) to this folder.
o ICAL
¦ To IDA - This folder stores the tabular version of the ICAL results (from
Science and Engineering for the Environment [SEE] and HGL; not shown
on Figure 2).
¦ From IDA - IDA posts the statistical report with appendices (pdf), along
with supporting calculations (csv; not shown on Figure 2).
• Matrix - There is one sub-folder for each of eight matrices, as well as folders with
combined matrices (e.g., "AqueousCombined; not shown on Figure 2).
o To IDA - Database Exports are posted to this folder (from Exa).
o From IDA - IDA posts the statistical report with appendices (pdf), along with
supporting calculations (csv) to this folder,
o Report Statistics - When final versions of Database Exports and IDA reports are
prepared, they are posted to this folder to provide access to EPA and General
Dynamics Information Technology (GDIT) contractors.
Each sub-folder in the Statistics sub-directory includes an Archive folder to store versions of
database exports and files with statistical results that have been replaced with revised file
versions.
Database
• Database - A copy of the Project Database (MS Access) is posted to this folder when the
MLV Study reports are completed. The version will be indicated by the matrix included
(AQ for aqueous media; SOL for soils/sediment; TS for tissue; BLL for biosolids/landfill
leachate) and the posted date in the filename (e.g., MLVS_AQ_Database_20230630).
• Documentation - When MLV Study reports are completed, current database
documentation files (e.g., database dictionary, valid value lists, QA/QC application,
scripts, archived database copies) are posted in this folder.
12
-------
Tracking - this folder contains the shared files used for logging submissions from laboratories,
data validators and reviewers, and tracking project status. This main directory includes the
following folders:
• Exa Internal Tracking - stores detailed information on file submissions and the status
of the review process.
• Archive - stores backup versions of the tracking files.
Laboratories have access to their specific folders ONLY as described in Section 3.1.2. The
Project Documents folder also allowed limited access as described below. Exa and HGL are
responsible for reviewing the files uploaded to the site by the laboratory, validator, and
statistician team members, ensuring their documents are properly filed and the file-naming
protocols are adhered to (described in Section 3.3).
3.1.2 Access and Permissions
There is a strict permission structure limiting access to certain folders to specific team members.
Exa is the only organization with Administrator permission, with full control to audit all site
content and receive administrative messages.
SharePoint information is permissions-trimmed, meaning that individuals only have access to
designated folders within the ExaBlue SharePoint folder structure. In other words, members from
each individual laboratory can only access their own EDDs and Data Packages in order to maintain
control of proprietary data. Similarly, individuals from the validation or statistics groups are only
able to access the folders designated to them.
Specific members of the MVS Team have access to different folders. For example, under the top-
level "Statistics" folder, some MVS Team members have access to the "To IDA" and "From IDA"
folders which store the draft versions of database exports and statistical results. A smaller group
will have permissions to access the final versions included in the "Report Statistics" folder. Table
3 includes the list of project participants that have access to the ExaBlue SharePoint.
13
-------
Table 3. Project Participants with Access to the ExaBlue SharePoint
Team / Organization
Team Member
Method Validation Study Team
NAVSEA
Janice Willev
SEE LLC
Tim Thompson
AFCEC
Hunter Anderson
SERDP/ESTCP
Andrea Leeson
EPA (OW)
Adrian Hanlev
SERDP/ESTCP
Anastasia Nickerson
SERDP/ESTCP
Stephen Levitas
GDIT
Chip McCartv
GDIT
Mirna Alpizar
Data Management Team
Exa
Dawn Smorong. Michael Tweiten. Peggy Mvre. Glenn Sutula
HGL
Joe Skibinski. Denise Rivers. Ken Rapuano. Andrea Fletcher.
Joe Vilain. John Powell
Laboratories
California DTSC
Katie Hamblin
Pace
Stephen Somerville
SGS
Andrea Colby
Battel lc
Jon Thorn
GEL
Vonda Fields
Vista Analytical
Anne Wilhoit: Jamie Fox
Maryland DOH
Sin Urban
Alpha Analytical
Alvcia Mogavzel
Eurofins Lancaster
Bradley Avars
ETA - Sacramento
Jill Kellman
Validators
Pvron
Mingta Lin
Jacobs
Maggie Radford. Jeremy Bishop
Chcm Val
Kathi Gumpper: John Gumpper
Statisticians (IDA)
Allyson Buytendyk
3.2 File Tracking System
A File Tracking System ("Tracking System") was developed to ensure that files and information
provided by project participants are logged at each stage of the project. The workflow for handling
data from the laboratories, through the validators and the statisticians, is discussed in Section 4.1.
In this section, the format of the Tracking System is defined and described.
14
-------
The Tracking System includes three shared documents, posted in the ExaBlue SharePoint:
1. MLVS_FileTracking.xlsx - Exa internal tracking, which is a detailed log of files
received.
2. MLVS_Review_Status.xlsx - summary status information for the overall project.
3. EPA NAVSEA Review Tracker.xlsx - status of the review of data validation reports
conducted by EPA and NAVSEA personnel.
3.2.1 Exa Internal Tracking
The purpose of Exa's internal tracking file (MLVSFileTracking.xlsx) is to log the receipt of
submissions from laboratories, validators and reviewers, record the status of the review process,
and ensure that file versioning is recorded and monitored. Exa is responsible for updating the
internal tracking tables as files are submitted.
Exa Internal Tracking includes three main stages of logging files, partitioned into separate
worksheets in the file:
• General - Defines the basis for a unique set of files from the laboratory, including the EDD
and the Data Package, linked to the laboratory of origin and the matrix analyzed. If an EDD
is rejected and resubmitted, then the resubmitted EDD/Data Package receives a new
version number and are tracked separately from the original.
• Laboratory - This element of the Tracking System defines the status of laboratory data
receipt and review by the Data Management Team.
• Validator - This element of the Tracking System defines the status of receipt, processing,
and return of the laboratory data to and from the data validators.
The MLVS FileTracking.xlsx file also includes the following ancillary worksheets:
• EDD for DB - identifies the final Amended EDD versions, with data validator and review
input added, which were incorporated in the Project Database
• NIS updates - tracks the revisions of percent recovery results for non-extracted internal
standards (NIS) in the Project Database, which were received separately from the main
EDD for three laboratories.
• ICAL files - a listing of Phase 3 ICAL files received from the laboratories.
• ValidValues - a listing of acceptable entries for fields in the Tracking System constrained
by valid values.
• Field Descriptions - a listing of fields, with field descriptions in the three main tracking
worksheets.
The status of data provided to the statistics team (IDA) is not included in the Tracking System,
since they receive Database Exports for each matrix (i.e., not on an EDD-specific basis).
15
-------
A summary of the tracking fields is provided in Appendix A. Several Tracking System fields are
limited to specific content ("valid values"); the list of acceptable entries for the valid value fields
is provided in Appendix B.
3.2.2 ML V Review Status
The purpose of the shared 'MLVS Review Status.xlsx' document is to communicate overall
status information to the MVS Team. Each project phase is included in separate worksheets and
each matrix has a separate table to record the status of review progress. Table 4 shows an example
of a Review Status table. Exa and SEE are responsible for updating the MLV Review Status tables
as files are submitted and review steps are completed.
16
-------
Table 4. Example Review Status Table
Phase 3 IDOC - Reagent Water (RW)
Laboratory
Name
Current
Version
(DP/EDD)
DP Approval
Status (HGL)
EDD
Approval
Status (Exa)
Data Package
to DV?
Amended
EDD to DV?
DV Reports
Received?
SEE DVR
Review
complete?
DVR Ready
for Navy/EPA
Review
EDD Ready for
Navy/EPA
Review
Navy/EPA DV
Review
complete?
DV qualifiers
added to EDD?
Navy/EPA
qualifiers added
to EDD?
Data
Ready for
IDA?
ALPHA
8
Approved
Approved
10-Oct-22
06-Mar-23
Tech Memo
VO - yes
1—/ \J W U111VX11*3
confirmed
Tech Memo
VO - yes
Yes V2
3/30/2023
Yes
No
No
V
BATTELLE
2
Approved
Approved
27-Apr-22
29-Apr-22
V2-yes
All documents
confirmed 9/16
Yes V2
9/16/2022
Yes V0
9/16/2022
Yes
No
No
V
ELLET
3
Approved
Approved
29-Mar-23
18-Aug-22
V3 - yes
All documents
confirmed 9/27
Yes V3
9/27/2022
Yes V2
9/20/2022
Yes
Yes
Yes
V
GEL
-
Rejected
Rejected
-
-
-
-
NA
NA
-
-
-
NA
PACE
1
Approved
Approved
27-Apr-22
29-Apr-22
V1 - yes
All documents
confirmed 9/16
Yes VI
9/16/2022
Yes V0
9/16/2022
Yes
No
No
V
CALEPA
5
Approved
Approved
12-Aug-22
12-Aug-22
V2 - Yes
All documents
confirmed 9/15
Yes V2
9/15/2022
Yes V2
9/15/2022
Yes
No
No
V
ETA
5
Approved
Approved
10-Mar-23
21-Mar-23
V2 - yes
All documents
confirmed 9/27
Yes V2
9/27/2022
Yes V2
9/20/2022
Yes
Yes
No
V
MDH
2/6
Approved
Approved
27-Apr-22
20-Sep-22
V2 - yes
All documents
confirmed 10/4
Yes V2
10/4/2022
Yes V3
10/7/2022
Yes
Yes
Yes
V
SGSNA
4/6
Approved
Approved
18-Aug-22
18-Aug-22
V3 - yes
All documents
confirmed 9/16
Yes V3
9/16/2022
Yes VI
9/16/2022
V3 DVR - Yes
VI EDD-Yes
Yes
No
V
VISTA
4/3
Approved
Approved
21-Jul-22
30-Aug-22
V4 - yes
All documents
confirmed 9/16
Yes V4
9/16/2022
Yes V2
9/16/2022
V4 DVR - Yes
V2 EDD - Yes
No
No
V
Acronyms: DP - data package; DV - data validator; DVR - data validation report; EDD - electronic data deliverable; HGL - HydroGeoLogic: IDA - Institute for Defence Analyses; SEE - Science, Engineering and the Environment LLC
17
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3.2.3 EPA NAVSEA Review Tracker
The purpose of the shared 'EPA NAVSEA Review Tracker.xlsx' document is to communicate the
status and summary results from the review of data validation reports conducted by EPA and
NAVSEA personnel. NAVSEA and EPA are responsible for updating the 'EPA NAVSEA Review
Tracker.xlsx' tables as reviews are completed.
3.3 File-Naming Protocols
As part of the File Tracking System, a strict file-naming protocol was devised and guidance
produced for the laboratories, validators, and statisticians. Each laboratory EDD and
accompanying Data Package (DP) was to be named according to the laboratory, the matrix, and
the version of the data. If the delivered data is a resubmission (Section 4.1.6), then the file name
reflects that the data are of a new version (Table 5). Similar file-naming protocols were developed
for the validators and statisticians.
The DMP states: "Importantly, the laboratory must resubmit BOTH the EDD and the Data
Package with a new version number, even if only one or the other was revised." However, as the
project progressed, multiple submissions and version numbers of EDD/Data Packages were not
updated together as indicated in the DMP due to the unforeseen magnitude of changes. Also,
there were exceptions to the required file-naming conventions, as not all labs were in
compliance.
The Quick Start Guides provided to the participating laboratories, validators and statisticians to
give instructions on file-naming protocols and using the ExaBlue SharePoint site are available in
Appendices B1 - B3 of the Data Management Plan (SERDP/ESTCP 2023, Attachment 4).
Table 5. Laboratory Data File->
aming Protocol Examples
Tracking ID
EDD File Name
Data Package File
Name
Laboratory
Name Code
Matrix
Code
Description
ALPHA_GW_verO
ALPHAGWverO.csv
ALPHA_GW_ver0.pdf
ALPHA
GW
First EDD/DP submitted
by Alpha for
groundwater
ALPHA_GW_verl
ALPHAGWver 1 .csv
ALPHA_GW_verl.pdf
ALPHA
GW
First revision of Alpha
EDD/DP for groundwater
ALPHA_GW_ver2
ALPHA_GW_ver2.csv
ALPHA_GW_verl.pdf
ALPHA
GW
Second revision of Alpha
EDD/DP for groundwater
ETASDverO
ETA SD verO.csv
ETA_SD_ver0.pdf
ETA
SD
First EDD/DP submitted
by ETA for sediment
ETA_SD_verl
ETA SD verl.csv
ETA_SD_verl.pdf
ETA
SD
First revision of ETA
EDD/DP for sediment
18
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4.0 DATA MANAGEMENT PROCESSES AND PROCEDURES
In addition to the ExaBlue SharePoint, a data management system (DMS) was developed to
compile the laboratory EDD data generated for the project, as well as the data validation and
EPA/NAVSEA reviewer results. The overall DMS consists of several elements. This section
provides an overview of the DMS, including the main components of the workflow (Section 4.1.1
- 4.1.5), a description of the rejection criteria and resubmission process (Section 4.1.6), an
overview of the QA/QC procedures applied to laboratory EDD submissions (Section 4.2), and a
description of the database and related tools for processing data (Section 4.3).
4.1 Workflow
An important element for meeting project goals and objectives is the use of a specific, rigorous,
and well-documented workflow for the data generated during the project. This section provides
detailed descriptions of every step of that workflow. At each step, dates of actions and descriptions
of decisions are logged in the Tracking System.
The workflow designed and described in the DMP was modified as the project progressed to
accommodate requests and requirements from the MVS Team. The workflow that reflects the
actual process used during the MLV Study is provided as a flowchart diagram in Figures 3a and
3b. The workflow outlines the sequence of processes that were followed by all team members,
including the Data Management Team (Exa/HGL), the MVS Team, laboratories, the validation
team, and the statistical analysis team (IDA).
One of the key elements of workflow is the multiple stages of data QA/QC by the Data
Management Team, the validators, and the MVS Team. At each stage, the Exa Data Manager
ensured that the review information was captured in the Tracking System so that the MVS Team
could always understand the status of the review procedures.
4.1.1 Receipt of Data Sets
As shown in Figure 3 a, the first component of the workflow is the receipt of data sets, where the
laboratories upload EDDs and Data Packages to the ExaBlue SharePoint site. The Exa team is
responsible for logging the receipt of the submission in the Tracking System.
19
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Receipt of Data Sets—>
Review Laboratory EDD/Data Package Submissions—>
Legend
O
Process step
Decision point
Communication
¦ — — — Back-and-forth
communication
Manual step
End of process
Data archiving
Enter information
in Tracking System
Figure 3a. Workflow for the PFAS Multi-Laboratory Validation Study
20
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CD
X 2
Export
Amended EDD
format and
upload to
Validator folders
Insert Validator
and EPA/NAVY
results to
database
DB QA/QC
procedures;
calculate matrix
Prepare Data
export for
statisticians
Archive
EDD
packages
and
database
<
o
Data Validation — >
Statistical Analyses —>
Data Archiving
Figure 3b. Workflow for the PFAS Multi-Laboratory Validation Study (continued)
21
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4.1.2 Review Laboratory Data Package/EDD Submissions
The next step in the workflow (Figure 3a) is to conduct a detailed review of the data submitted
from the laboratory. This involves two major steps. First, the HGL Project Chemists review the
Data Package for completeness and record the findings in a checklist. If errors or omissions were
found, HGL rejected the Data Package and informed the laboratories that they must address the
issue(s) and resubmit the Data Package. HGL managed the timetable for submissions and this was
logged separately from the Tracking System. If there were no issues with the Data Package, HGL
posted the Data Package and the completed checklist to the Validator folders on the ExaBlue
SharePoint.
The second step of this part of the workflow involves Exa conducting automated QA/QC checks
on the EDD using a customized application. If errors were found, the Exa team completed an Error
Report with the reasons for rejection and sent this to the laboratory, and noted the EDD as rejected
in the Tracking System.
The automated QA/QC checks ensured that the EDDs contained all information required by the
template guidance (SERDP/ESTCP 2023, Attachment 3), and each data field in the EDD was
completed in accordance with those instructions. Section 4.2 provides the specific details on the
EDD checking procedures.
The final step of this component of the workflow was to load the EDD data into the Project
Database.
Details on the rejection criteria and resubmission process are described in Section 4.1.6.
4.1.3 Data Validation
The next component of the workflow is Data Validation and is shown in Figure 3b. Three
independent third-party validators were responsible for the validation of Data Packages and EDDs
in accordance with the study data validation guidelines (SERDP/ESTCP 2023, Attachment 5).
Following review and approval of the EDD and Data Packages by the Data Management Team,
the Exa team generated an Amended EDD file from the database, which included the laboratory
EDD fields, as well as several additional fields incorporated for the validator to populate. The
format of the validator Amended EDD is described in Section 4.3.5 and Appendix C. The
Amended EDD was then posted for the validator in the appropriate folder on the ExaBlue
SharePoint. Amended EDDs were posted for the validators review only after HGL approved the
Data Package.
22
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The validator then conducted the data validation procedures. If the validator found errors in the
laboratory data that require the laboratory to revise the information and data submitted, the
validator informed the MVS Team to determine the course of action to be followed. In some cases
the data validators communicated directly with the laboratories regarding the action(s) needed. If
a laboratory resubmission was warranted, HGL managed the timetable for submissions and this
was logged separately from the Tracking System.
If no errors were found in the laboratory data, the validator completed the data validation
procedures and provided: a data validation report; the associated Amended EDD with the validator
fields populated; a file with evidence of 10% verification; and, the data validation checklist. The
Exa team is responsible for logging the receipt of the submitted files into the Tracking System.
The next step in the workflow is for the SEE Co-Principal Investigator to review the files submitted
by the data validators to ensure it is complete and ready for EPA/NAVSEA review. If issues were
found, SEE communicated this to the data validators and they revised the data validation files and
posted updated files with a revised version number. When this review was complete, SEE was
responsible for updating the Tracking System.
The next step in the workflow is for NAVYSEA and EPA members of the MVS Team to review
the validator results. If the EPA/NAVSEA reviewers disagree with the validator qualifiers, they
enter qualifiers and comments into the Reviewerqualifier and Reviewernotes fields of the
Amended EDD; these changes are communicated to the data validator. If the EPA/NAVSEA
reviewers found issues with the data validation report and associated files, they posted a narrative
of their review findings to the validator folders on the ExaBlue SharePoint. The data validators
then revised the data validation report and posted updated files with a revised version number.
If a resubmission of the data validation report was not warranted, the EPA/NAVSEA reviewers
will upload the revised Amended EDD, with the Reviewer fields populated and a suffix on the file
name indicating the review is complete, as well as a narrative of their review findings (.doc), to
the appropriate folder in the ExaBlue SharePoint. The Exa Database Manager then ran a routine
to link the Project Database to the appropriate file to incorporate validator and validator reviewer
qualifiers and comments.
Exa was responsible for logging the receipt of the files submitted by the data validators and
EPA/NAVSEA reviewers into the Tracking System.
4.1.4 Statistical Analyses
The next step of the workflow is Statistical Analyses and is shown in Figure 3b. Once the database
is complete for a matrix, the Exa Data Manager executed automated database-level checks to
23
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ensure results are consistent for the given matrix to ensure the dataset is ready for statistical
analysis. In addition, the Exa team calculated matrix percent recovery considering the native
concentration in the samples (see Section 4.3.4).
The Exa team then exported the complete dataset for that matrix and posted it to the statistics team
member (IDA) in the Statistics folder in the ExaBlue SharePoint. The format of this Database
Export is described in Section 4.3.5 and Appendix C. Upon completion of the statistical analysis,
IDA uploaded all statistical files to the appropriate ExaBlue SharePoint folder [for each matrix,
this included a report with appendices (pdf), supporting calculations (csv), figures (png), and their
log file (txt) documenting the statistical output].
The Phase 3 ICAL results had a slightly different workflow - these data were compiled from the
laboratory Data Packages by HGL and then provided to Exa for QA/QC review. Subsequently,
Exa uploaded the file to the appropriate folder in the ExaBlue SharePoint (Phase 3 ICAL/To IDA).
After statistical analyses were complete, IDA posted the files with statistical results to the ExaBlue
SharePoint. Note that Phase 3 ICAL data is not stored in the Project Database.
If the statisticians encountered issues with the Database Export provided to them by Exa, the issues
were resolved and a new Database Export was provided with a revised version number.
4.1.5 Data Archiving
The final step of the workflow (Figure 3b) is to archive the data, both during the project and at
project completion. When the review procedures are completed for a given matrix, all of the final
files are moved from the various folders on the ExaBlue SharePoint and compiled in the 'Final
DVR and Data' folder (in the Project Documents top-level folder). This includes the final versions
for: laboratory data package, HGL data package review checklist, data validation reports, validated
EDDs, and EPA/NAVSEA review documents.
The master version of the Project Database will be backed up regularly on Exa's servers. When a
Study report is drafted, a copy of the Project Database is posted on the ExaBlue SharePoint for the
matrices addressed in the Study report, with the date of posting.
At project completion, the Exa team will provide a final report documenting data processing
procedures and a summary of the contents of the final database. This report will take the form of
a Data Management Final Report. This report will summarize components of data management
for the project, including workflow, database structure, data sharing, Tracking System, and the
processes and procedures established for managing the data and conducting QA/QC procedures.
Prior to the completion of the MLV project, Exa will coordinate with team members to assess
options for archiving the data from the project. Some of the long-term data needs that will be
addressed include:
24
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The level of long-term access required by the MVS team, other government
entities, or the public;
Whether to utilize existing government data archive resources and platforms;
Data security level required;
The options for accessible data formats;
The need to retain preliminary versions of files from the laboratories, data
validators and statisticians;
Requirements for metadata, if any; and
Consistency with other SERDP programs and/or databases.
A Data Archive Plan will be produced and delivered as part of this project. Upon acceptance, the
data will be archived to these specifications at the completion of the project and documented in
the Data Management Report.
As a part of project completion, Exa will work with team partners to ensure smooth technology
transition of all work products to the SERDP and the EPA. This delivery will include
documentation that provides information on the data structure, all developed processes, automated
tools and scripts, and related export products. Sufficient documentation will accompany the
archived data to fully describe the source, contents, and structure of the data to ensure future
usability.
The ExaBlue SharePoint has several features as a part of the Microsoft Enterprise environment, to
ensure the information stored on the SharePoint site is always recoverable (Microsoft 2022). For
example, the Microsoft datacenters are geo-distributed to mitigate the impact of a natural disaster
or local power outage; backups are retained for 14 days and can be restored to any point in time.
4.1.6 Rejection and Resubmission Process
There are several steps along the workflow where laboratory EDDs/Data Packages could be
rejected, as shown in Figure 3a and 3b and described in Sections 4.1.1 through 4.1.4. If the
laboratory EDD and/or Data Package includes any inconsistencies with the instructions provided
in their contract, or they did not follow the instructions for populating the EDD template, the
submission was rejected. In addition, the laboratory EDD/Data Package could be rejected if the
data validators found issues with the data that required re-analysis. If the EDD/Data Package was
rejected, the laboratory was informed that they must address the errors and resubmit. HGL
managed the timetable for submissions, and this was logged separately from the Tracking System.
The resubmittal was given a revised version number as described above and shown in Table 5.
The Data Management Plan states that ".. .the Exa data managers will not conduct any editing or
data cleaning procedures to amend the data provided by the laboratories." However, in order to
expedite the flow of EDDs, Exa directly edited minor inconsistencies in the EDDs after receiving
25
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permission from the laboratories. There were also instances where updates were made to the
original database entries at the request of the MVS Team. When edits were made the Exa data
manager added comments in the DM Notes field of the Project Database, to document the
revision.
4.2 EDD QA/QC Procedures
The purpose of this section of the report is to describe specific data quality checking processes and
procedures conducted on the electronic data deliverables (EDDs) from the study laboratories. The
study requires technically sound and legally admissible data; thus the QA/QC procedures
documented in this section are a key element to project success. The data management
methodology is critical to ensure that laboratory analytical data, validation information, and final
statistical calculations are of the highest quality to support and defend the publication of the final
method.
Electronic data from the laboratories are submitted to the MVS Team in a specific electronic data
deliverable (EDD) format, as described in the Study Plan (SERDP/ESTCP 2023; Attachment 3).
The EDD records are imported into a Microsoft® (MS) Access database using automated Visual
Basic for Applications (VBA) code. In addition to the checking routines, there are additional
functions to post-process the data which will be described in Section 4.2.3.
There are three phases of EDD QA/QC in the workflow:
1. Preliminary checks conducted upon import of the EDD;
2. Detailed checks conducted on individual EDDs, prior to submission of the data to the
validators;
3. Database checks on the cumulative Project Database conducted prior to submission to
the data analysis (statistics) team.
The custom application for processing data for the MLV Study was designed and developed by
the Exa team and tested extensively. Testing involved multiple Exa team members running the
procedures on multiple test data sets to identify bugs and inconsistencies. Fixes were then
incorporated into the automated routines.
Each of these phases of QA/QC procedures will be discussed in the following sections.
4.2.1 QA/QC Checks at Import
Upon receipt of data files submitted from the laboratories, the files are logged into the Tracking
System and HGL confirms that the data files (data packages, EDDs, supplemental files) are
appropriately filed on the ExaBlue SharePoint.
26
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Import of the EDDs into the database is the first step of the MLV Study QA/QC tool (Figure 4).
As each EDD is imported, a series of preliminary checks are conducted to ensure that the EDD is
imported properly. This includes checks to ensure all EDD template fields are present and named
properly, and all of the EDD records were imported.
m Main Form
MLV Study
EDD QA/QC tool
Import Data Lab
EDD Template
Import data from the Laboratory EDD Template.
Ensure a relevant path is entered in tbIPath prior to
import.
Remove ImpLabEDDResults
Go To Checking
Routines
Close
Figure 4. Opening Form of the MLV Study EDD QA/QC Tool
27
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4.2.2 Detailed EDD OA OC and Reporting
Once the EDD is imported as a stand-alone table into the database (i.e., not yet appended to the
main database tables), a series of automated QA/QC checks are conducted. These checks
underwent modification as the project progressed, but the description provided below is
comprehensive for the EDDs received for Phase 4 as of the publication of this report.
The EDD QA/QC checks are executed in a sequential order (Routines 1-3, Figure 5). Results of
the checks are written to the QA/QC Report for review and generating feedback to the data
provider (Routine 4).
Data File
MLV
Checking Routines (to be executed in sequence)
Check
Required
Fields and
Relationships
Unique
Records Check
Additional
Checks
Check all required fields have entries and
relationships are maintained.
Check each table to ensure that the primary key
uniquely identifies each record in the table.
A number of additional tests are conducted.
Reports
QA/QC Report
and Detailed
Queries
View the QjVQC report showing the results of
the automated checking routines and the detailed
QAj'QC queries that identify problem records.
Lab_rep must be reviewed and updated
before proceeding.
Figure 5. EDD Checking Routines and Reporting Form
The first routine checks that all required fields have been fully populated. The list of required fields
(Table 6) is drawn from the EDD Instructions and Format (SERDP/ESTCP 2023, Attachment 3,
Table 1).
28
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Table 6. List of Required Fields
Field Name
ANALYSIS
LAB_SAMPLE_ID
S A M P LE_S 1 ZE_U N IT
COMPOUND
MATRIX
SAMPLE_TYPE
CONC_FOUND
METHOD
STUDY_PHASE
CONC_SPIKE
PFAS_ACRONYM
UNIT
DILUTION
SAMPLE_NO
LABJD
SAMPLE_SIZE
In addition, the first routine also checks that relationships between tables are maintained -
specifically the links between the EDD and the standardized SamplelD (from the lu MatrixKey
table) and the standardized compound codes in the lucompound table.
The second routine checks for unique records based on the following fields: LABID,
SAMPLENO, LABSAMPLEID, PF ASACRONYM, DILUTION, and SAMPLETYPE. If
there is more than one record in the EDD with the same combination of these fields, this check
will generate an error message.
The third routine ("Additional Checks" in Figure 5) includes a wide variety of automated QA/QC
checks and summaries, some that require manual review (Table 7). Range checks are conducted
on numeric fields to ensure that the values are "reasonable" (e.g., dilution is checked if is less than
0 or greater than 100, Table 8). Fields that are constrained to valid entries are checked for specific
required content, including exact spelling. These fields are: ANALYSIS, LAB FLAG, MATRIX,
SAMPLE TYPE, STUDY PHASE, UNIT, PFAS ACRONYM, COMPOUND, CAS NO,
ResultType.
29
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Table 7. Detailed List of EDD QA/QC Checks
Type of Check
Description
Completeness
71 results for each sample
All compounds have been reported for all samples
Three sample types for each sample
Review sample type counts
Re-analysis results without the original analysis reported
Missing SAMPLENO
Missing compounds (from all samples)
Units
Consistent units
Correct units
Consistent sample size units
Correct sample size units
SAMPLE SIZE is consistent within EDD and across the matrix
Formatting
No suffixes added to SAMPLE NO
ANALYSIS DATE is in the correct format
PERCENT REC must be a whole number
Numeric entries in number fields
Re-analysis has incremented lab rep
Null and placeholders
Null in CONCFOUND field
Null in CONCSPIKE field
Null in DILUTION field
Null in LOQ field
Null in MDL field
Null in SAMPLE SIZE field
CONC SPIKE = 0 ok
CONC SPIKE not equal to 0 ok
PERCENTREC = null ok
PERCENTREC not null ok
CAS NO can only be null for EIS or NIS
Sample Type/Matrix Coding
MATRIX is coded correctly for blank samples
MATRIX is coded correctly for study samples
MATRIX is coded correctly for QC samples
SAMPLE NO is coded correctly for blank samples
SAMPLE NO is coded correctly for QC samples
SAMPLE NO is coded correctly for study samples
SAMPLE TYPE is coded correctly for NIS and EIS result type
SAMPLE TYPE is coded correctly for TRG result type
SAMPLE TYPE is not EIS or NIS for TRG resultJype (not EIS or NIS)
Mis-coded Normal samples
Mis-coded compounds
Detection Limit / Qualifier
Checks
MDL is not greater than the LOQ
LABFLAG not set to J when CONC FOUND >MDL and MDL and U flagged
MDL can only be null for EIS or NIS
LOQ can only be null for EIS or NIS
LOQ should not be populated for EIS/NIS
MDL should not be populated for EIS/NIS
Calculations
PERCENT REC calculations (>100)
PERCENT REC calculations (>10 and <100)
PERCENT REC calculations (<10)
Review fields that must reported to 3 sig figs
ANALYSIS DATE is after the EXTRACTION DATE
NIS PERCENT REC are not all 100
30
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Table 8. Fields with Range Checks
Field Name
Min
Max
Default
CONC_FOUND
0.0001
1000
REQUIRED
CONC_SPIKE
1
1000
0
DILUTION
0
100
1
PERCENT_REC
0
170
NULL
SAMPLE_SIZE
0.004
1000
REQUIRED
MDL
0.0001
100
LOQ
0.0001
100
In conjunction with developing the data management system, the EDD Template instructions were
reviewed and 'MLVStudySupplementalEDDInstructions' were developed and distributed to
the MLV Study team, to clarify some details of how the EDD Template is expected to be
populated. Many of the QA/QC checks listed in Table 7 are based on the Supplemental EDD
Instructions (2022, unpublished), in particular, the sample coding guidance (Table 9). Narrative
guidance included in the Supplemental EDD Instructions are found in Appendix D.
Table 9. Allowed Code Combinations for Sample No, Matrix, and Sample Type fields
Phase
SAMPLENO
Compound Type
Matrix
Sample type
CONCSPIKE
PERCENTREC
Phase 4
GWA0
Method analytes
GW, SW, etc
NORMAL
0
NULL
Phase 4
GWA0
EIS
GW, SW, etc
EIS
Populated
Populated
Phase 4
GWA0
NIS
GW, SW, etc
NIS
Populated
Populated
Phase 4
MB
Method analytes
RW, OS, RT
BLANK
0
NULL
Phase 4
MB
EIS
RW, OS, RT
EIS
Populated
Populated
Phase 4
MB
NIS
RW, OS, RT
NIS
Populated
Populated
Phase 4
OPR*
Method analytes
QC
OPR
Populated
Populated
Phase 4
OPR*
EIS
QC
EIS
Populated
Populated
Phase 4
OPR*
NIS
QC
NIS
Populated
Populated
Phase 4
LLOPR*
Method analytes
QC
LLOPR
Populated
Populated
Phase 4
LLOPR*
EIS
QC
EIS
Populated
Populated
Phase 4
LLOPR*
NIS
QC
NIS
Populated
Populated
Phase 3 IDC
IPR*
Method analytes
QC
IPR
Populated
Populated
Phase 3 IDC
IPR*
EIS
QC
EIS
Populated
Populated
Phase 3 IDC
IPR*
NIS
QC
NIS
Populated
Populated
Phase 3 IDC
MDLB
Method analytes
RW, OS, RT
MDLB
0
NULL
Phase 3 IDC
MDLB
EIS
RW, OS, RT
EIS
Populated
Populated
Phase 3 IDC
MDLB
NIS
RW, OS, RT
NIS
Populated
Populated
Phase 3 IDC
MDLS*
Method analytes
QC
MDLS
Populated
Populated
Phase 3 IDC
MDLS*
EIS
QC
EIS
Populated
Populated
Phase 3 IDC
MDLS*
NIS
QC
NIS
Populated
Populated
Phase 3 IDC
LOQVER*
Method analytes
QC
LOQVER
Populated
Populated
Phase 3 IDC
LOQVER*
EIS
QC
EIS
Populated
Populated
Phase 3 IDC
LOQVER*
NIS
QC
NIS
Populated
Populated
Phase 3 IDC
MB
Method analytes
RW, OS, RT
BLANK
0
NULL
Phase 3 IDC
MB
EIS
RW, OS, RT
EIS
Populated
Populated
Phase 3 IDC
MB
NIS
RW, OS, RT
NIS
Populated
Populated
*spiked samples
31
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During the execution of the checking routines, an error report with standardized error messages is
automatically generated for the checks that failed. This report can be viewed within the application
by selecting "View Report" (Figure 6) and is also exported to an Excel file to generate the Error
Summary Report that was provided to the laboratories. This auto-generated report was carefully
reviewed by the Exa team and apparent errors were examined prior to sending to laboratories.
Most of the QA/QC checks are associated with detailed queries that provide information on what
the specific problem is (see the bottom part of Figure 6, "Detailed QA/QC Queries"). For the errors
that are applicable to a certain check, the query results are copied into separate worksheets of the
Error Summary report and provided to the laboratories, to assist them in identifying the issue(s) in
the submitted EDD. The standardized error messages and the worksheets containing the detailed
QA/QC query results are cross-referenced with the query name (e.g.,
qry Edd review sample no).
32
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tH QA/QC Reports and Detailed Queries — ~ X
QAi'QC Report
(* jQA/QC Report (results of the automated checking routines) j
r Include details about items that passed' checks
View Report
Detailed GAi'QC Queries
Select query to view problem records. View
Query
1
Review - check for 71 results for each sample
2
Review - all compounds have been reported for all samples
3
Review - 3 sample types for each sample.
4
Review - no suffixes added to SAMPLE_NO
5
Consistent units
6
Correct units
7
MDL is not greater than the LOQ
8
LAB_FLAG not set to J when CONC_FOUND >MDL and
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4.2.3 Final Processing Steps
There are additional data processing steps that occur after the QA/QC routines have been executed
on individual EDDs (Figure 7). Routine 5 populates the spike category (spike cat) field, and
Routine 6 appends the EDD to the main database table (LabEDDResults), with separate steps
to populate the Tracking ID, LABID and SDG fields. Finally, Routine 7 automatically exports an
individual EDD in the Amended EDD format which will be provided to the data validators in Excel
format. Table 10 lists the additional fields that are not in the EDD laboratory template but are
included in the Amended EDD (also see Appendix C).
Fill SpikeCat
Step 1
Populates spike_cat field.
Append to DB
Step 1
Step 2
Step 3
EnterTrackingID and LABJD
Append to database: opens table to enter SDG
information.
Updates database with SDG information.
Export Amended EDD
Step 1
Step 2
Create temp export file based on Tracking ID
Export to Excel. Rename file to the current
Tracking ID, and post to SharePoint site.
Return to
Previous
0
Figure 7. Append to Master EDD Database and Generate Amended EDD Form
34
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Table 10. Additional Fields Included in the Amended EDD
Field
Definition
TrackingID
Tracking ID from Tracking System; incorporated during ETL
procedures
sdgnum
SDG number; incorporated during ETL procedures; extracted from
Lab_Sample_ID
labrep
Lab rep number added to easily filter for re-analysis/dilutions.
ResultTvpe
Code for Result Type. See Valid Value list.
validation_level
Stores information on the level of data validation that has been
completed for the chemistry data. Automatically populated with 'Level
4'.
validator
Code for Data Validator. See Valid Value list.
dvqualifier
Code for Data Validator qualifiers. See Valid Value list.
dvqual ifierreason
Data validation qualifier reason codes.
dv_notes 1
Include comments to distinguish the meaning of the dvqualifier
assignment (e.g., distinguishing the -J qualifier)
dv_notes2
Additional information provided by validator deemed pertinent to their
dv qualifier assignment.
dv_result
Validator recommended result for concentration. If this is provided,
entries must be made in the dv_ResultChange_yn field and
dv_ResultChange_desc fields.
dv_ResultChange_yn
Enter Y or N. Indicates whether the validator made a recommendation
to change the result for concentration.
dv_ResultChange_desc
Description of the reasons for validator recommending a change to the
result for concentration.
Reviewerqualifier
Code for qualifiers applied by NAVY/EPA reviewers of data validation
results. See Valid Value list.
Reviewer_notes
Notes from NAVY/EPA reviewers of data validation results.
35
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4.3 Database and Tools
The purpose of this section is to describe the structure and associated tools for compiling the EDDs
into the Project Database. The Project Database is a relational database using MS Access as the
selected database software. MS Access was chosen due to its common usage and ease of
transforming the data to other formats, as necessary. The master version of the Project Database
will be stored on Exa's local server, ensuring that access to the 'working' database is limited to
the Database Managers. If project participants requested access to the Project Database, they were
given permissions to access a copy of the database posted on the ExaBlue SharePoint.
Alternatively, Exa generated customized data exports for specific purposes, when requested.
The goals of the Project Database and associated toolsets are as follows:
• Maximize the reliability of the database by designing and implementing automated QA/QC
and verification checks;
• Store the data in a structured database with rules that restrict entries for certain fields to
specific valid values, and that follow relational database rules such as primary keys and
inter-table relationships;
• Promote accurate and rapid transfer of data to a variety of export and imports formats for
use by team members (validators, IDA) and reporting to the MVS Team.
The custom application for processing data for the MLV Study was designed and developed by
the Exa team and tested extensively. Testing involved multiple Exa team members running the
procedures on multiple test data sets to identify bugs and inconsistencies. Fixes were then
incorporated into the automated routines.
4.3.1 Database Structure
The structure of the database is provided in Figure 8 as an entity-relationship diagram (ERD),
which describes the tables and fields in the database and how they are related. The field definitions
are compiled in the database dictionary as seen in Appendix C.
The main EDD data table (Lab EDD Resuits) parallels the format of the laboratory EDD
(SERDP/ESTCP 2023, Attachment 3), with EDD field names shown in all capital letters in Figure
8. In addition to the EDD fields, several additional fields were added to the main EDD table, shown
in lower case, including the TrackingID, result type, spike level, and fields to capture results from
the data validators and EPA/NAVSEA (Appendix C).
The valid value tables (dicValidValues, luCompound) were maintained separately but linked to
the main EDD table to enforce entries in fields constrained by valid values, and are shown in
36
-------
Appendices E and F, respectively. Retaining strict valid values enable both the validators and IDA
to accurately filter and analyze the output data.
The database structure includes the lu SpikeLevels table which stores the spike concentrations
reported in the ERA Certificates of Spiking. This facilitates the matrix spike percent recovery
calculations (see Section 4.3.4).
The lu MatrixType table stores the required sample nomenclature, matrix types and spike levels
from the Study Plan (SERDP/ESTCP 2023; Attachment 2). This facilitates the matrix spike
percent recovery calculations (see Section 4.3.4) and QA/QC EDD checks that ensure the Sample
Identifiers used by the laboratories are compliant.
The dicEDD table stores information on whether individual EDDs are Approved or Rejected; it
was decided by the MVS Team to include rejected EDDs in the database, when possible.
As the project progressed, modifications were made to the structure of the Project Database, as
needed.
37
-------
dicValidValues
Table
Field
Field Subcategory
Value
Description
WL_match_a lt_f i e I d
WL_match_alt_code
Validator
dicEDD
Matrix
TrackinglD
Approval_status
DV_Revi ew_f I a gs_a d
Lab_EDD_Results
ie TrackinglD
LA6_ID_Reported
LAB_ID
lab_num
? SAMPLE.NO
H LAB_SAMPLE_ID
ANALĄSIS_DATE
ANALYSIS
? PFAS_ACRONYM
H DILUTION
CONC_FOUND
LAB_FLAG
CONC.SPIKE
PERCENT_REC
MDL
LOQ
UNIT
unit_final
SAM PLE_T RAN SIT 10 N_RAT IC
EXPECT ED_T RAN SIT 10 N_RAT
RRT
SAMPLE.SIZE
SAM PLE_S IZE_U N IT
EXT RACT10 N_D AT E
PERC.MOISTURE
MATRIX
METHOD
STUDY_PHASE
H SAMPLEJYPE
result_type
spike_cat
spike_level
? Iab_rep
validationjevel
validator
dv_qualifier
final_qualifier
dv_qualifier_reason
dv_notes1
dv_notes2
dv result
LU_Compound
8 PFAS.ACRONYM
8 Compound
! CAS.NO
Result_Type
SORT ORDER
LU_Spike_Levels
sort
PFAS.ACRONYM
Matrix
Low_Spike
High_Spike
Unit
lu_MatrixKey
Matrix Type
Requested Name
Description
Matrix Code
Sample Identifier
SamplelD
spike_cat
Rep
Selected
Figure 8. Entity-Relationship Diagram (ERD) for the Project Database
38
-------
4.3.2 Populating Final Result and Final Qualifier
After data are compiled and finalized for a matrix, the Exa team populates the FinalQualifier
field based on these rules:
• Data validators only populate the dvqualifier field if they do not agree with the
laboratory qualifier. If a qualifier should be changed, they enter the new qualifier; if they
want to remove a qualifier, they enter "[null]".
• EPA/NAVSEA only populate the reviewer_qualifier field if they do not agree with the
dv qualifier or LABFLAG qualifier. If a qualifier should be changed, they enter the
new qualifier; if they want to remove a qualifier, they enter "[null]".
• The following logic is used for updating finalqualifier: 1. update with LAB FLAG
entry; 2. Overide with dv_qualifier entry; 3. Override with reviewer_qualifier entry; 4.
Update [null] entries to null.
Similar logic would be employed to populate the FinalResult field (CONCFOUND would be
overridden with the dv result entry, but at the date of publishing this report the data validators
have not included entries in the dv result field. Therefore, finalresult has been updated with the
CONC FOUND entry.
4.3.3 QA/QC Checks on Master EDD Database
In addition to the checks applied to individual EDDs, there are additional QA/QC checking
routines that were developed to apply to the entire database. The purpose of this operation is to
review the data across Study Phases, laboratories and matrices to ensure that there are no internal
inconsistencies or other issues that arise as the data are compiled. These checks identify differences
in how the data are reported from different laboratories and/or validators and ensure consistency
in the data exports provided to the project statisticians. It is good practice to incorporate
redundancy in the QA/QC procedures to ensure that issues are not overlooked.
Examples of these database-wide queries include:
• Min-max checks on number fields
• Dictionary checks
• Unique record check
• Date range checks
• Consistent unit checks
• Review of summary of lab flag, lab qual, dv qualifier, reviewer qual, final qualifier
• Review of summary of conc found, dv result, final result, dv_ResultChange_yn,
dvResultChangedesc
39
-------
4.3.4 Matrix Spike Percent Recovery Calculation Procedures
After data are compiled and finalized for a matrix, the Exa team calculates matrix percent recovery
considering the native concentration in the samples. This calculation applies to target compounds
in matrix samples (i.e., it did not apply to QA/QC samples). The general calculation is:
Final result Spiked Sample/[spike level + Final result Unspiked sample]
There were specific data handling options developed by the MVS Team for certain scenarios and
the specific procedures used for calculating matrix percent recovery are provided in Table 11.
Table 11. Data Rules for Calculating Percent Matrix Spike Recoveries
Case
Un-spiked Sample
Spiked Sample
Calculation of MS Spike Recovery
Data for Statistical Analyses
1
detected
detected
Base case. Use Equation 1
All resultant values used
2
not detected
detected
(Final Result Spiked Sample [ ] / (Spike
[] Added])* 100
All resultant values used
3
not detected/X-flagged
not detected/X-
flagged
when spiked sample is X or U, it is
excluded, and %recovery is not
calculated
No % recovery value for that sample and
analyte pair
4
not detected/X-flagged
detected
(Final Result Spiked Sample [ ] / (Spike
[] Added])* 100
All resultant values used
5
detected/X-flagged
detected
(Final Result Spiked Sample [ ] / (Spike
[] Added])* 100
Values were reviewed on a case-by-case basis
for inclusion or rejection.
6
detected [ ] > spike
level
detected
Not calculated
No % recovery value for that sample and
analyte pair
7
detected
< Un-spiked [ ]
Calculated, but results in negative %
recovery.
Negative % Recovery values excluded from
statistical analyses
Notes: [ ] - reported analyte concentration; X-flagged data are excluded from calculations and excluded from statistical analyses.
4.3.5 Import and Export File Structures
The primary import structure for the Project Database is the laboratory EDD, provided as
Attachment 3 in the Study Plan (SERDP/ESTCP 2023).
There are several other import and export routines that were used in the overall workflow of the
MLV Study using queries in the database:
• Export of the Amended EDD for the validators - Includes the laboratory EDD results, and
additional fields to be populated by the validator when reviewing the results provided by
one laboratory for one matrix.
• Import of the Amended EDD, with validation fields populated - Used to update the Project
Database with the results from the validator and the EPA/NAVSEA reviewers.
• Database Export for the statistics team - Used to create a dataset for a single matrix, or a
combination of matrices, for IDA in generating statistics and analysis for the project. This
40
-------
database export includes final results and qualifiers, considering laboratory, data validator
and data validator reviewer results.
• EDD archiving - Procedures were developed to extract and archive EDDs loaded into the
Project Database and subsequently rejected (i.e., EDDs that passed initial QA/QC checks
but were then rejected by the data validators; these EDDs were replaced by re-
submissions).
The output formats provided to the validators and IDA are available in Appendix C (see columns
named 'Include in Amended EDD for DV' and 'Include in Exports for IDA', respectively).
41
-------
5.0 REFERENCES
Microsoft. 2022. How SharePoint and OneDrive safeguard your data in the cloud.
https://docs.microsoft.com/en-us/sharepoint/safeguarding-vour-data
SERDP/ESTCP PFAS Method Validation Study Team. 2023. Study Plan for Multi-Laboratory
Validation of Draft EPA Method 1633 - PFAS in Aqueous, Solid, Biosolids, and Tissue
Samples by LC- MS/MS. Prepared for Program Manager for Environmental Restoration,
Strategic Environmental Research and Development Program (SERDP).
Willey, J., R. Anderson, A. Hanley, M. Mills, C. Hamilton, T. Thompson, and A. Leeson. 2021.
Report on the Single-Laboratory Validation of PFAS by Isotope Dilution LC-MS/MS.
Strategic Environmental Research and Development Program (SERDP) Project ER19-
1409. https://serdp-estcp.org/content/download/54966/539631/file/Single-
Laboratorv%20Validation%20Studv%20Report.pdf
42
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Appendix A - Description of the File Tracking System
tuackim;
WOUKSIII.IT
tuackim; i ir.i.i)
YY 1 kl.l
tuackim; i h i d i)i:scuirno\
GENERAL
Trucking II)
Root lile name
Project Phase
Project Phase. See 'ValidValues'
EDD File Name
EDD File name
Data Package File Name
Data Package File Name
Laboratory Name
Yes
Laboratory Name. See 'ValidValues'
Matrix
Yes
Matrix. See 'ValidValues'
Notes
Notes regarding submitted files
Log Date
Date the reciept of files was logged into the Tracking System
LABORATORY
EDD/DP Due Date
Due date for the Lab EDD/Data Package (mm/dd/yyyy)
EDD/DP Date Received
Date Lab EDD/Data Package received (mm/dd/yyyy; uploaded to
Sharepoint)
E1GL Reviewer
Initials of HGL staff conducting the Data Package review
Date HGL Review Complete
Date HGL review complete (mm/dd/yyyy)
EDD Rejected or Approved -
Yes
Indicate whether EDD/Data Package was rejected by HGL. See
HGL
'ValidValues'
Summary of Errors - E1GL
Brief summary of issues found during HGL Data Package review
Exa Reviewer
Initials of Exa staff conducting the automated EDD review
Date Exa Review Complete
Date Exa review complete (mm/dd/yyyy)
EDD Rejected or Approved - Exa
Yes
Indicate whether EDD/Data Package was rejected by Exa. See
'ValidValues'
Summary of Errors - Exa
Brief summary of issues found during Exa EDD review
Date Data Package to DV
Date the Data Package was posted to the Validator folder
(mm/dd/yyyy).
Date Amended EDD to DV
Date the Amended EDD was posted to the Validator folder
(mm/dd/yyyy).
VALIDATOR
Data Validator
Yes
Data Validator. See 'ValidValues'.
DP version reviewed
Current version number of the Data Package provided to the data
validator for review.
Amended EDD version reviewed
Current version number of the Amended EDD provided to the data
validator for review.
Date DV Report/Files Received
Date of receipt for the current data validator report/files (mm/dd/yyyy).
DV Amended EDD version
Current version number of the Amended EDD with validator fields
populated (posted by the data validator).
DV Report version
Current version number of the data validator report (posted by the data
validator).
DV Verification version
Current version number of the Verification file (posted by the data
validator).
DV Checklist version
Current version number of the Checklist (posted by the data validator).
EDD Rejected or Approved - DV
Yes
Indicate whether EDD/Data Package was rejected by the Data Validator.
See 'ValidValues'
Notes
Notes regarding submitted files
Date EPA/NAVY Files Received
Date of receipt for the current review files posted by EPA/NAVY
reviewers (mm/dd/yyyy).
Acronyms: DB - Project Database
DP - Data Package
DV - Data Validator
EDD - Electronic Data Deliverable
27
-------
Appendix B - File Tracking System Valid Values List
WorksluTl
Held
Y;ili(l Y.due
('ode
\';ili(l Y;due ( ode Description
GENERAL
Laboratory Name
AI.l'IIA
Alpha Analytical
GENERAL
Laboratory Name
BATTELLE
Battelle
GENERAL
Laboratory Name
CALEPA
CalEPA DTSC
GENERAL
Laboratory Name
ELLET
Eurofins Lancaster Labs
GENERAL
Laboratory Name
ETA
ETA, Sacramento
GENERAL
Laboratory Name
GEL
GEL Laboratories
GENERAL
Laboratory Name
MDH
Maryland Department of Health
GENERAL
Laboratory Name
PACE
GCAL/Pace
GENERAL
Laboratory Name
SGSNA
SGS North America
GENERAL
Laboratory Name
VISTA
Vista Analytical
GENERAL
Matrix
GW
Groundwater
GENERAL
Matrix
SW
Surface water
GENERAL
Matrix
SD
Sediment
GENERAL
Matrix
ss
Soil
GENERAL
Matrix
TS
Tissue
GENERAL
Matrix
WW
Wastewater
GENERAL
Matrix
LC
Landfill Leachate
GENERAL
Matrix
BS
Biosolids
GENERAL
Project Phase
Phase 3 - ICAL
Initial Calibration
GENERAL
Project Phase
Phase 3 - IDC
Initial Demonstration of Capabilities (IDC)
GENERAL
Project Phase
Phase 4.4.1
GW, SW, and WW matrices
GENERAL
Project Phase
Phase 4.4.2
SS and SD matrices
GENERAL
Project Phase
Phase 4.4.3
Tissue matrices
GENERAL
Project Phase
Phase 4.4.4
LC and BS matrices
LABORATORY
EDD Rejected or Approved - HGL
Approved
Passed review
LABORATORY
EDD Rejected or Approved - HGL
Rejected
Did not pass review
LABORATORY
EDD Rejected or Approved - HGL
NA
Not applicable (not reviewed)
LABORATORY
EDD Rejected or Approved - HGL
To Validator
Bypassed review and went straight to validator.
LABORATORY
EDD Rejected or Approved - HGL
Re-submitting
Re-submission from the lab expected
LABORATORY
EDD Rejected or Approved - HGL
Pending
Lab has submitted a data package and it's
pending review
LABORATORY
EDD Rejected or Approved - HGL
Not Submitted
Lab hasn't submitted
LABORATORY
EDD Rejected or Approved - Exa
Approved
Passed review
LABORATORY
EDD Rejected or Approved - Exa
Rejected
Did not pass review
LABORATORY
EDD Rejected or Approved - Exa
NA
Not applicable (not reviewed)
LABORATORY
EDD Rejected or Approved - Exa
Re-submitting
Re-submission from the lab expected
LABORATORY
EDD Rejected or Approved - Exa
Pending
Lab has submitted an EDD and it's pending
review
LABORATORY
EDD Rejected or Approved - Exa
Not submitted
Lab hasn't submitted
VALIDATOR
Data Validator
CHEMVAL
ChemVal
VALIDATOR
Data Validator
PYRON
Pyron Environmental
VALIDATOR
Data Validator
JACOBS
Jacobs Engineering
VALIDATOR
EDD Rejected or Approved - DV
Approved
Approved as is (no DV input)
VALIDATOR
EDD Rejected or Approved - DV
Revised
Approved with DV input added
VALIDATOR
EDD Rejected or Approved - DV
Rejected
Did not pass review
VALIDATOR
EDD Rejected or Approved - DV
NA
Not applicable (not reviewed)
28
-------
Appendix C - Project Database - Database Dictionary
1 :i lilt-
Data l\lu-
Definition anil ( 'ommeiit>>
Di nil
Innii
I.DI)
\ aliil
Value
Iit-Id
Uci|iiiml
ll.ld
Default
\ .iliit-
I'liina n
Ur\
Inclihli- in
Amended
I I)|) lor
HHNI
Ini'luile in
|-'.\porl* lor
IDA
Lab
EDD
Results
TrackingID
text
Tracking ID from Tracking System; incorporated during ETL
procedures
No
No
Yes
X
Yes
No
Lab
EDD
Results
Lab ID Reported
text
LAB ID reported by the laboratories in the EDD
Yes
No
Yes
No
No
Lab
EDD
Results
I.AIS ID
text
^Laboratory Name. See Valid Value list.
No ]
Yes
Yes
X
Yes
No
Lab
EDD
Results
lab num
number
Lab ID code, to keep laboratories anonymous. See Valid Value list.
No |
Yes
Yes
No
Yes
Lab
EDD
Results
:sdg num
text
SDG number; incorporated during ETL procedures; extracted from
Lab Sample ID
No
No
No
Yes
Yes
Lab
EDD
Results
SAMPLENO
text
For samples, these are the sample identification names (IDs) from the
Chain of Custody. The Sample No is the same, regardless of whether
or not the sample is diluted or reanalyzed. For preparation batch QC,
these are "MB" for the Method Blank, "OPR" for the OPR, and
"LLOPR" for the LLOPR. For IDOC samples, "IPR" for the IPR
samples, "MDLB" for the MDLb samples "MDLS" for the MDLs
samples, and "LOQVER" for the LOQVER samples.
Yes
No
Yes
X
Yes
Yes
Lab
EDD
Results
[LAB S AMPLE ID
text
The ID the laboratory assigns to the sample (which identifies the
sample on the associated data files and reports).
IFor samples that need to be re-analyzed for issues other than dilution,
; attach the following identifiers to the end of the lab sample identifier
^without a space between them (e.g., 02082022-01R):
;"R" for analytes, EISs & NISs reported from first re-analysis not due to
! dilution
;"R1" for analytes, EISs & NISs reported from second re-analysis not
:due to dilution
;"R2" for analytes, EISs & NISs reported from second re-analysis not
Idue to dilution
;If more re-analyses not due to dilution are needed to be reported
:beyond three for a sample, continue on with the numbering (e.g., R3,
R l. R5. etc.).
Yes
No
f Yes
X
Yes
Yes
Lab
EDD
Results
ANALYSISDATE
short date;
; mm/dd/yyyy
[Use format mm/dd/yyyy (e.g. 11/20/2019) - do not include time stamp.
Yes
No
Yes
Yes
No
Lab
EDD
Results
ANALYSIS
text
Fill in "PFAS". See Valid Value list.
Yes
Yes
Yes
PFAS
Yes
No
Lab
EDD
Results
PFAS_ ACRONYM
text
Use acronyms included in the example EDD. See Valid Value list.
Yes
Yes
Yes
X
Yes
Yes
Lab
EDD
Results
lab rep
text
l ab replicate identifier
" No j
No
Yes
1
Yes
Yes
15
-------
Appendix C - Project Database - Database Dictionary
Table
Field
Data type
Definition and Comments
Direct
from
EDD
Valid
Value
Field
Required
field
Default
Value
Primary
Key
Include in
Amended
EDD for
DV
Include in
Exports for
IDA
Lab EDD
Results
DILUTION
number
Dilution made post extraction (e.g., extract diluted 1:10 is entered as
"10"). If analyzed without dilution, enter "1".
Yes
No
Yes
1
X
Yes
Yes
Lab EDD
Results
LABFLAG
text
Laboratory qualifiers. See Valid Value list.
Yes
Yes
No
Yes
No
Lab EDD
Results
CONCFOUND
number
Enter numeric quantitative result value only. Report to three significant
figures. Do NOT enter any text string strings or symbols (e.g., "ND",
For analytes that are not detected, the laboratory's sample
specific MDL (i.e. with extract dilution factor, sample volume/weight
and final volume taken into account) is entered. Solids are reported on
a dry-weight basis. Tissues are reported on a wet-weight basis. Report
result units in "Unit" field, consistent for all sample fields.
Yes
No
Yes
Yes
No
Lab EDD
Results
CONCSPIKE
number
For unspiked samples enter "0" for method analytes. For spiked
samples, enter the spike concentration representing the estimated
concentration in the final extract (i.e. with extract dilution factor,
sample volume/weight and final volume taken into account). Solids are
reported on a dry-weight basis. Tissues are reported on a wet-weight
basis. For EIS and NIS, enter the spike concentration representing the
concentration in the final extract in units consistent with sample result
units. The reporting units for this project are parts per trillion (ppt) or
nanograms per liter (ng/L) for aqueous samples and parts per billion
micrograms per kilogram ((.ig/kg) for solid samples. Report to 3
significant figures.
Yes
No
Yes
Yes
Yes
Lab EDD
Results
PERCENTREC
number
For unspiked samples, leave blank. No text should be included in this
field (e.g. N/A). For spiked samples (OPR LLOPR, MDLs and
LOQVER), enter the spike percentage recovery as a whole number
(e.g., 95 versus 0.95). Do NOT include "%" symbol. For EIS and NIS
recoveries, enter the spike % recovery as a whole number (e.g., 95
versus 0.95). Report to 3 significant figures. Do NOT include "%".
Yes
No
No
Yes
Yes
Lab EDD
Results
MDL
number
Method Detection Limit. Enter the sample specific MDL (i.e. with
extract dilution factor, sample volume/weight and final volume taken
into account). The reporting units for this project are parts per trillion
(ppt) or nanograms per liter (ng/L) for aqueous samples and parts per
billion micrograms per kilogram ((.ig/kg) for solid samples. Report to 3
significant figures.
Yes
No
No
-9
Yes
Yes
15
-------
Appendix C - Project Database - Database Dictionary
Table
Field
Data type
Definition and Comments
Direct
from
EDD
Valid
Value
Field
Required
field
Default
Value
Primary
Key
Include in
Amended
EDD for
DV
Include in
Exports for
IDA
Lab EDD
Results
LOQ
number
Limit of Quantitation. Enter the sample specific LOQ (i.e. with extract
dilution factor, sample volume/weight and final volume taken into
account). Report to 3 significant figures. The reporting units for this
project are parts per trillion (ppt) or nanograms per liter (ng/L) for
aqueous samples and parts per billion micrograms per kilogram ((.ig/kg)
for solid samples. Report to 3 significant figures.
Yes
No
No
-9
Yes
Yes
Lab EDD
Results
UNIT
text
The reporting units must be consistent for the sample record including
Cone Found, MDL, LOQ etc. The reporting units for this project are
parts per trillion (ppt) or nanograms per liter (ng/L) for aqueous
samples and parts per billion micrograms per kilogram ((.ig/kg) for solid
samples. Ensure that all values for the sample record are reported in the
same units. See Valid Value list.
Yes
Yes
Yes
No
No
Lab EDD
Results
unit final
text
The reporting unit, standardized
No
Yes
Yes
Yes
Yes
Lab EDD
Results
SAMPLE_
TRAN SITIONRATIO
text
Enter the calculated Transition Ratio (Quant Ion Area/Conf Ion Area)
for each analyte in the sample. Report to 3 significant figures. For
analytes this does not apply to (PFBA, PFPeA, NMeFOSE, NEtFOSE,
PFMPA, and PFMBA), leave this field blank. No text should be
included in this field (e.g. N/A).
Yes
No
No
Yes
No
Lab EDD
Results
EXPECTED_
TRAN SITIONRATIO
text
Enter the expected Transition Ratio (Quant Ion Area/Conf Ion Area)
for each analyte per the method. Report to three significant figures. For
analytes this does not apply to (PFBA, PFPeA, NMeFOSE, NEtFOSE,
PFMPA, and PFMBA), leave this field blank. No text should be
included in this field (e.g., N/A).
Yes
No
No
Yes
No
Lab EDD
Results
RRT
text
Enter relative retention time
Yes
No
No
Yes
No
Lab EDD
Results
SAMPLESIZE
number
Enter volume (aqueous samples) or weight (solid samples) of sample
extracted (in liters for aqueous samples, in kilograms for solids).
Yes
No
Yes
Yes
No
Lab EDD
Results
SAMPLESIZEUNIT
text
Will be liters (L) for aqueous samples or kilograms (Kg) for solid
samples
Yes
No
Yes
Yes
No
Lab EDD
Results
EXTRACTIONDATE
short date;
mm/dd/yyyy
Use format mm/dd/yyyy (e.g. 11/20/2019) - do not include time stamp.
Yes
No
Yes
Yes
No
Lab EDD
Results
PERCMOISTURE
number
Percent moisture in solid samples only. Enter the percent moisture as a
whole number (e.g., 73 versus 0.73). Do NOT include "%" symbol.
Yes
No
No
Yes
No
Lab EDD
Results
MATRIX
text
Matrix analyzed. See Valid values list.
Yes
Yes
Yes
Yes
Yes
15
-------
Appendix C - Project Database - Database Dictionary
1 :i lilt-
Data l\lu-
Definition anil ( 'oniuicut>>
Di nil
Innii
I.DI)
\ aliil
Value
Iit-Id
Uci|iiiml Default
Ill-Id Value
I'liina n
Ur\
Include ill
Amended
COD for
HHNI
Include
|-'.\porl*
IDA
Lab
EDD
Results
METHOD
text
Laboratory SOP Name in format of "name(space)revision number"
Yes
No
Yes
Yes
No
Lab
EDD
Results
jSTUDYPHASE
text
(Multi-Lab Validation Study Phase. See Valid Value list.
Yes
Yes
Yes
Yes
No
Lab
EDD
Results
] SAMPLE TYPE
text
(See Valid Value list.
Yes
Yes
Yes
X
Yes
Yes
Lab
EDD
Results
(result type
text
(Code for Result Type. See Valid Value list.
' No
Yes
Yes
Yes
Yes
Lab
EDD
Results
spike cat
text
(Code for Spike Category. See Valid Value list.
" No
Yes
Yes
Yes
Yes
Lab
EDD
Results
validation level
text
Stores information on the level of data validation that has been
completed for the chemistry data.
No ]
No
Yes ( Level 4
Yes
No
Lab
EDD
Results
(validator
text
(Code for Data Validator. See Valid Value list.
No
Yes
Yes
Yes
No
Lab
EDD
Results
(dv qualifier
text
(Code for Data Validator qualifiers. See Valid Value list.
No
Yes
r No r
Yes
No
Lab
EDD
Results
dv qualifier reason
text
Data validation qualifier reason codes.
" No (
No
No
Yes
No
Lab
EDD
Results
dv notes 1
text
(Include comments to distinguish the meaning of the dv qualifier
(assignment (e.g., distinguishing the -J qualifier)
"" No
No
No r
Yes
No
Lab
EDD
Results
dv notes2
text
(Additional information provided by validator deemed pertinent to their
(dv qualifier assignment.
" No (
No
I" No
Yes
No
Lab
EDD
Results
d\ result
number
( Validator recommended result for concentration. If this is provided,
(entries must be made in the dv ResultChange yn field and
(dv ResultChange desc fields.
No j
No
No
Yes
No
Lab
EDD
Results
(dv ResultChange yn
Logical
(Enter Y or N. Indicates whether the validator made a recommendation
(to change the result for concentration.
No ;
No
Yes
Yes
No
Lab
EDD
Results
(dv ResultChange desc
text
Description of the reasons for validator recommending a change to the
result for concentration.
No !
No
r No r
Yes
No
Lab
EDD
Results
Reviewer qualifier
text
Code for qualifiers applied by NAVY/EPA reviewers of data
validation results. See Valid Value list.
No j
Yes
r No
Yes
No
Lab
EDD
Results
(Reviewer notes
text
Notes from NAVY/EPA reviewers of data validation results.
No
No
f No
Yes
No
Lab
EDD
Results
( final qualifier
text
iCode for Final Qualifier. See Valid Value list.
No |
Yes
r No r
No
Yes
Lab
EDD
Results
final result
number
(Final result for concentration. Combines CONC FOUND and
(validator result fields.
No
No
Yes
No
Yes
Lab
EDD
Results
lab rep
text
Data manager assigned. Laboratory replicate number; to assist with
completeness and duplicate checks.
No ;
No
Yes
Yes
No
Lab
EDD
Results
(sample rep
text
(Data manager assigned. From lu MatrixType.Rep field; to assist with
(spike percent rec calculation
" No
No
r No r
No
No
Lab
EDD
Results
(sample root
text
Data manager assigned. Sample NO without the Reg suffix; to assist
with spike percent rec calculation
No !
No
No
No
No
Lab
EDD
Results
(spike level
number
Data manager assigned. From lu SpikeLevel table; to assist with
spike percent rec calculation
No
No
r No r
No
Yes
15
-------
Appendix C - Project Database - Database Dictionary
Direct Valid Include in jncju(je jn
Table Field Datatype Definition and Comments from Value Re?Z le''Ult P™y Exports for
EDO Field fidd Value Key EDDDvf°r IDA
Lab EDD Results
cone minus native
spike percent rec
spk pet rec DNC
CONCFOUNDval
LOQ val
MDL val
LABSAMPLEIDclean
qaqc dup
DM notes
DM notes2
EditDate
number
Data manager calculated. Interim value in spike percent rec
calculation
No
No
No
No
Yes
Lab EDD Results
number
Data manager calculated. Matrix spike percent recovery.
No
No
No
No
Yes
Lab EDD Results
text
Data manager assigned. Determination of Calculate/DNC (do not
calculate)for spike percent rec calculation
No
No
No
No
Yes
Lab EDD Results
text
Data manager assigned. CONC FOUND as a value; to assist with
database-wide QAQC checks.
No
No
No
No
No
Lab EDD Results
text
Data manager assigned. LOQ as a value; to assist with database-wide
QAQC checks.
No
No
No
No
No
Lab EDD Results
text
Data manager assigned. MDL as a value; to assist with database-wide
QAQC checks.
No
No
No
No
No
Lab EDD Results
text
Data manager assigned. Standardized LAB SAMPLE ID to remove re-
analysis suffixes; to assist with completeness and duplicate checks.
No
No
Yes
No
Yes
Lab EDD Results
text
Data manager assigned. Identifies LLOPR OPR and MB double-duty
samples and exclude one of the results for the 'all in' database exports.
No
No
No
No
No
Lab EDD Results
text
Data manager notes.
No
No
No
No
No
Lab EDD Results
text
Data manager notes - 2.
No
No
No
No
No
Lab EDD Results
text
Date of append to Lab EDD Results table.
No
No
Yes
No
No
dicValidValues
Table
text
Valid value table name.
No
No
Yes
No
No
dicValidValues
Field
text
Valid value field name.
No
No
Yes
No
No
dicValidValues
Value
text
Acceptable valid value codes.
No
No
Yes
No
No
dicValidValues
Description
text
Description of valid value codes, if necessary
No
No
Yes
No
No
dicValidValues
VVL match alt field
text
Related valid value field name.
No
No
No
No
No
dicValidValues
VVL match alt code
text
Matching valid value code.
No
No
No
No
No
dicValidValues
Validator
text
Data validator assoicated with each LAB ID CODE
No
No
No
No
No
LU Compound
SORT ORDER
number
Sort order to apply to data summary tables.
No
No
Yes
No
No
LU Compound
PFAS_ ACRONYM
text
Use acronyms included in the example EDD. See Valid Value list.
No
Yes
Yes
X
No
No
LU Compound
COMPOUND
text
Use the names included in the example EDD. Method analytes, and EIS
and NIS compounds must be reported for each sample. See Valid Value
list.
Yes
Yes
Yes
Yes
Yes
LU Compound
CAS NO
text
Chemical Abstract Service Registration Number
Yes
Yes
Yes
Yes
Yes
LU Compound
result type
text
Code for Result Type. See Valid Value list.
No
Yes
Yes
No
No
LU Spike Levels
PFAS_ ACRONYM
text
Use acronyms included in the example EDD. See Valid Value list.
No
Yes
Yes
X
No
No
LU Spike Levels
Matrix
text
Name of the matrix. See Valid Value list.
No
Yes
Yes
X
No
No
LU Spike Levels
Low Spike
number
Low spike concentration
No
No
Yes
No
No
LU Spike Levels
High Spike
number
High spike concentration
No
No
Yes
No
No
15
-------
Appendix C - Project Database - Database Dictionary
1 able
Data l\lu-
Definition anil ( 'oniuicut>>
Di reel
Innii
inn
\ aliil
Value
Held
Uci|iiiml
ll.ld
Default
\ .iliie
I'liina n
l\e\
Include ill
Amended
COD for
HHNI
Include in
lAporl* lor
IDA
LU Spike Levels
Unit
text
Unit of spike concentration
No
No
Yes
No
No
lu MatrixKey
Matrix Type
text
Matrix (full name)
No !
No
Yes
No
No
lu MatrixKey
¦ Requested Name
text
Descriptive name of sample
: No
No
Yes
No
No
lu MatrixKey
: Description
text
¦Description of sample
No '
No
Yes
No
No
lu MatrixKey
Matrix Code
text
Matrix (code)
: No
No
Yes
No
No
lu MatrixKey
Sample Identifier
text
Sample identifier (middle component of SamplelD)
No '
No
Yes
No
No
lu MatrixKey
SamplelD
text
SamplelD (EDD SAMPLE NO must match to this code)
No
No
Yes
No
No
lu MatrixKey
spike cat
text
Spike category (low, high, etc)
No
No
Yes
No
No
lu MatrixKey
¦ Rep
text
Sample replicate number (last component of SamplelD)
No
No
Yes
No
No
lu MatrixKey
: Selected
text
Indicates if sample was selected for use in the study
No
No
Yes
No
No
Note: The Required Fields may be revised during database development; maximum field lengths will be incorporated into the database structure during development.
15
-------
ADDendix D - Supplemental guidance for correctly DODulatine the EDD Template
Item
Guidance
1
If possible, include all results in one worksheet.
2
We will be running QA/QC routines on the EDDs to ensure they are populated correctly. These will be delivered to you in an Excel file (e.g.,
L ABN AME_RW_verO_EDD_Error_Summary. xlsx).
If you have questions/issues regarding the Error Summary report, please incorporate comments directly into the Excel file and send it back to us for review
(via SharePoint).
3
Instructions for reporting CONCFOUND for NIS compounds:
1. Option 1: Report NIS Mass in CONC FOUND, and in the accompanying report provide example calculation and point to where the data in the
numerator (e.g., field sample) and the denominator (e.g. CCV) are found.
2. Option2: Complete the EDDs with the NIS percent recoveries based on areas (i.e., no mass reported). CONC FOUND does not need to be populated.
a. If Option 2 is selected then
i. In the report provide the formula and example calculations for one sample per batch
ii. Point to where those areas values are found in their data packages (i.e., ensure they have reported the NIS area for the field (target) sample and
the comparative area from either the mid-point of the ICAL, CCV, or equivalent.
4
Instructions for populating EDD when a single sample is serving the purpose of the MDLB and MB samples:
1. Copy the results and code the SAMPLE NO field as 'MDLB' for one set of results, and 'MB' for the other set of results.
2. Ensure that the case narrative clearly identifies that the blank sample was used for multiple purposes.
5
Ensure that B flags are applied as indicated by the instructions:
"For analytes that were detected in the associated MB of a sample that exceeded Vi LOQ or is at a concentration greater than 1/1 Oth the concentration in
the sample, whichever is greatest. The MB must also be flagged with a "B" for all concentrations greater than 'A the LOQ."
If the CONC FOUND is between the MDL and LOO AND it is at a concentration greater than 1/2 LOO. the flag should be BJ or JB.
6
Although the instructions for the CONC FOUND field indicate "For analytes that are not detected, the laboratory's sample specific MDL", the exceptions
are for the following sample types, where CONC FOUND can be less than the MDL:
MDLS
LOQVER
Blanks (MB and MDLB)
7
For instances where there are re-analysis not due to dilution, all results must be reported in the EDD (i.e., the original analysis and all subseqent re-analysis).
35
-------
ADDendix D - SuDDlemental guidance for correctly DODulatine the EDD Template
8
The Sample Coding spreadsheet lists the mandatory batch QC samples that are required for Phase 3 and Phase 4 submittals. All mandatory batch QC
samples must be present in the EDD submittals.
9
Do not add suffixes to SAMPLE NO (e.g., IPR1, MLDB 2) - LAB SAMPLE ID will differentiate samples.
10
Fields that must be reported to 3 significant figures:
CONC FOUND
CONC SPIKE
PERCENT REC (DOES need to be reported to 3 sig figs; report as a whole number (95.1), not a fraction (0.951)
MDL
LOQ
SAMPLE TRANSITION RATIO
EXPECTED TRANSITION RATIO
Note that the results in these fields must be rounded appropriately to 3 significant figures. Changing the display for the number of decimal places is not
sufficient.
11
Solids are reported on a dry-weight basis. Tissues are reported on a wet-weight basis.
12
UNIT field must be consistent across all samples.
13
The reporting units for this project are parts per trillion (ppt) or nanograms per liter (ng/L) for aqueous samples and parts per billion micrograms per
kilogram (ng/kg) for solid samples.
14
Do not include text in number fiels (e.g. N/A, %, ND, <).
15
Percent recovery must be reported in the EDD for IPR samples.
36
-------
Appendix E - Project Database - Valid Value Codes and Descriptions
YYI.Iuld
YalidYalue
YY l)i'v(i i|>linii
YYI. mahli
all Ik-Id
YYI.
inalcli all
code
Yalidalor
LAB ID CODE
ALPHA
Alpha Analytical
lab num
3
JACOBS
LAB ID CODE
BATTELLE
Battelle
lab num
6
JACOBS
LAB ID CODE
CALEPA
CalEPA DTSC
lab num
2
PYRON
LAB ID CODE
ELLET
Eurofins Lancaster Labs
lab num
10
JACOBS
LAB ID CODE
ETA
ETA, Sacramento
lab num
1
PYRON
LAB ID CODE
GEL
GEL Laboratories
lab num
8
JACOBS
LAB ID CODE
MDH
Maryland Department of Health
lab num
5
JACOBS
LAB ID CODE
PACE
GCAL/Pace
lab num
9
JACOBS
LAB ID CODE
SGSNA
SGS North America
lab num
7
PYRON
LAB ID CODE
VISTA
Vista Analytical
lab num
4
PYRON
MATRIX
BS
Biosolids
MATRIX
GW
Groundwater
MATRIX
LC
Landfill Leachate
MATRIX
OS
Ottawa sand for all soil, sediment, and biosolid MBs
MATRIX
QC
Quality Control Sample
MATRIX
RT
Reference Tissue for tissue MBs
MATRIX
RW
Reagent water for all aqueous MBs
MATRIX
SD
Sediment
MATRIX
ss
Soil
MATRIX
sw
Surface water
MATRIX
TS
Tissue
MATRIX
WW
Wastewater
result type
EIS
Extracted Internal Standard
result type
NIS
Non-Extracted Internal Standard
result type
TRG
Target analyte
SAMPLE TYPE
BLANK
method analytes in MBs
SAMPLE TYPE
EIS
EIS in all samples
SAMPLE TYPE
IPR
method analytes in IPR IDC samples
SAMPLE TYPE
LLOPR
method analytes in LLOPRs
SAMPLETYPE
LOQVER
Method analytes in MDL LOQVER IDC samples
SAMPLE TYPE
MDLB
Method analytes in MDL Blank IDC samples
SAMPLE TYPE
MDLS
Method analytes in MDL Spike IDC samples
SAMPLE TYPE
NIS
NIS in all samples
SAMPLE TYPE
NORMAL
method analytes in field samples
SAMPLE TYPE
OPR
method analytes in OPRs
spike cat
HIGH
High
spike cat
LOW
Low
STUDYPHASE
Phase 3 - ICAL
Initial Calibration
STUDY PHASE
Phase 3 - IDC
Initial Demonstration of Capabilities (IDC)
STUDY PHASE
Phase 4.4.1
GW, SW, and WW matrices
STUDY PHASE
Phase 4.4.2
SS and SD matrices
STUDY PHASE
Phase 4.4.3
Tissue matrices
STUDY PHASE
Phase 4.4.4
LC and BS matrices
validator
CHEMVAL
ChemVal
validator
JACOBS
Jacobs Engineering
validator
PYRON
Pyron Environmental
Analysis
PFAS
NULL
Lab Flag
B
Detected in the associated MB of a sample that
exceeded lA LOQ or is at a concentration greater
than l/10th the concentration in the sample,
whichever is greatest.
37
-------
Appendix E - Project Database - Valid Value Codes and Descriptions
YYI. I-kid
YalidYalue
YY l)i'v(i i|>linii
YYI. mahli
all Held
YYI.
inalcli all
code
Yalidalor
Lab Flag
D
When the reported result is from a dilution
Lab Flag
I
Fail to meet ion ratio criteria
Lab Flag
J
At a concentration between the MDL and LOQ
Lab Flag
U
Not detected or were detected at a concentration less
than the MDL
UNIT
ng/L
nanograms per liter
MATRIX
GW
UNIT
ng/L
nanograms per liter
MATRIX
LC
UNIT
ng/L
nanograms per liter
MATRIX
SW
UNIT
ng/L
nanograms per liter
MATRIX
WW
UNIT
ug/kg
micrograms per kilogram
MATRIX
BS
UNIT
ug/kg
micrograms per kilogram
MATRIX
SD
UNIT
ug/kg
micrograms per kilogram
MATRIX
ss
UNIT
ug/kg
micrograms per kilogram
MATRIX
TS
dv qualifier
I
Suspect
dv qualifier
J
Estimated
dv qualifier
J-
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J- when the %D is below acceptance
criteria
dv qualifier
J-
If branched isomers were not included in the
summed result reported, qualify associated detects
as J-
dv qualifier
J+
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J+ when the %D is higher than acceptance
criteria
dv qualifier
U
Values below the MDL are considered non-detects
and are qualified as U at the stated MDL.
dv qualifier
UJ
Verify that the %Ds are within the acceptance
criteria. Non-detects are qualified as UJ in all
associated samples for %D outside of acceptance
criteria.
dv qualifier
UJ
Estimated non-detect
dv qualifier
X
Exclusion of data is recommended
Reviewer qualifier
I
Suspect
Reviewer qualifier
J
Estimated
Reviewer qualifier
J-
If branched isomers were not included in the
summed result reported, qualify associated detects
as J-
Reviewer qualifier
J-
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J- when the %D is below acceptance
criteria
Reviewer qualifier
J+
Verify that the %Ds are within the acceptance
criteria. If any target analytes do not meet the
acceptance criteria, qualify detects for that analyte as
estimated J+ when the %D is higher than acceptance
criteria
38
-------
Appendix E - Project Database - Valid Value Codes and Descriptions
YYI. I-kid
\ ulid\ ahu-
YY l)i'v(i i|>linii
YYI. maUli
all Held
YYI.
inalcli all
code
Yalidalor
Reviewer qualifier
ll
Values below the MDL are considered noil-delects
and are qualified as U at the stated MDL.
Reviewer qualifier
UJ
Verify that the %Ds are within the acceptance
criteria. Non-detects are qualified as UJ in all
associated samples for %D outside of acceptance
criteria.
Reviewer qualifier
UJ
Estimated non-detect
Reviewer qualifier
X
Exclusion of data is recommended
39
-------
Appendix F - Project Database - Valid Value Codes and Descriptions for Compounds
PIWS At RON Y\1
Compound
( AS NO
Kesul(_ 1 >pe |
13C2-4:2FTS
| lH,lH,2H,2H-Perfluoro-l-[l,2-13C2]hexanesulfonic acid
NA
EIS
13C2-6:2FTS
111.111.211.21 l-IVi 1 Iiioio- 1 -| 1.2-1 '( 2|iiclaiicsiiirniiic acid
NA
EIS
13C2-8:2FTS
lH.lH.2H.2H-Pcrfluoro-l-| 1.2-13C2|dccancsulfonic acid
NA
EIS
13C2-PFDoA
Pcrfluoro-n-l 1.2-13C2|dodccanoic acid
NA
EIS
13C2-PFTcDA
Pcrfluoro-n-| 1.2-13C2|lclradccanoic acid
\ \
EIS
13C3-HFPO-DA
Tclrafluoro-2-hcplafluoropropoxy-13C3-propanoic acid
\ \
EIS
13C3-PFBS
Pcrfluoro-1 -|2.3.4-13C3 |bulancsulfonic acid
\ \
EIS
13C3-PFH.\S
Pcrflnoro-1 -| 1.2.3-13C3|hcxancsulfonic acid
\ \
EIS
13C4-PFBA
Pcrfluoro-n-l 13C4|bulanoic acid
\ \
EIS
13C4-PFHpA
Pcrfluoro-n-[l,2,3,4-13C4]heptanoic acid
\ \
EIS
13C5-PFH.\A
Pcrfluoro-n-[l,2,3,4,6-13C5]hexanoic acid
\ \
EIS
13C5-PFPcA
Pcrlluoro-n-l 13C5"|pcnlanoic acid
\ \
EIS
13C6-PFDA
Pcrfluoro-n-l 1.2.3.4.5.6-13C6|dccanoic acid
\ \
EIS
13C7-PFUnA
Pcrfluoro-n-| 1.2.3.4.5.6.7-13C7|undccanoic acid
NA
EIS
13C8-PFOA
Pcrfluoro-n-[13C8]octanoic acid
NA
EIS
13C8-PFOS
Pcrfluoro-l-[13C81oclancsulfonic acid
\ \
EIS
13C8-PFOSA
Pcrfluoro-1 -| 13C8 |oclancsulfonamidc
\ \
EIS
13C9-PFNA
Pcrfluoro-n-[13C9]nonanoic acid
\ \
EIS
D3-NMcFOSA
N-mcthyl-d3 -perfluoro- 1-octanesulfonamide
\ \
EIS
D3-NMcFOSAA
:N-mclhyl-d3-pcrfluoro-1-oclancsulfonamidoacclic acid
NA
EIS
D5-NEIFOSA
N-clhv l-d5-pcrfluoro-1 -oclancsulfonamidc
\ \
EIS
D5-NEIFOSAA
N-clhv l-d5-pcrfluoro-1 -oclancsulfonamidoacclic acid
\ \
EIS
D7-NMcFOSE
N-mcthyl-d7 -perfluorooctanesulfonamidoethanol
\ \
EIS
D9-NEIFOSE
N-clhy l-d9-pcrfluorooclancsulfonamidoclhanol
\ \
EIS
13C2-PFDA
Pcrfluoro-n-| 1.2-13C2|dccanoic acid
\ \
NIS
13C2-PFH.\A
Pcrfluoro-n-[l,2-13C2]hexanoic acid
\ \
NIS
13C3-PFBA
¦Pcrfluoro-n-l2.3.4-13C3|bulanoic acid
\ \
NIS
13C4-PFOA
Pcrfluoro-n-[ 1.2.3.4-13C4]oclanoic acid
\ \
NIS
13C4-PFOS
Pcrfluoro-n-| 1.2.3.4-13C4|oclancsulfonic acid
NA
NIS
13C5-PFNA
Pcrfluoro-n-[l,2,3,4,5-13C5]nonanoic acid
NA
NIS
1802-PFHxS
Pcrfluoro-l-hexane[1802]sulfonic acid
\ \
NIS
1 lCl-PF30UdS
1 l-chlorocicosafluoro-3-oxaundccanc-l-sulfonic acid
TRG
3:3 FTC A
3-Pcrfluoropropyl propanoic acid
i5(>-i>2-5
TRG
4:2FTS
1H. lH.2H.2H-Pcrfluorohcxanc sulfonic acid
757124-72-4
TRG
5:3 FTC A
211.211. '11. '1 l-IVi'l'liKii\KiclaiKnc acid
914637-49-3
TRG
6:2FTS
1H. lH.2H.2H-Pcrfluorooclanc sulfonic acid
27619-97-2
TRG
7:3 FTC A
3-Pcrfluorohcplyl propanoic acid
812-70-4
TRG
8:2FTS
1H. lH.2H.2H-Pcrfluorodccanc sulfonic acid
39108-34-4
TRG
9C1-PF30NS
9-chlorohexadecafluoro-3-oxanonane-l-sulfonic acid
756426-58-1
TRG
ADONA
4.8-dio.\a-3H-pcrfluorononanoic acid
919005-14-4
TRG
HFPO-DA
Hcxafluoropropylcnc oxide dimcr acid
13252-13-6
TRG
NElFOSA
N -cl hy 1 pc rfl uo roocla ncsul fo na midc
415 I-5U-2
TRG
NElFOSAA
N-clhyl perfluorooctanesulfonamidoacetic acid
2991-50-6
TRG
NElFOSE
N-clhy 1 pcrfluorooclancsulfonamidoclhanol
1691-99-2
TRG
NFDHA
Nonafluoro-3.6-dioxahcplanoic acid
151772-58-6
TRG
NMcFOSA
N-mclhvl pcrfluorooclancsulfonamidc
TRG
NMcFOSAA
jN-methyl perfluorooctanesulfonamidoacetic acid
2355-31 -9
TRG
NMcFOSE
N-mclhvl pcrfluorooclancsulfonamidoclhanol
24448-09-7
TRG
PFBA
Pcrfluorobulanoic acid
375-22-4
TRG
PFBS
(Perfluorobutanesulfonic acid
375-73-5
TRG
40
-------
Appendix F - Project Database - Valid Value Codes and Descriptions for Compounds
PIWS At RON Y\1
Compound
( AS NO
Resull T\pe
PI 1) \
Pcrfluorodccanoic acid
>35-76-2
TRG
PI \ )o\
Pcrfluorododecanoic acid
>07-55-1
TRG
Pll)^
Pcrfluorododecanesulfonic acid
-35-77-3
TRG
PI IIS \
Pcrriiioro(2-clho.\> clhanc)siiironic acid
1 1 ^507-82-7
TRG
PI 1 Ip \
Pcrfluorohcplanoic acid
'"5-S5-1'
TRG
PI 1 lp-
Pcrfluoroheptanesulfonic acid
:"5-'J:-S
TRG
PI 1 K \
Pcifluorohcxanoic acid
TRG
PI 1 K-
Pcrfliiorohcxancsuironic acid
;55-4i-4
TRG
PI All! \
Pcrniioro-4-mclho.\\bulanoic acid
S(..()'J()-S'J-5
TRG
PIMP \
Pcifliinrn-'-iiiclhn\\ propanoic acid
TRG
Pl \ \
Pcrfluorononanoic acid
;"5-.)5-|
TRG
PI\S
Pcrfluorononancsulfonic acid
i.s:5'j-i:-i
TRG
PI () \
Pcrfluorooclanoic acid
:'5-(>"-l
TRG
PR >S
PcifliinriKiclMiicMiirniiic acid
n.-:-i
TRG
PI ()S\
Pcrfliiorooclancsuironamidc
"54-'H-(.
TRG
PI IV \
Pcrfluoropcnlanoic acid
TRG
Pi ivs
Pcrfluoropcnlancsulfonic acid
:"()(,-•) 1-4
TRG
PI 1 cl) \
IViriiininicliadccaiinic acid
TRG
PI III) \
Pcrfluorolridccanoic acid
TRG
PFUnA
(Pcrlluoroundecanoic acid
,2058-94-8
TRG
41
-------
PFAS Multi-Laboratory Validation Study Report
Aqueous Media: Wastewater, Surface Water, and Groundwater
SERDP
Appendix D
PFAS MLVS Institute for
Defense Analyses Report
Date: July 25, 2023
-------
IDA
INTEROFFICE MEMORANDUM
SCIENCE & TECHNOLOGY
DIVISION
26 July 2023
To: Dr. Kimberly Spangler, Dr. Andrea Leeson, SERDP/ESTCP
CC: Mr. Timothy Thompson, Science, Engineering and the Environment, LLC
From: Dr. Allyson Buytendyk, Institute for Defense Analyses (IDA)
Subject: IDA Statistical Analyses in the PFAS Multi-Lab Validation
In 2022, SERDP/ESTCP sponsored IDA as the independent organization to conduct the
statistical analyses in the joint Department of Defense (DoD) and Environmental Protection
Agency (EPA) multi-laboratory validation (MLV) of a PFAS measurement method—EPA Draft
Method 1633. IDA's role in the PFAS MLV study is to summarize the overall performance of the
laboratories for each test where those values inform the quality control (QC) acceptance criteria
set by the EPA for the method.
The study plan for the PFAS MLV closely follows the process outlined in the EPA
Alternate Test Procedure (ATP) guidance1 which, describes the tests and procedures for
developing QC acceptance criteria based on data generated in a study. The ATP specifies three
tiers of statistical formulas based on the number of labs analyzing each sample. The PFAS MLV
study includes ten participating laboratories and three types of datasets: initial calibration (ICAL),
initial demonstration of capability (IDC) and environmental matrix samples.
IDA analyzed the ICAL, aqueous IDC and three environmental matrices: wastewater
(WW), surface water (SW) and ground water (GW) datasets provided by the sponsor2. IDA used
the statistical formulas outlined in the MLV/EPA's ATP at Tier 33 for most tests and identified
alternative calculations in instances when a discrepancy between the PFAS MLV dataset and
1 EPA, Protocol for Review and Validation of new Methods for Regulated Organic and Inorganic Analytes in
Wastewater Under EPA's Alternative Test Procedure Program. February 2018. EPA 821-B-18-001
2 IDA perforins calculations on the dataset using coded scripts in Python version 3.7.8, rounds statistical values based
on the number of significant figures reported in the dataset and delivers the outputs as CSV files to the sponsor.
3 QC acceptance criteria at Tier 3 requires a minimum of nine laboratories. EPA ATP, pg. G-22.
1
-------
formulas ocurred. This memo explains the formulas IDA used in the statistical analyses and
documents the version of the dataset and corresponding tables generated for the PFAS MLV study.
STATISTICAL FORMULAS
ICAL DATASET
Calibration Linearity
Equation 1: Pooled Percent RSD4
_ l^-DRSPf
mVpooled ~ ^ s(n._i) ,
where n = number of RF values, RSDi = relative standard deviation of ith RF values.
IDC DATASET
Method Detection Limit (MDL)
MDL Spiked Samples
Equation 2: MDL Spiked Samples (MDLS)5
MDLSj — S sj 1 t(n_i ,l-oc=0.99)'
where Ss,j=sample standard deviation, of spiked sample measured concentrations for lab j, t(n_11_K=0 99) =
student's t-value for the one tailed test at the 99% confidence level with n-1 degrees of freedom.
MDL Blank Samples6
• If none of the blank samples give a numerical result, the MDL for the blank samples does
not apply.
4 https://goldbook.iupac.org/terms/view/P04757; PureAppl. Chem., 1981, 53 (9), 1805-1826.
http://dx.doi.org/10.1351/pacl98153091805
5 EPA ATP, pg. G-9.
6 Ibid.
2
-------
• If some (but not all) of the blank samples give a numerical result, the MDL for the blank
samples is the max value.
• If all of the blank samples give a numerical result, the MDL for the blank samples is:
Equation 3: MDL Blank Samples (MDLb)7
MDLjyj — Xj + Sjjj ¦ t(n-i,i-oc=o.99)<
where Xj = mean measured concentration of the blank samples for lab j, Sb = sample standard deviation, of the
blank samples measured concentration for lab j, t!11_ l l_K=0 c|c|) = student's t-value for the one tailed test at the
99% confidence level with n-1 degrees of freedom.
where MDLsj = the MDL for the spiked samples for lab j, MDLbj = the MDL for the blank samples for lab j.
where m = number of labs, MDLj = method detection limit for the jth lab, n,j = number of replicates for the jth
lab, N = total number of replicates, tinl_u=099) = student's t-value for the one tailed test at the 99% confidence
level with n degrees of freedom.
Limit of Quantitation Verification (LOQVER)
7 EPA ATP, pg. G-9.
8 40 CFR 136, Appendix B (2020).
9 EPA, ATP pg. G-22.
Lab MDL
Equation 4: MDL8
MDLj = max{MDLsj, MDLb j);
Pooled MDL
Equation 5: Pooled MDL9
3
-------
Equation 6: LOQ Percent Bias10
spike concentration-X; _
LOQbtas / = :—L ¦ 100;
spike concentration
where X, = mean of the measured sample concentrations for lab j.
Initial Precision and Recovery (IPR)
Equation 7: Between Lab Standard Deviation (Sb)11
km-1)1
S'=J m — 1
where m = the number of labs, X = overall mean percent recovery, Xj = the mean percent recovery for the jth
lab.
Equation 8: Within Lab Standard Deviation (sw)12
fcr=ife)2
S*» = \sr-
where m = the number of labs, Sj = the variance of the percent recovery values for the jth lab.
Equation 9: IPR Combined Standard Deviation (sipr)13
where m = the number of labs, n = the number of data points per lab, Sb = the between lab standard deviation,
sw = the within lab standard deviation.
Equation 10: RSD14
RSD = ^ ¦ 100;
X
where sw = the within lab standard deviation, X= mean percent recovery across all labs.
10 DoD QSM Version 5.4 (2021), Module 4, Section 1.5.2, pg. 77.
11 EPA, ATP pg. G-25.
12 EPA ATP, pg. G-25.
13 Ibid.
14 EPA ATP, pg. G-26.
4
-------
ENVIRONMENTAL MATRIX DATASET
Ongoing Precision and Recovery (OPR) & Low-Level Ongoing Precision and Recovery
(LLOPR)
Equation 11: OPR Combined Standard Deviation (sopr)15
where m = the number of labs, n = the number of data points per lab, Sb = the between-lab standard deviation,
sw = the within-lab standard deviation.
Equation 10 provides the formula for the RSD for the OPR test. The calculations for the
LLOPR test follow those for the OPR using Equations 7, 8, 10, and 11.
Matrix Spike Recovery
The calculations for the matrix spike test include those in Equations 7 and 8 to determine
Sb and sw as well as Equation 10 to find the RSD for the matrix test.
DATASETS & TABLES
Dataset Type & File Version
IDA Generated Tables
ICAL
ICAL Concentrations 08182022.xlsx
ICAL Average RF_05182023.xlsx
IC AL_calibration_V0_220907_093 746. csv
AverageRF ICAL results V4 230519 091739.csv
IDC
RW_DBexport_Vl_2023 0426. csv
MDL_results_Vl_230503_215159. csv
LOQVER_results_Vl_230503_215921.csv
IPR_results_V 1_230503_215140.csv
WW
WW_DBexport_V7_20230328.csv
LLOPR_results_V4_23 0406_212723. csv
15 EPA ATP, pg. G-26.
5
-------
Dataset Type & File Version
IDA Generated Tables
OPR_results_V4_23 0406_21223 7. csv
Matrix EIS results V4 230406 212819.csv
Matrix sample results V4 230406 211329.csv
Matrix compiled results V4 230406 211329.csv
MB_results_V4_230406_212853.csv
SW
SW_DBexport_V4_20230407.csv
LLOPRresultsV0 23 0411_08013 0. csv
OPRresultsV0 23 0411_080146. csv
Matrix EIS results V0 230411 080212.csv
Matrix sample results V0 230411 080232.csv
Matrix compiled results V0 230411 080232.csv
MB_results_V0_23041 l_080058.csv
GW
GW_DBexport_V6_2023 0417b. csv
LLOPRresultsV0 23 0421_07493 5. csv
OPRresultsV0 23 0420_183 700. csv
Matrix EIS results V0 230420 175829.csv
Matrix sample results V0 230421 153930.csv
Matrix compiled results V0 230421 153930.csv
MB_results_V0_230420_l 83436.csv
All
Aqueous
WW_SW_GW_EXPORT_2023 0605. csv
LLOPRresultsV 1 _23 0607_12465 5. csv
OPR_results_V 1 _23 0607_124749. csv
Matrix EIS results VI 230607 124828.csv
Matrix_NIS_results_Vl_230607_124909.csv
6
-------
PFAS Multi-Laboratory Validation Study Report
Aqueous Media: Wastewater, Surface Water, and Groundwater
SERDP
Appendix E
Wastewater Supporting
Tables
Date: July 25, 2023
-------
Appendix E: List of Tables
El Target analytes detected in unspiked wastewater samples by kaboratory
E2 Minimum and maxium target analytes concentrations in unspiked wastewater samples
E3 Summary of wastewater spike percent recoveries in low spike samples for each laboratory.
E4 Summary of wastewater spike percent recoveries in high spike samples for each laboratory.
E5 Summary of wastewater EIS percent recovery for each laboratory.
-------
Table E-l. Target Analytes Detected in Unspiked Wastewater Samples by Laboratory (ng/L)
Analyte
Number
Lab 1
Lab 2
Lab 3
Lab 4
Lab 5
Lab 6
Lab 7
Lab 9
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
IIII / - Hospital
PFBA
8
2.64
J
3.58
J
1.04
U
1.86
J-
24.1
0.597
U
25.1
6
PFPeA
8
5.76
6.23
Jl
8.56
5.1
5.03
0.563
U
4.4
5.06
PFHxA
8
14.2
11.8
13.1
9.82
9.7
8.69
9.4
10.4
PFHpA
8
2.5
2.41
J
2.8
2.4
2.48
0.173
u
1.8
J
1.95
PFOA
8
2.09
3.75
J
2.24
2.35
2.45
BJ+
2.75
1.6
J
1.62
PFBS
8
1.84
J
2.35
J
4.16
1.57
J
1.82
0.177
u
1.8
J
2.02
PFPeS
8
2.1
2.22
J
2.8
2.03
2.07
1.72
1.6
J
1.82
PFHxS
8
14.1
18
21.8
18
16.1
13.6
7.8
11.7
PFOS
8
3.04
5
5.6
4.63
3.37
3.44
2.2
1.7
J
6:2FTS
8
1.76
J
7.92
U
2.82
U
1.6
U
1.46
U
1.54
J
3.5
U
0.945
U
PFOSA
8
0.346
U
0.724
U
0.416
u
0.565
U
0.746
BJ+
0.472
J
0.67
U
0.154
U
PFMPA
8
0.578
U
1.09
u
0.48
u
0.556
u
0.745
J
0.628
u
0.99
u
0.321
u
II ll./-mril Influent
PFBA
8
4.93
J
4.2
J
5.04
J
4.64
J-
4.63
J
0.597
u
12.2
5.83
PFPeA
8
9.19
10.1
11.1
9.45
8.88
0.563
u
9.1
9.37
PFHxA
8
21.7
21.2
21.8
18.2
17.2
20.2
18.7
19.8
PFHpA
8
7.97
8.24
9.12
7.83
7.68
5.96
8.5
7.98
PFOA
8
12
13.7
16.5
12.5
14.2
11.3
12.6
13.2
PFNA
8
3.12
3.3
J
3.6
2.93
2.59
3.53
3.2
3.44
PFDA
8
1.29
J
1.62
J
1.2
J
1.22
J
0.892
U
0.223
u
1.9
J
1.3
PFBS
8
4.43
4.72
0.528
u
3.58
0.348
U
0.177
u
3.3
4.96
PFPeS
8
0.351
u
1.31
u
0.272
u
0.375
u
0.729
U
0.129
u
1.1
u
1.37
1
PFHxS
8
4.2
2.92
J
3.52
3.68
3.04
2.83
2.1
3.03
PFOS
8
7.45
6.18
7.6
7.63
7.25
7.09
6.2
7.38
J
6:2FTS
8
23.7
25.3
26.2
25.6
22.3
24.4
22.5
24.9
8:2FTS
8
4.5
J
7.48
u
5.36
J
3.56
u
4.67
J
4.38
J
5.6
J
5.32
PFOSA
8
0.346
u
0.724
u
0.416
u
0.565
u
0.397
BJ+
0.188
u
0.67
u
0.154
u
NMeFOSAA
8
1.44
J
3.3
u
1.68
2.19
1.49
J
0.655
u
2
1.97
NEtFOSAA
8
0.75
J
2.26
u
0.856
u
0.61
u
0.531
Jl
0.571
u
1.3
u
0.283
u
5:3FTCA
8
5.54
u
16.7
u
9.36
u
6.66
u
29.2
U
4.72
J
8.7
u
1.88
u
-------
Table E-l. Target Analytes Detected in Unspiked Wastewater Samples by Laboratory (ng/L)
Analyte
Number
Lab 1
Lab 2
Lab 3
Lab 4
Lab 5
Lab 6
Lab 7
Lab 9
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
WWL - Bus Washing Station
PFBA
8
11.7
3.06
J
11.5
9.77
J-
8.98
0.597
U
14
11.4
PFPeA
8
45
41
61.1
35.6
35.2
43.8
38.9
37.6
PFHxA
8
81.6
84.1
83.9
76.9
78.6
66.5
81
79.5
PFHpA
8
32.2
32.5
31.3
28.4
29.5
29.7
32.1
30.7
PFOA
8
8.36
9.53
11
8.61
11.8
8.85
7.3
9
PFNA
8
2.18
2.24
J
2.8
2.16
2.33
2.12
2.3
2.28
PFDA
8
1.21
J
1.53
J
1.04
Jl
0.899
J
-
X
0.223
U
0.77
J
1.01
PFUnA
8
0.609
U
1.73
J
0.664
U
0.574
U
-
X
0.203
u
0.6
U
0.182
U
PFDoA
8
0.603
U
1.16
J
0.752
U
0.345
U
-
X
0.301
u
0.6
U
0.169
U
PFBS
8
0.289
u
1.45
J
0.528
u
0.628
u
0.941
J
0.177
u
1.4
J
1.03
PFHxS
8
1.3
Jl
1.43
U
0.464
u
0.789
u
0.803
J
0.291
u
0.7
u
0.171
u
PFOS
8
2.08
1.75
J
2.48
1
1.98
1
-
X
1.42
J
0.54
u
2.23
J
6:2FTS
8
6.15
J
7.92
U
5.2
J
4.42
J
4.72
J
2.63
J
35
u
4.07
PFOSA
8
0.346
u
1.02
J
0.416
u
0.565
u
-
X
0.188
u
0.67
u
0.154
u
HFPO-DA
8
1.85
u
4.17
u
2
J
2.89
u
2.14
u
0.748
u
0.97
u
0.891
u
3:3FTCA
8
2.12
J
3.97
u
3.36
J
3.19
J
6.57
u
1.67
u
4.5
u
1.48
u
7:3FTCA
8
6.53
u
27.7
J
5.18
u
4.15
u
25.3
u
5.22
u
7.9
u
2.56
u
-------
Table E-l. Target Analytes Detected in Unspiked Wastewater Samples by Laboratory (ng/L)
Analyte
Number
Lab 1
Lab 2
Lab 3
Lab 4
Lab 5
Lab 6
Lab 7
Lab 9
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
IIIIM-mill HJJlucnl
PFBA
8
10
9.28
J
10.7
8.26
J-
8.56
0.597
U
14.6
12
PFPeA
8
10.5
12.9
15
10.6
10.6
0.563
U
10.2
10.8
PFHxA
8
38.1
41.4
41.4
36.2
39.3
32.3
36
38.5
PFHpA
8
4.07
4.47
4.4
4.2
3.97
3.26
3.6
4.38
PFOA
8
12
12.9
14.2
11.7
13.8
10.1
10
12.3
PFNA
8
0.93
J
1.06
U
1.76
1
0.718
J
0.851
J
1.35
J
0.63
J
1.18
PFDA
8
2.33
2.96
J
2.16
1.97
J
1.58
J
2.14
1.9
J
1.92
PFUnA
8
0.609
U
1.48
J
0.664
U
0.574
U
0.786
U
0.203
u
0.6
U
0.182
U
PFDoA
8
0.603
U
1.31
J
0.752
U
0.345
U
0.412
U
0.301
u
0.6
U
0.169
U
PFTrDA
8
0.478
u
1.02
J
0.608
u
0.281
u
0.838
u
0.363
u
0.84
u
0.196
u
PFBS
8
4.53
5.25
3.44
3.83
3.8
0.177
u
3.6
5.68
PFHxS
8
2.88
1
1.53
J
2.08
0.789
u
1.48
J
2.03
0.86
J
1.41
PFOS
8
2.73
3.23
J
2.96
3.35
3.15
2.53
2.2
2.68
J
6:2FTS
8
6.96
J
7.92
U
9.44
6.96
J
7.92
6.75
7.8
J
7.07
PFOSA
8
0.346
u
1.11
Jl
0.416
u
0.565
u
0.359
BJ+
0.188
u
0.67
u
0.154
u
NMeFOSA
8
0.453
u
0.809
J
0.704
u
1.21
u
0.341
U
0.199
u
0.64
u
0.153
u
NMeFOSAA
8
0.739
J
3.3
X
1.08
J
0.84
J
0.655
u
0.98
u
0.186
u
7:3FTCA
8
6.53
u
25.4
J
5.18
u
4.15
u
25.3
U
5.22
u
7.9
u
2.56
u
II IIX - Pulp mid Paper lijlhicnl
PFBA
8
0.941
u
3.42
J
2.64
J
-
X
5.51
J
-
X
1.9
u
-
X
PFPeA
8
0.552
u
3.42
J
13.8
0.306
u
6.7
0.563
u
3.4
J
3.19
PFHxA
8
0.454
u
2.99
J
4.56
2.36
2.7
0.412
u
2.7
2.14
PFHpA
8
0.501
u
1.07
J
1.12
J
0.368
u
1.7
Jl
0.173
u
1.5
J
0.158
u
PFOA
8
1.1
J
1.96
J
1.68
1.29
J
1.82
BJ+
1.63
1.4
J
1.56
PFNA
8
0.657
u
1.06
u
2.08
1
0.29
u
0.792
U
0.25
u
0.61
u
0.166
u
PFBS
8
0.289
u
1.08
u
1.2
J
0.628
u
0.864
J
0.177
u
0.95
J
0.104
u
PFHxS
8
1.65
J
1.57
J
1.36
J
1.32
Jl
1.27
J
1.04
J
1.2
J
1.39
PFOS
8
3.55
3.85
4.72
3.61
3.78
3.21
2.8
3.41
J
PFOSA
8
0.346
u
0.724
u
0.416
u
0.565
u
0.344
BJ+
0.188
u
0.67
u
0.154
u
-------
Table E-l. Target Analytes Detected in Unspiked Wastewater Samples by Laboratory (ng/L)
Analyte
Number
Lab 1
Lab 2
Lab 3
Lab 4
Lab 5
Lab 6
Lab 7
Lab 9
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
11 IK)-ro/ ll lljjlucnl
PFBA
8
7.88
J
7.94
J
8.56
7.4
J
8.33
0.597
U
12.3
8.31
PFPeA
8
22.6
25
27.1
23.1
23
22.8
22.4
22.4
PFHxA
8
51.7
61
52.9
50.7
57.7
46.2
52.7
49
PFHpA
8
8.4
8.86
9.04
8.01
7
6.78
8
8.31
PFOA
8
9.56
12.1
12.9
9.43
11.1
7.6
10.3
10.7
PFNA
8
1.95
J
2.64
J
3.36
J-
1.84
J
2.64
2.51
2.5
2.71
PFDA
8
1.06
J
1.36
U
0.72
Jl
0.596
U
0.892
U
0.223
U
0.69
J
0.181
U
PFBS
8
10.7
11.1
13.4
9.33
9.64
15.3
14.2
13.1
PFPeS
8
1.66
J
1.94
J
2.08
1.96
1.75
J
0.129
u
2.2
2
PFHxS
8
12.5
13.6
14.2
13.4
13.9
11.1
10.8
12.2
PFHpS
8
0.874
J
3.06
U
1.6
0.633
U
0.731
J
0.204
u
0.49
U
0.112
U
PFOS
8
35.2
27.6
35.5
32.5
31.3
31.2
30.3
28.8
6:2FTS
8
233
341
289
267
274
352
277
264
8:2FTS
8
1.41
U
7.48
u
2.5
U
3.56
u
1.45
U
1.08
J
4.1
U
0.544
u
PFOSA
8
0.346
U
0.724
u
0.416
U
0.565
u
0.228
BJ+
0.188
u
0.67
u
0.154
u
5:3FTCA
8
9.54
J
18.5
J
11.8
J
13.1
J
29.2
U
13.8
J
8.7
u
1.88
u
Compounds undetected in all samples included: PFTeDA, PFNS, PFDS, PFDoS, 4:2FTS, NEtFOSA, NMeFOSE, NEtFOSE, PFMBA, NFDHA, ADONA, PFEESA, 9CI-PF30NS, HCI-PF30UdS
-------
Table E-2. Minimum and Maxium Target Analytes Concentrations in Unspiked Wastewater Samples (ng/L)
Analyte
Number of
Labs
WW I
WW,I
WWL
WWM
WWN
wwo
min
max
min
max
min
max
min
max
min
max
min
max
PFBA
8
0.597 U
25.1
0.597 U
12.2
0.597 U
14
0.597 U
14.6
0.941 U
5.51 J
0.597 U
12.3
PFPeA
8
0.563 U
8.56
0.563 U
11.1
35.2
61.1
0.563 U
15
0.306 U
13.8
22.4
27.1
PFHxA
8
8.69
14.2
17.2
21.8
66.5
84.1
32.3
41.4
0.412 U
4.56
46.2
61
PFHpA
8
0.173 U
2.8
5.96
9.12
28.4
32.5
3.26
4.47
0.158 U
1.7 JI
6.78
9.04
PFOA
8
1.6 J
3.75 J
11.3
16.5
7.3
11.8
10
14.2
1.1 J
1.96 J
7.6
12.9
PFNA
8
0.166 U
1.06 U
2.59
3.6
2.12
2.8
1.06 U
1.761
0.166 U
2.081
1.84 J
3.36 J-
PFDA
8
0.181 U
1.36 U
0.223 U
1.9 J
0.223 U
1.53 J
1.58 J
2.96 J
0.181 U
1.36 U
0.181 U
1.06 J
PFUnA
8
0.182 U
0.928 U
0.182 U
0.928 U
0.182 U
1.73 J
0.182 U
1.48 J
0.182 U
0.928 U
0.182 U
0.928 U
PFDoA
8
0.169 U
0.822 U
0.169 U
0.822 U
0.169 U
1.16 J
0.169 U
1.31 J
0.169 U
0.822 U
0.169 U
0.822 U
PFTrDA
8
0.196 U
0.978 U
0.196 U
0.978 U
0.196 U
0.978 U
0.196 U
1.02 J
0.196 U
0.978 U
0.196 U
0.978 U
PFBS
8
0.177 U
4.16
0.177 U
4.96
0.177 U
1.45 J
0.177 U
5.68
0.104 U
1.2 J
9.33
15.3
PFPeS
8
1.6 J
2.8
0.129 U
1.371
0.166 U
1.31 U
0.166 U
1.31 U
0.166 U
1.31 U
0.129 U
2.2
PFHxS
8
7.8
21.8
2.1
4.2
0.171 U
1.3 JI
0.789 U
2.881
1.04 J
1.65 J
10.8
14.2
PFHpS
8
0.112U
3.06 U
0.112 U
3.06 U
0.112U
3.06 U
0.112 U
3.06 U
0.112U
3.06 U
0.112 U
1.6
PFOS
8
1.7 J
5.6
6.18
7.63
0.54 U
2.481
2.2
3.35
2.8
4.72
27.6
35.5
6:2FTS
8
0.945 U
1.76 J
22.3
26.2
7.92 U
6.15 J
7.92 U
9.44
0.945 U
7.92 U
233
352
8:2FTS
8
0.544 U
7.48 U
3.56 U
5.6 J
0.544 U
7.48 U
0.544 U
7.48 U
0.544 U
7.48 U
0.544 U
1.08 J
PFOSA
8
0.154 U
0.746 BJ+
0.154 U
0.397 BJ+
0.154 U
1.02 J
0.154 U
1.11 JI
0.154 U
0.344 BJ+
0.154 U
0.228 BJ+
NMeFOSA
8
0.153 U
1.21 U
0.153 U
1.21 U
0.153 U
1.21 U
0.153 U
0.809 J
0.153 U
1.21 U
0.153 U
1.21 U
NMeFOSAA
8
0.186 U
3.3 U
0.655 U
2.19
0.186 U
9.8 U
0.186 U
1.08 J
0.186 U
3.3 U
0.186 U
3.3 U
NEtFOSAA
8
0.283 U
2.26 U
0.283 U
0.75 J
0.283 U
13 U
0.283 U
2.26 U
0.283 U
2.26 U
0.283 U
2.26 U
PFMPA
8
0.321 U
0.745 J
0.321 U
1.33 U
0.321 U
1.33 U
0.321 U
1.33 U
0.321 U
1.33 U
0.321 U
1.33 U
HFPO-DA
8
0.338 U
4.17 U
0.339 U
4.17 U
0.748 U
2 J
0.354 U
4.17 U
0.319 U
4.17 U
0.355 U
4.17 U
3:3FTCA
8
0.86 U
6.57 U
0.86 U
6.57 U
1.48 U
3.36 J
0.86 U
6.57 U
0.86 U
6.57 U
0.86 U
6.57 U
5:3FTCA
8
1.88 U
29.2 U
1.88 U
4.72 J
1.88 U
29.2 U
1.33 U
29.2 U
1.33 U
29.2 U
1.88 U
18.5 J
7:3FTCA
8
2.56 U
25.3 U
2.56 U
25.3 U
2.56 U
27.7 J
2.56 U
25.4 J
2.56 U
25.3 U
2.56 U
25.3 U
-------
Table E-3. Summary of wastewater spike percent recoveries in low spike samples for each laboratory.
Analyte
Lab 1 spike % recover
y
Lab 2 spike % recover
y
Lab 3 spike % recover
y
Lab 4 spike % recover
y
Lab 5 spike % recover
y
n
Min
Max
Mean
n
Min
Max
Mean
n
Min
Max
Mean
n
Min
Max
Mean
n
Min
Max
Mean
PFBA
18
91.6
132.5
101.5
18
100.6
128
110.9
17
107.2
113.6
110.6
14
87.1
112.3
103
18
51.4
96.4
80.7
PFPeA
15
90.1
148.2
103
15
100
139.9
113.1
14
102.6
116
110.2
17
92.1
116.2
103.2
18
64.5
101
87.2
PFHxA
6
87
170.5
108.8
6
92.5
124.5
102.9
6
96
110.5
104.7
9
91.4
121
101.9
9
77.5
113
94.3
PFHpA
15
81
149.5
98.1
15
95.2
129
104.1
14
95.3
110
100.4
15
89.4
108.4
97.6
15
72.5
104
87
PFOA
18
84.7
152.5
99.5
18
89.5
127.8
108.3
17
91
138
117
18
87
105.8
98.3
18
68.5
138.5
99.1
PFNA
18
80.1
139.5
96.7
18
94.5
141.5
105.6
17
96.2
133.7
113.3
18
88.5
119
98.2
18
70
106.5
89.8
PFDA
18
89.2
169.5
106.2
18
92.2
121.5
99.6
17
97.3
137.2
108.8
18
90.5
109.5
98.6
18
70.5
106
86.8
PFUnA
18
71
148
94.5
18
65
113.4
94.2
17
90.5
135
109.9
18
81
100
94.9
18
69
107
83.9
PFDoA
18
68
131
84.8
18
37
109.5
86.7
17
81
119
95.9
18
85
106.5
95.9
16
62
96.5
78.5
PFTrDA
18
62
138
86.4
18
15.6
105.5
60.8
17
57.5
129
89.9
17
84
102.5
94.6
16
41
95
68.4
PFTeDA
17
75
127
96.2
17
18
111
81.9
17
90.5
140
111.2
17
95
122
103.8
12
79.5
124.5
96.7
PFBS
18
76.4
144.5
93.9
18
98.9
129.2
105.4
17
100.5
141
115.8
18
91.1
112
101.7
18
72.7
109.5
83.7
PFPeS
18
83.2
147
101.9
18
91.6
129.6
102.8
17
95.5
116.8
102.1
18
93.9
110.1
101.7
18
81.2
114.9
92.7
PFHxS
18
81.1
139.6
93.8
18
91.7
140.3
102
14
95.1
113.9
103.6
18
89.6
130.8
106.6
18
77.6
117.4
96.1
PFHpS
18
85.5
139.5
98.2
18
100
154
112.1
17
99
129
109.1
18
87.5
127.5
102.4
18
78.5
173
102.4
PFOS
15
90.6
143.7
105.3
15
94.5
121.5
102.3
15
95.9
120.7
105.1
15
85.4
105.7
95
15
81.6
103.5
93.1
PFNS
18
66.3
133.7
88.4
18
60.4
97.5
79.7
17
81.7
109.9
96.4
18
53.5
102
89.9
18
31.8
90.6
69.6
PFDS
18
29.2
125.3
67.7
18
19.9
89.9
59.4
17
65.7
114.6
92.3
18
14.7
96
78.9
18
00
00
89.4
51.7
PFDoS
18
14.3
86.9
45.4
17
00
00
63.8
37.7
17
40.2
113.1
77.4
17
53.8
93
74.5
15
5.1
54.3
29.6
4:2FTS
18
92.2
126.7
103.9
18
97.6
120.1
105.2
17
99
111.2
104.9
18
75.2
111.3
92.8
18
84.4
103.4
93.4
6:2FTS
15
76.9
121.8
97.5
15
94
143.8
112.4
15
104
119.5
110.2
15
90.5
109
100.2
15
86.1
109.4
97
8:2FTS
18
92.8
123.7
102.2
18
100.1
136.8
110.9
17
106
151.8
123.6
18
69.8
116.7
102.9
18
87.5
110.8
100.4
PFOSA
18
91
151
103.4
18
72.5
136
100.9
17
98.5
124.5
110.1
18
96
183.5
113.9
13
73.5
104.3
86.2
NMeFOSA
18
75.5
122.5
86.8
18
32.8
108.5
84.9
17
77.5
164
98.3
18
49.8
117.5
90.2
13
69.5
104
93.3
NEtFOSA
18
78.5
125
88.8
17
23.5
92.5
74.8
17
73
168
97.3
18
57.5
110
90.9
12
82.5
99
91.4
NMeFOSAA
18
79
213
127.5
18
78.5
197
144.5
6
146.6
188.6
171.1
18
103
535
215.6
17
80.5
165
124
NEtFOSAA
18
72.5
223
119.5
18
64.5
205.5
136.8
17
106
381.5
172.1
18
100
400
188.4
15
87
177
123.8
NMeFOSE
18
72.5
94.4
85
17
34.2
95
77.2
17
47.1
126.9
83.2
17
46.3
101.9
83.9
12
66.9
113.8
87.3
NEtFOSE
18
73.8
89.4
81.6
17
21.9
96.2
71.1
17
56.4
135.6
90.6
17
53.1
101.2
84.8
10
61.6
126.9
97
PFMPA
18
64.8
102.2
89.1
18
78.2
116.8
100.4
17
62
109.5
97.4
17
15.2
107
84.5
18
36
113.5
79.9
PFMBA
18
85
146.2
101.4
18
98.8
129.8
111.2
17
115.3
139.5
127.2
17
98
156
112.8
18
99.2
163.2
123.4
NFDHA
18
78.2
121.2
93.9
18
58.8
111.5
83.5
17
64.2
141.2
99.6
18
25.8
102.8
79.8
18
90.3
131.2
113.2
HFPO-DA
18
96.4
124.8
104.7
18
110.5
228.8
151.9
17
96.1
108.6
102.8
18
88.6
128.8
105.6
18
88.1
125
102.2
ADONA
18
92.5
130.9
107.9
18
120.7
228.2
153.7
17
92.8
124.7
106.7
18
88.8
446.4
129.7
18
89.9
120.6
102
PFEESA
18
100.2
159.6
109.8
18
45.9
99
76.8
17
83
125.2
98.2
18
95
118.7
102.8
18
81.3
119.5
100.3
9C1-PF30NS
18
99.4
144.5
114.6
18
81.7
144.5
122.5
17
71
110.8
95.9
18
56.7
447.1
126.5
18
9.9
121.2
80.2
llCl-PF30UdS
18
36
113.6
74.4
18
9.3
111.1
66.3
17
44.9
106.5
82.7
18
5
313
104.6
16
3.7
95.4
55.2
3:3FTCA
18
51.7
94.3
80.1
18
58.8
102.6
79.5
17
94.1
114.2
103.2
17
51
136
101.3
18
40.4
151.2
83.9
5:3FTCA
18
80.8
253.3
94.6
18
67.4
133.8
91.9
17
77.5
116.7
93.9
18
82.6
302.5
114.6
18
64
123.3
96.6
7:3FTCA
18
81
257.5
98.9
18
61.7
255.8
98.6
17
90.8
189.2
128.6
18
63.9
301.7
103.3
18
24.6
105.8
73.9
-------
Table E-3. Summary of wastewater spike percent recoveries in low spike samples for each laboratory.
Analyte
Lab 6 spike % recover
y
Lab 7 spike % recover
y
Lab 9 spike % recover
y
All Labs
n
Min
Max
Mean
n
Min
Max
Mean
n
Min
Max
Mean
n
Min
Max
Mean
PFBA
16
78.9
99.2
88.6
18
92.9
125
103.1
15
42.1
104.4
91.3
134
42.1
132.5
98.8
PFPeA
15
58.5
195
106.7
18
79
113.8
101.2
18
20.5
97
87.7
130
20.5
195
100.8
PFHxA
6
99
151.5
122.4
9
86
108
98.6
9
78
102
90.6
60
77.5
170.5
101.7
PFHpA
15
52.1
101
84
15
86
105
94
15
23.9
97
84.3
119
23.9
149.5
93.6
PFOA
18
68.8
99
82.2
18
90
109.5
99.1
18
22.5
94
83.5
143
22.5
152.5
98.2
PFNA
18
66
100
81.3
18
86
104
94.7
18
43
96
88.1
143
43
141.5
95.8
PFDA
18
61.5
107.5
80.6
18
89
116.5
101.3
18
52
98.5
90.1
143
52
169.5
96.4
PFUnA
18
66.5
119.5
88.8
18
72.5
108
84.9
18
52.5
105
87.5
143
52.5
148
92.2
PFDoA
18
49.2
105.5
74.8
18
64
116.5
93.2
18
48.7
106.5
83.5
141
37
131
86.7
PFTrDA
18
48.6
144
84.3
18
60
113
80.8
18
37.2
91.5
65.3
140
15.6
144
78.8
PFTeDA
18
53
109
79
18
88
180.5
115.6
18
42.7
110
84.7
134
18
180.5
96
PFBS
18
55.5
137.5
102.6
18
83.8
110.5
99.1
18
18.5
101.8
90.7
143
18.5
144.5
99
PFPeS
18
68.3
117.8
86
18
84.7
106.9
96.3
18
42.1
96
89.3
143
42.1
147
96.6
PFHxS
18
48.8
108.3
82
18
60.7
110.9
87
18
19.4
113.4
87.9
140
19.4
140.3
94.6
PFHpS
18
64
114
87.9
18
97.5
117
109.3
18
51.5
101.5
91.7
143
51.5
173
101.6
PFOS
15
69.8
95.8
84.1
15
79
108.5
97.5
15
76.9
99
88.4
120
69.8
143.7
96.4
PFNS
18
57.4
83.2
70.3
18
67.3
99.5
82.6
18
43
88.1
76.5
143
31.8
133.7
81.6
PFDS
18
37.4
88.4
66
18
48
90.4
68.9
18
40.2
84.8
64.6
143
00
00
125.3
68.5
PFDoS
18
22.3
66.8
50.6
18
30.2
92
56.7
18
11.7
63.8
43.5
138
5.1
113.1
52.2
4:2FTS
18
64.2
125.3
91.8
18
63.1
99.7
85.9
18
47.1
94.4
89
143
47.1
126.7
95.8
6:2FTS
15
45.3
152.8
89.6
15
78.9
143.8
104.1
15
90.2
100.4
95.6
120
45.3
152.8
100.8
8:2FTS
18
60.1
107.6
81.7
18
80.2
140.5
109.6
18
54.6
107.4
99.4
143
54.6
151.8
103.7
PFOSA
18
68
113.1
85.7
18
81
108.5
97
18
47.5
770
205.4
138
47.5
770
113.8
NMeFOSA
18
63
92
80.6
18
73
102
83.9
18
47.6
115.5
87.3
138
32.8
164
87.9
NEtFOSA
18
63
91
75.5
18
69
97.5
81.7
18
45.5
114
86.5
136
23.5
168
85.6
NMeFOSAA
18
66
202
121.9
18
100
183
140.9
18
52
194.5
128.8
131
52
535
144.7
NEtFOSAA
18
69
211.5
126.7
18
90
174
125.9
18
58
237
126.6
140
58
400
140.1
NMeFOSE
17
49.8
87.5
73.4
18
70.6
113.1
85.5
18
46.1
106.9
77.8
134
34.2
126.9
81.5
NEtFOSE
17
53.4
77.5
67.6
18
68.8
110
81.9
17
46.8
106.2
76.9
131
21.9
135.6
80.6
PFMPA
18
23.5
84
50
18
68.2
92.2
81
18
20.2
90.3
69.4
142
15.2
116.8
81.3
PFMBA
18
48.8
92.2
72.3
18
91.5
100.5
95.4
18
45.2
123.5
92.1
142
45.2
163.2
104.3
NFDHA
18
55.8
155
119.5
18
37.5
81.2
65.4
18
45.8
91.5
78.5
143
25.8
155
91.6
HFPO-DA
18
70.8
102.9
85.1
18
89.4
101.9
93.6
18
46.4
97.1
90.2
143
46.4
228.8
104.5
ADONA
18
53.4
89
70.2
18
108
134.7
117.1
18
47.9
107.5
94.9
143
47.9
446.4
110.3
PFEESA
18
64.1
106.5
86.2
18
86.8
98.8
92.7
18
47.6
97.3
89.3
143
45.9
159.6
94.5
9C1-PF30NS
18
44
80.4
61.8
18
67.6
155.7
107.8
18
47.8
109.2
94.1
143
9.9
447.1
100.5
1 lCl-PF30UdS
18
28.7
72.6
49.7
18
38
132.2
74.5
18
37.8
94.4
69.1
141
3.7
313
72.2
3:3FTCA
18
53.5
95.5
76.7
18
71.8
97.5
87.3
18
52.6
157.5
105.1
142
40.4
157.5
89.5
5:3FTCA
18
68.4
130
95.9
18
76.8
121.7
98.1
18
54.2
165
119
143
54.2
302.5
100.6
7:3FTCA
18
75
121.7
90.4
18
84.2
125.8
101.9
18
46.8
136.7
100.3
143
24.6
301.7
99.3
-------
Table E-4. Summary of wastewater spike percent recoveries in high spike samples for each laboratory.
Analyte
Lab 1 spike % recover
y
Lab 2 spike % recover
y
Lab 3 spike % recover
y
Lab 4 spike % recover
y
Lab 5 spike % recover
y
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
18
92.8
106.8
100.6
18
100.8
131.4
109.9
18
22.5
114.7
104.3
13
101.8
112.7
106.8
17
82.1
94.5
88.5
PFPeA
18
81.5
113
96.4
18
97.5
137.9
112.4
18
22.2
119.2
103.1
18
93.3
105.4
98.5
18
82
97.6
90.6
PFHxA
18
83.4
110
94.3
18
89.9
118.2
101.1
18
32.2
120.2
100
18
88.3
110.3
97.8
18
62.3
115.4
89.9
PFHpA
18
81.8
102
92.1
18
95.5
117.6
104.5
18
21.1
105.9
93.4
18
85.6
105.2
95
18
75.5
105.5
92.1
PFOA
18
87.4
104
97.7
18
100
120.2
105.8
18
21.6
125.8
108.4
18
88.2
107.3
95.8
18
96.2
132.2
108.8
PFNA
18
80.1
97.9
89.3
18
99.8
121
106.7
18
19.5
141.2
106.7
18
90.2
101.3
96.2
18
70
104.7
87.8
PFDA
18
88.6
110
101.2
18
89.2
122
99.6
18
22.7
120.8
98.6
18
88
105
96.9
18
73.9
105
88
PFUnA
18
72.5
107
89.3
18
70.1
123
98.3
18
27
124
101.8
18
84.4
101
94.2
18
75.3
109
88.6
PFDoA
18
65.7
91.6
79.7
18
39.6
101
83.2
18
28.5
140
93.1
18
86.4
107
95.3
17
63.8
90.6
79.4
PFTrDA
18
62.1
101
82.3
18
17.3
95.8
61.6
18
26
144
85.3
18
84.4
105
93.5
17
57
87
74
PFTeDA
18
77
118
93.4
18
22.9
118
84.2
17
24.6
157
113.7
18
92.9
113
101.5
16
80.5
109
91.8
PFBS
18
86.5
98.4
91.8
18
97.8
120.6
105
18
21.8
120
104.4
18
93.8
111.2
101.6
18
79.8
91.3
85.3
PFPeS
18
87.3
108
96.8
18
96.9
123.8
104.4
18
22.4
122
98.9
18
91.8
110
98
18
84.8
116.3
94.1
PFHxS
18
81.6
95.9
89.5
18
82.5
126
101.4
18
23.4
112.5
98.3
18
91.4
108
100.7
18
99.7
110.9
105
PFHpS
18
85.2
103
93.8
18
95.6
136
109.6
18
22.3
156
104.9
18
88.7
111
100
18
79.7
143.3
93.9
PFOS
18
92.4
110.3
100
18
96
118
103.7
18
25.3
134
102.1
18
85.9
110.5
96.3
18
86.9
115.7
93.9
PFNS
18
70.8
103
86.9
18
65.6
95.7
79.8
18
19.4
110
91.4
18
80.9
106
94.5
18
54.8
90.1
80.1
PFDS
18
35
95.5
69.7
18
35.6
83.3
56.6
18
17.3
112
86.7
18
73.7
96.4
84.7
18
26.9
95
68.3
PFDoS
18
17
71.7
47
18
11.3
67.4
35.3
18
3
103
70.5
18
59.3
96.9
77
18
5.3
56.7
35.6
4:2FTS
18
91.7
110.4
102.7
18
92.9
120
103.5
18
34
108.7
96.1
18
80
117.1
92.2
18
91.2
101.7
96.6
6:2FTS
18
79.6
104.6
94.8
15
100.5
123.4
109.5
15
100.4
115.3
107.3
15
91.3
112.3
101.4
15
94.6
109.6
100
8:2FTS
18
91.7
113.8
101.3
18
97.1
124.6
107.8
18
47.9
147.5
121.4
18
82.1
111.7
98.7
18
92.9
111.4
104.4
PFOSA
18
91.2
110
99.3
18
73.2
130
100.5
18
25.8
124
104.7
18
92.5
130
105.2
14
81
101.3
88.4
NMeFOSA
17
75.4
99.1
84.3
18
37.6
101
79.6
18
39
212
99.5
18
59
122
91
16
82.1
99.7
93
NEtFOSA
17
75.6
94.8
86.5
18
23.4
93.6
75
18
38.7
193
99.3
18
67.3
124
95.9
16
80.3
97.3
91
NMeFOSAA
18
81
125
101.2
18
79.7
138
116
6
126
165.3
138.2
18
89.3
200.8
134.9
18
89
115.2
101
NEtFOSAA
18
72.6
112
94.9
18
64.9
139
110.4
18
30.6
182
117.2
18
96.8
206
124.2
17
94.2
119
103.9
NMeFOSE
18
76.2
97.5
86.1
18
37
96.2
76.1
18
59.2
134.8
89.5
18
62.5
104.5
88.1
16
76.5
114.2
93.8
NEtFOSE
17
70.8
93.5
82.7
18
25.8
96
72
18
60.5
136.5
94.2
18
62.3
109.5
90.1
16
77.2
107.2
89.8
PFMPA
18
59.5
99
85.6
18
81
111.5
98.8
18
20.9
104.5
90
18
17.5
106
77.7
18
37.4
118
82.2
PFMBA
18
86
115
97.6
18
97
135.5
108.8
18
24.5
138
116.7
18
97.5
141.5
110.4
18
111.5
175
132.1
NFDHA
18
73
104.5
88.9
18
54
122.5
91.4
18
19.6
123.5
93.7
18
52.5
114.5
81.5
18
88.5
114
101.1
HFPO-DA
18
94.2
110
101.7
18
109.2
198.3
135.9
18
35.6
108.7
95.8
18
89.6
120.4
103.9
18
93.8
116.3
103.8
ADONA
18
90.8
111.7
100.3
18
109.6
216.2
141.1
18
35.1
116.7
97.3
18
94.6
132.5
110.4
18
91.2
126.2
107.9
PFEESA
18
85.5
99.5
92.4
18
44.8
96
79
18
21.4
117.5
91.1
18
91
108.5
99
18
85.5
119
100.1
9C1-PF30NS
18
95.4
124.2
112.1
18
71.7
170.4
116.8
18
33.1
104.2
84.6
18
94.2
143.8
109.3
18
21.1
135.8
101.1
1 lCl-PF30UdS
18
37.2
105.8
77.1
18
26.2
101.2
60.7
18
7
106.2
73.1
18
74.6
127.1
97
18
5.7
115.4
75.7
3:3FTCA
18
51.7
93.8
79.2
18
62.3
105.5
86.1
18
20.6
116
97.8
18
60
131.5
103.1
18
35.2
173.2
94.5
5:3FTCA
18
75
89.5
81.4
18
63
133
100.7
18
6.3
110.5
86.1
18
90
115
101.7
18
61
117.5
94.6
7:3FTCA
18
82.5
95
89.4
18
71
195
107.3
18
6.6
153.5
107.2
18
73.5
105
93.3
18
22
120
84.6
-------
Table E-4. Summary of wastewater spike percent recoveries in high spike samples for each laboratory.
Analyte
Lab 1 spike % recover
y
Lab 2 spike % recover
y
Lab 3 spike % recover
y
Lab 4 spike % recover
y
Lab 5 spike % recover
y
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
18
92.8
106.8
100.6
18
100.8
131.4
109.9
18
22.5
114.7
104.3
13
101.8
112.7
106.8
17
82.1
94.5
88.5
PFPeA
18
81.5
113
96.4
18
97.5
137.9
112.4
18
22.2
119.2
103.1
18
93.3
105.4
98.5
18
82
97.6
90.6
PFHxA
18
83.4
110
94.3
18
89.9
118.2
101.1
18
32.2
120.2
100
18
88.3
110.3
97.8
18
62.3
115.4
89.9
PFHpA
18
81.8
102
92.1
18
95.5
117.6
104.5
18
21.1
105.9
93.4
18
85.6
105.2
95
18
75.5
105.5
92.1
PFOA
18
87.4
104
97.7
18
100
120.2
105.8
18
21.6
125.8
108.4
18
88.2
107.3
95.8
18
96.2
132.2
108.8
PFNA
18
80.1
97.9
89.3
18
99.8
121
106.7
18
19.5
141.2
106.7
18
90.2
101.3
96.2
18
70
104.7
87.8
PFDA
18
88.6
110
101.2
18
89.2
122
99.6
18
22.7
120.8
98.6
18
88
105
96.9
18
73.9
105
88
PFUnA
18
72.5
107
89.3
18
70.1
123
98.3
18
27
124
101.8
18
84.4
101
94.2
18
75.3
109
88.6
PFDoA
18
65.7
91.6
79.7
18
39.6
101
83.2
18
28.5
140
93.1
18
86.4
107
95.3
17
63.8
90.6
79.4
PFTrDA
18
62.1
101
82.3
18
17.3
95.8
61.6
18
26
144
85.3
18
84.4
105
93.5
17
57
87
74
PFTeDA
18
77
118
93.4
18
22.9
118
84.2
17
24.6
157
113.7
18
92.9
113
101.5
16
80.5
109
91.8
PFBS
18
86.5
98.4
91.8
18
97.8
120.6
105
18
21.8
120
104.4
18
93.8
111.2
101.6
18
79.8
91.3
85.3
PFPeS
18
87.3
108
96.8
18
96.9
123.8
104.4
18
22.4
122
98.9
18
91.8
110
98
18
84.8
116.3
94.1
PFHxS
18
81.6
95.9
89.5
18
82.5
126
101.4
18
23.4
112.5
98.3
18
91.4
108
100.7
18
99.7
110.9
105
PFHpS
18
85.2
103
93.8
18
95.6
136
109.6
18
22.3
156
104.9
18
88.7
111
100
18
79.7
143.3
93.9
PFOS
18
92.4
110.3
100
18
96
118
103.7
18
25.3
134
102.1
18
85.9
110.5
96.3
18
86.9
115.7
93.9
PFNS
18
70.8
103
86.9
18
65.6
95.7
79.8
18
19.4
110
91.4
18
80.9
106
94.5
18
54.8
90.1
80.1
PFDS
18
35
95.5
69.7
18
35.6
83.3
56.6
18
17.3
112
86.7
18
73.7
96.4
84.7
18
26.9
95
68.3
PFDoS
18
17
71.7
47
18
11.3
67.4
35.3
18
3
103
70.5
18
59.3
96.9
77
18
5.3
56.7
35.6
4:2FTS
18
91.7
110.4
102.7
18
92.9
120
103.5
18
34
108.7
96.1
18
80
117.1
92.2
18
91.2
101.7
96.6
6:2FTS
18
79.6
104.6
94.8
15
100.5
123.4
109.5
15
100.4
115.3
107.3
15
91.3
112.3
101.4
15
94.6
109.6
100
8:2FTS
18
91.7
113.8
101.3
18
97.1
124.6
107.8
18
47.9
147.5
121.4
18
82.1
111.7
98.7
18
92.9
111.4
104.4
PFOSA
18
91.2
110
99.3
18
73.2
130
100.5
18
25.8
124
104.7
18
92.5
130
105.2
14
81
101.3
88.4
NMeFOSA
17
75.4
99.1
84.3
18
37.6
101
79.6
18
39
212
99.5
18
59
122
91
16
82.1
99.7
93
NEtFOSA
17
75.6
94.8
86.5
18
23.4
93.6
75
18
38.7
193
99.3
18
67.3
124
95.9
16
80.3
97.3
91
NMeFOSAA
18
81
125
101.2
18
79.7
138
116
6
126
165.3
138.2
18
89.3
200.8
134.9
18
89
115.2
101
NEtFOSAA
18
72.6
112
94.9
18
64.9
139
110.4
18
30.6
182
117.2
18
96.8
206
124.2
17
94.2
119
103.9
NMeFOSE
18
76.2
97.5
86.1
18
37
96.2
76.1
18
59.2
134.8
89.5
18
62.5
104.5
88.1
16
76.5
114.2
93.8
NEtFOSE
17
70.8
93.5
82.7
18
25.8
96
72
18
60.5
136.5
94.2
18
62.3
109.5
90.1
16
77.2
107.2
89.8
PFMPA
18
59.5
99
85.6
18
81
111.5
98.8
18
20.9
104.5
90
18
17.5
106
77.7
18
37.4
118
82.2
PFMBA
18
86
115
97.6
18
97
135.5
108.8
18
24.5
138
116.7
18
97.5
141.5
110.4
18
111.5
175
132.1
NFDHA
18
73
104.5
88.9
18
54
122.5
91.4
18
19.6
123.5
93.7
18
52.5
114.5
81.5
18
88.5
114
101.1
HFPO-DA
18
94.2
110
101.7
18
109.2
198.3
135.9
18
35.6
108.7
95.8
18
89.6
120.4
103.9
18
93.8
116.3
103.8
ADONA
18
90.8
111.7
100.3
18
109.6
216.2
141.1
18
35.1
116.7
97.3
18
94.6
132.5
110.4
18
91.2
126.2
107.9
PFEESA
18
85.5
99.5
92.4
18
44.8
96
79
18
21.4
117.5
91.1
18
91
108.5
99
18
85.5
119
100.1
9C1-PF30NS
18
95.4
124.2
112.1
18
71.7
170.4
116.8
18
33.1
104.2
84.6
18
94.2
143.8
109.3
18
21.1
135.8
101.1
1 lCl-PF30UdS
18
37.2
105.8
77.1
18
26.2
101.2
60.7
18
7
106.2
73.1
18
74.6
127.1
97
18
5.7
115.4
75.7
3:3FTCA
18
51.7
93.8
79.2
18
62.3
105.5
86.1
18
20.6
116
97.8
18
60
131.5
103.1
18
35.2
173.2
94.5
5:3FTCA
18
75
89.5
81.4
18
63
133
100.7
18
6.3
110.5
86.1
18
90
115
101.7
18
61
117.5
94.6
7:3FTCA
18
82.5
95
89.4
18
71
195
107.3
18
6.6
153.5
107.2
18
73.5
105
93.3
18
22
120
84.6
-------
Table E-5. Summary of wastewater EIS percent recovery for each laboratory.
Analyte
Lab 1 % recovery
Lab 2 % recovery
Lab 3 % recovery
Lab 4 % recovery
Lab 5 % recovery
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
13c4-pfba
42
22.4
130
74.2
42
39.1
92.6
73.2
42
13
291
83.5
42
1
84.9
43.5
42
8.44
83.8
45.4
13C5-PFPeA
42
72
127
89.3
42
55.4
105
85.5
42
46
244
79.5
42
2.1
87.8
69
42
45.4
85.8
68.7
13C5-PFHxA
42
80.6
127
91.8
42
58.8
96.3
85.4
42
66
306
98.8
42
28.3
86.3
75.6
42
48
97.2
74.7
13C4-PFHpA
42
75.5
123
88.3
42
49.4
113
80.9
42
67
350
110.3
42
64.7
85.4
75.4
42
31.1
90.8
72.6
13C8-PFOA
42
77.7
135
93.4
43
55.9
100
82.2
42
68
268
95.4
42
66
86.1
77.2
42
25.9
105
77.6
13c9-pfna
42
79.5
134
91.8
42
49.2
97.4
81.6
42
58
266
94.6
42
68.5
87.2
77.8
42
12.2
110
73.6
13c6-pfda
42
74.2
134
91.1
42
43.9
94.6
77.9
42
47
302
90
42
60.1
84.7
72.7
42
2.68
92
67.6
13C7-PFUnA
42
43.7
101
79.5
42
29.3
82.6
65.7
42
26
278
81.9
42
38
82.6
71
42
0.617
96.8
60.7
13C2-PFDoA
42
26.2
97.5
67.3
42
12.3
75.3
52.8
42
15
282
90.8
42
10.6
77.2
63
42
0.563
85.6
53.6
13C2-PFTeDA
42
8.9
85
44.9
42
0.242
56.7
32.3
42
1
130
52.1
42
0.5
69.2
51.9
42
0.0848
57.5
27.8
13c3-pfbs
42
82
119
92.4
42
54.4
94.1
83.8
42
58
273
86.4
42
19
88.6
75.6
42
40.9
85
69.4
13C3-PFHxS
42
82.5
134
93.6
42
51
97.7
85.4
42
59
337
99.2
42
66.8
88.5
75.8
42
11.8
83.1
68.5
13c8-pfos
42
70.1
120
84.2
42
34.3
89.1
77.1
42
48
288
94.2
42
61.1
82.7
73.1
42
0.251
83.8
56.9
13C2-4:2FTS
42
112
175
136.8
42
128
546
298.4
42
111
550
165.5
42
45.7
155
105.5
42
78.3
194
136.7
13C2-6:2FTS
42
65.7
187
136.4
42
68
426
199
42
58
328
103.8
42
69.8
125
91
42
18.6
132
95.5
13C2-8:2FTS
42
93.9
378
157.9
42
48.3
439
218.3
42
54
428
130.1
42
61.8
390
139.6
42
2.52
285
118.1
13c8-pfosa
42
9.96
91.2
66.2
42
27.6
98.4
70.9
42
57
282
88.2
42
49.6
72.7
59.8
42
0.122
64
43.2
D3-NMeFOSA
42
7.4
67.2
44.6
42
11.9
65.3
46.1
42
24
225
69.8
42
28.1
61.2
46.2
42
1.43
52.4
28.2
D5-NEtFOSA
42
9.07
63.8
39.5
42
7.44
50.8
34.6
42
18
220
68.2
42
12.8
66.4
45.8
42
0.948
50.8
25.4
D3-NMeFOSAA
42
54.7
92.5
72.3
42
40.4
140
99.9
42
24
599
143.3
42
46.6
95.6
72.8
42
1.07
122
59.1
D5-NEtFOSAA
42
48.4
110
71.7
42
34.7
178
117.3
42
15
279
97
42
29.6
88.4
72.4
42
0.846
90.8
53.5
D7-NMeFOSE
42
8.13
72.4
42.4
42
8.7
94
46.7
42
35
299
89.1
42
0.1
70.4
54.7
42
0.396
65.2
29.3
D9-NEtFOSE
42
7.81
66
37.8
42
5.44
76.8
43.6
42
24
289
79.5
42
0.2
68.4
51.2
42
0.331
44
21.1
13C3-HFPO-DA
42
72.9
126
84.7
42
25.5
80.3
54.2
42
68
305
98.9
42
17.7
89.5
68
42
48.7
98
72.2
-------
Table E-5. Summary of wastewater EIS percent recovery for each laboratory.
Analyte
Lab 6 % recovery
Lab 7 % recovery
Lab 9 % recovery
All]
^ahs
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
13C4-PFBA 42
3.54
88.9
38
42
30
87
66.9
42
3
161
47.7
336
1
291
59.1
13C5-PFPeA 42
54
149
90.9
42
48
91
76.8
42
38
156
73.3
336
2.1
244
79.1
13C5-PFHxA 42
71.5
120
87.4
42
57
98
82
42
62
158
83.1
336
28.3
306
84.8
13C4-PFHpA 42
69.5
142
97.5
42
62
105
84.5
42
59
152
79.5
336
31.1
350
86.1
13C8-PFOA 42
64.5
115
86.8
42
62
107
84.3
42
63
157
84.4
337
25.9
268
85.1
13C9-PFNA 42
62.1
111
86
42
62
97
82.2
42
59
154
83.8
336
12.2
266
83.9
13C6-PFDA 42
66
132
88.6
42
59
90
78.6
42
52
148
80.7
336
2.68
302
80.9
13C7-PFUnA 42
57.1
119
81.1
42
48
78
64.3
42
31
126
75.9
336
0.617
278
72.5
13C2-PFDoA 42
40.4
134
79.7
42
44
71
57.1
42
11
109
63.1
336
0.563
282
65.9
13C2-PFTeDA 42
22.7
105
63.2
42
22
53
37.8
42
2
108
42.1
336
0.0848
130
44
13C3-PFBS 42
74.7
153
114
42
63
95
83
42
61
157
81.2
336
19
273
85.7
13C3-PFHxS 42
64.7
141
95.5
42
73
104
85.2
42
58
159
82.8
336
11.8
337
85.8
13C8-PFOS 42
64.6
108
82.9
42
57
89
77.1
42
49
150
79.9
336
0.251
288
78.2
13C2-4:2FTS 42
113
323
167.1
42
62
150
106.3
42
156
327
220.7
336
45.7
550
167.1
13C2-6:2FTS 42
68.7
282
145.2
42
56
135
91
42
92
226
148.6
336
18.6
426
126.3
13C2-8:2FTS 42
57.6
362
128.8
42
54
140
91.3
42
91
441
165.5
336
2.52
441
143.7
13C8-PFOSA 42
61
96
79.1
42
53
98
73.2
42
47
139
75.5
336
0.122
282
69.5
D3-NMeFOSA 42
38.4
80.5
59.8
42
40
65
50.3
42
19
83
52.2
336
1.43
225
49.7
D5-NEtFOSA 42
33
75.5
55.3
42
31
61
47.2
42
9
81
43.6
336
0.948
220
44.9
D3-NMeFOSAA 42
65.8
116
91.4
42
65
143
95.9
42
46
140
81.9
336
1.07
599
89.6
D5-NEtFOSAA 42
63
142
89.9
42
66
138
95.2
42
26
132
80.1
336
0.846
279
84.6
D7-NMeFOSE 42
2.82
92
56
42
34
59
45.6
42
0.252
86
39.7
336
0.1
299
50.4
D9-NEtFOSE 42
2.65
80
51.4
42
25
59
43.9
42
0.145
68
29.3
336
0.145
289
44.7
13C3-HFPO-DA 42
75.6
171
111.5
42
44
84
68.6
42
59
156
79.3
336
17.7
305
79.7
-------
PFAS Multi-Laboratory Validation Study Report
Aqueous Media: Wastewater, Surface Water, and Groundwater
SERDP
Appendix F
Surface Water Supporting
Tables
Date: July 25, 2023
-------
Appendix F: List of Tables
F1 Target analytes detected in unspiked wastewater samples by kaboratory
F2 Minimum and maxium target analytes concentrations in unspiked wastewater samples
F3 Summary of wastewater spike percent recoveries in low spike samples for each laboratory.
F4 Summary of wastewater spike percent recoveries in high spike samples for each laboratory.
F5 Summary of wastewater EIS percent recovery for each laboratory.
-------
Table F-l. Target Analytes Detected in Unspiked Surface Water Samples by Laboratory (ng/L)
Analyte
Number
of Labs
Lab 1
Lab 2
Lab 3
Lab 4
Lab 5
Lab 6
Lab 7
Lab 9
Lab 10
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
Cone
Qual
SU D -SU Oil!) If)
PFBA
9
0.941
U
4.05
J
2.56
J
1.31
U
2.23
J
0.597
U
6.5
J
2.99
J
2.53
J
PFPeA
9
0.552
U
1.7
JI
1.12
J
0.306
U
1.26
J
0.563
U
1
J
1.1
IJ
0.549
U
PFHxA
9
1.65
J
2.02
J
1.04
JI
1.32
J
1.02
J
0.412
u
1.1
J
1.16
0.298
U
PFHpA
9
0.849
J
1.66
J
0.8
J
0.788
JI
0.845
J
0.173
u
0.66
J
0.785
J
1.02
J
PFOA
9
1.89
J
--
X
1.2
J
1.12
J
1.17
J
1.28
J
1
J
1.18
1.33
J
PFNA
9
0.657
u
--
X
1.28
J
0.332
J
0.792
U
0.25
u
0.61
U
0.331
J
0.565
J
PFBS
9
0.736
J
1.18
JI
1.36
J
0.94
J
0.348
U
0.177
u
0.78
J
0.879
J
1.22
JI
PFHxS
9
0.393
u
--
X
0.464
U
0.789
u
0.625
u
0.291
u
0.7
U
0.363
J
0.567
u
PFOS
9
0.978
J
--
X
1.28
J
1.7
u
1.43
JI
0.96
J
0.54
u
0.977
J
0.415
u
6:2FTS
9
1.07
u
--
X
2.82
U
1.6
u
2.39
J
1.48
u
3.5
u
0.945
U
2.36
UJ
PFOSA
9
0.346
u
--
X
0.416
u
0.565
u
0.198
u
0.188
u
0.67
u
11.1
0.212
u
.S'll / '- !lurh'\Crook
PFBA
9
0.941
u
1.93
J
1.04
u
--
X
1.47
J
--
X
1.9
u
--
X
0.952
u
PFPeA
9
0.552
u
1.08
u
0.768
u
0.306
u
0.772
u
0.563
u
0.94
u
0.726
J
0.549
u
PFHxA
9
0.454
u
1.45
u
0.8
J
0.768
J
0.604
J
0.412
u
0.67
J
0.704
J
0.298
u
PFHpA
9
0.501
u
1.06
u
0.4
J
0.382
J
0.76
u
0.173
u
0.44
u
0.415
J
0.519
u
PFOA
9
1.5
J
2.93
J
0.88
J
0.924
J
1.09
J
0.29
u
0.74
J
0.932
J
1.09
J
PFBS
9
0.801
J
1.08
u
1.04
JI
0.628
u
0.717
J
0.177
u
0.66
J
0.928
J
0.292
JI
PFPeS
9
0.425
J
1.31
u
0.272
u
0.502
JI
0.729
u
0.129
u
1.1
u
0.399
IJ
0.468
u
PFHxS
9
0.835
J
1.43
u
1.04
J
0.968
J
0.679
J
0.784
J
0.79
J
0.912
J
0.824
J
PFOS
9
0.441
u
1.68
u
0.64
J
1.7
u
0.486
u
0.248
u
0.54
u
0.563
J
0.415
u
PFOSA
9
0.346
u
0.724
u
0.416
u
0.565
u
0.198
u
0.188
u
0.67
u
12.3
0.212
u
NEtFOSAA
9
0.554
u
2.26
u
0.88
J
0.61
u
0.531
u
0.571
u
1.3
u
0.283
u
0.693
u
.S irr; - Sci/nim Somvulor
PFHxA
9
0.454
u
1.45
u
0.472
u
0.455
u
0.509
J
0.412
u
0.39
u
0.493
J
0.298
u
PFOA
9
0.367
u
1.78
u
0.696
u
0.651
u
0.427
u
0.29
u
0.46
u
0.189
J
0.634
u
PFHxS
9
0.393
u
1.43
u
0.384
u
0.789
u
0.625
u
0.291
u
0.7
u
0.189
J
0.567
u
PFOSA
9
0.346
u
0.724
u
0.432
u
0.565
u
0.198
u
0.188
u
0.67
u
13.6
0.212
u
Compounds undetected in all samples included: PFDA, PFUnA, PFDoA, PFTrDA, PFTeDA, PFHpS, PFNS, PFDS, PFDoS, 4:2FTS, 8:2FTS, NMeFOSA, NEtFOSA, NMeFOSAA, NMeFOSE,
NEtFOSE, PFMPA, PFMBA, NFDHA, HFPO-DA, ADONA, PFEESA, 9CI-PF30NS, llCI-PF30UdS, 3:3FTCA, 5:3FTCA, 7:3FTCA
-------
Table F-2. Minimum and Maximum Detected Values Reported
)y all Laboratories
Analyte
Number
SWD1
SWF1
SWG1
of Labs
Min
Max
Min
Max
Min
Max
PFBA
9
0.597 U
6.5 J
0.941 U
1.93 J
0.545 U
1.9 U
PFPeA
9
0.306 U
1.7 JI
0.306 U
0.726 J
0.289 U
1.08 U
PFHxA
9
0.298 U
2.02 J
0.298 U
0.8 J
0.298 U
0.509 J
PFHpA
9
0.173 U
1.66 J
0.173 U
0.415 J
0.158 U
1.06 U
PFOA
9
1 J
1.89 J
0.29 U
2.93 J
0.29 U
0.189 J
PFNA
9
0.25 U
1.28 J
0.166 U
1.06 U
0.166 U
1.06 U
PFBS
9
0.177 U
1.36 J
0.177 U
1.04 JI
0.104 U
1.08 U
PFPeS
9
0.116 U
1.1 U
0.129 U
0.502 JI
0.116 U
1.31 U
PFHxS
9
0.291 U
0.363 J
1.43 U
1.04 J
0.291 U
0.189 J
PFOS
9
0.415 U
1.43 JI
0.248 U
0.64 J
0.248 U
1.7 U
6:2FTS
9
0.945 U
2.39 J
0.945 U
7.92 U
0.945 U
7.92 U
PFOSA
9
0.188 U
11.1
0.188 U
12.3
0.188 U
13.6
NEtFOSAA
9
0.283 U
1.3 U
0.283 U
0.88 J
0.283 U
2.26 U
'or Unspiked Samples
-------
Table F-3. Summary of surface water spike percent recoveries in low spike samples for each laboratory.
Analyte
Lab 1 spike % recover
y
Lab 2 spike % recover
y
Lab 3 spike % recover
y
Lab 4 spike % recover
y
Lab 5 spike % recover
y
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
9
18.8
101
85.9
6
90.3
98.8
94.5
9
75.8
103.3
94.3
6
91.2
102.5
97.0
9
78.7
91.2
86.6
PFPeA
9
93.2
100
97.4
9
89.2
98.2
93.6
9
92.8
104.5
100.0
9
96.8
108.2
103.1
9
81.4
101.2
90.0
PFHxA
9
86
373.8
123.4
9
92.9
103
98.9
9
87
101
95.1
9
93
108.2
98.1
9
74
99.5
91.1
PFHpA
9
65.3
97.5
88.8
9
101.2
113
107.1
9
94
99
96.7
9
87
103
93.3
9
77.3
97.5
90.0
PFOA
9
86
388
126.1
6
98.8
113
105.5
9
89.5
111
99.4
9
95.4
109
99.8
9
86.6
115.6
97.6
PFNA
9
4.1
106.5
83.2
9
93
106
100.7
9
87
112.1
97.4
9
91
105.3
98.4
9
77
108.5
92.6
PFDA
8
86
100.5
90.0
9
86
101
94.7
9
91.5
128.5
113.3
9
92.5
113
104.2
9
73.5
99.5
84.4
PFUnA
8
82
102.5
92.3
8
91
98.5
95.2
9
74
121
95.9
9
96
112.5
100.6
9
84
110
94.3
PFDoA
8
73.5
103
85.5
8
84.5
95.5
90.1
9
75.5
93
86.2
9
90.5
101
96.8
9
65.5
88.5
81.8
PFTrDA
8
85.5
105.5
92.6
8
63
83
74.2
9
68.5
101
82.2
9
86.5
94
91.4
9
49.6
95.5
82.7
PFTeDA
8
82.5
102.5
91.9
8
75.5
84
80.6
9
75
100
88.3
9
91.5
99.5
94.8
9
76
105
90.7
PFBS
9
81
166.3
95.1
9
91.6
105
97.3
9
82.3
100.2
90.8
9
94.3
108.5
101.6
9
75.9
89.5
82.8
PFPeS
9
84
147
96.4
9
93.1
135.6
100.5
9
88.1
107.9
97.9
9
98
112.4
102.5
9
81.2
91.6
85.9
PFHxS
9
86.1
1447.8
239.9
9
94.5
104
98.9
9
92
112.4
99.9
9
100.5
113.1
107.2
9
73.2
92.5
81.7
PFHpS
9
20.8
100.5
83.7
5
97.5
121.5
109.7
9
101
134.5
114.8
9
87.5
114.5
99.8
9
82
103
90.7
PFOS
9
86
1095.1
204.0
8
98
125.5
109.5
9
85
116.6
100.1
9
88.5
108.5
98.9
9
83.9
97
89.2
PFNS
8
77.7
94.6
87.1
8
57.4
99.5
83.2
9
76.7
100.5
91.3
9
80.7
98
89.0
9
70.3
85.6
76.8
PFDS
8
74.2
84.3
79.8
5
36.1
89.4
65.8
9
48.9
85.9
75.0
9
74.2
97
84.3
9
74.7
91.4
81.1
PFDoS
8
59.8
76.9
67.1
8
14.6
66.8
51.8
9
34.2
76.9
64.1
9
73.9
100
80.8
9
44
66.3
52.6
4:2FTS
8
74.4
99.2
89.1
9
77
93.5
87.1
9
87.1
108.2
98.3
9
80.9
108
93.5
9
91.8
99.4
94.8
6:2FTS
9
15.4
101
86.8
9
106.4
130
115.4
9
94.9
102.8
97.8
9
90.4
111.5
103.4
9
93.1
106.5
101.1
8:2FTS
8
92.5
104
98.0
9
85.9
120.8
105.3
9
97.6
121.1
110.8
9
101.1
117.2
110.6
9
95.6
105.4
102.8
PFOSA
8
87
103.5
96.0
9
91
106
98.8
9
85
148
113.3
9
93.5
117.5
103.5
9
83
98
89.4
NMeFOSA
8
79
91.5
84.6
8
85.5
102.5
95.7
9
75
103
89.1
9
74.5
101.5
91.8
9
90.5
99.5
96.3
NEtFOSA
8
77
97
86.1
8
85
101
89.7
9
71
101.5
86.8
9
78.5
104
88.7
9
86
95.5
92.1
NMeFOSAA
8
95
222.5
132.8
9
89.5
205.5
138.5
9
92.5
280.5
168.4
9
97
253.5
156.0
9
89.5
198
126.2
NEtFOSAA
8
85.5
289
142.8
8
91
242.5
153.7
9
87
321.5
169.8
9
93.5
302.5
170.6
9
92
283
153.3
NMeFOSE
8
74.4
91.2
84.5
8
73.1
88.1
82.3
9
62.1
88.8
77.8
9
75.6
97.5
86.7
9
76.2
112.5
95.7
NEtFOSE
8
57.8
88.1
78.2
5
82.5
87.5
84.5
9
50.9
91.9
72.7
9
65
92.5
80.0
9
70.6
110.6
91.6
PFMPA
8
48.5
98.8
77.5
9
21.2
59
40.7
9
78.5
92
87.3
9
10.2
79.8
51.7
9
68.5
114.5
92.3
PFMBA
8
90.5
106.5
99.1
9
95.7
112.5
103.3
9
83.5
100.7
93.4
9
98
130
108.1
9
106.8
124
115.5
NFDHA
8
83
98.8
91.5
9
70.8
102.8
86.0
9
84.5
101.8
90.9
9
85.2
125.7
105.8
9
93.5
123.8
109.2
HFPO-DA
8
86.2
101.8
95.3
9
101.8
122.8
110.8
9
90.8
114.1
102.1
9
79
116.1
93.4
9
90
116.6
104.2
ADONA
8
94.1
99
96.6
9
97.5
127.2
111.9
9
85.7
105.4
95.2
9
93.9
109.2
100.7
9
90.3
124.2
106.0
PFEESA
8
99
112.7
104.1
9
91.3
100.7
97.4
9
93.3
121.9
105.0
9
93.5
112
103.7
9
84
101
91.7
9C1-PF30NS
8
90
103.7
96.4
8
53.2
113
91.2
9
69.6
101.9
89.8
9
91
106.7
98.9
9
89.4
118.7
105.1
llCl-PF30UdS
8
78.6
86.5
82.8
8
18.8
83.2
61.7
9
29.4
80.9
63.4
9
74.1
93
84.8
9
81.2
110.8
98.4
3:3FTCA
8
38.9
86.8
66.0
9
29.1
72.5
53.3
9
74.8
95
88.3
9
59.2
102.1
86.6
9
46.8
83.4
70.2
5:3FTCA
8
74.5
94.2
82.6
9
87.5
108.3
99.6
9
85
96.7
92.0
9
85
106.7
97.4
9
85
101.7
94.0
7:3FTCA
8
66.1
90.8
79.4
9
68.8
102.5
92.0
9
73.5
98.3
84.0
9
64.2
101.7
87.3
9
66.6
91.7
80.9
-------
Table F-3. Summary of surface water spike percent recoveries in low spike samples for each laboratory.
Analyte
Lab 6 spike % recover
y
Lab 7 spike % recover
y
Lab 9 spike % recover
y
Lab 10 spike % recovery
All Labs
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
6
0.9
83
67.0
9
87.9
98.9
93.5
6
88.8
95.5
93.5
9
104.7
116.6
111.2
69
0.9
116.6
92.1
PFPeA
9
4.4
101.5
74.5
9
89.5
100.5
94.5
9
88.2
96.2
93.5
9
88.5
118
106.6
81
4.4
118
94.8
PFHxA
9
72
91.5
83.6
9
85.1
96.5
90.9
9
89.5
97.5
93.2
9
97.5
128
111.9
81
72
373.8
98.5
PFHpA
9
70.5
90
79.2
9
83
91
87.7
9
85.4
94
90.3
9
91.5
124
111.3
81
65.3
124
93.8
PFOA
9
75
84.5
78.9
9
88.3
99.5
92.7
9
83.8
90.6
86.9
9
99.6
142
117.1
78
75
388
100.3
PFNA
9
63
82.5
74.4
9
89.5
125
104.3
9
86.5
96.5
92.3
9
92
133
110.2
81
4.1
133
94.8
PFDA
9
75.5
100
83.9
9
81
163.5
114.7
9
88.5
97
92.5
9
98.5
124.5
111.2
80
73.5
163.5
98.9
PFUnA
9
68
87.5
76.2
9
86
151
110.8
9
81
92
88.6
9
90
125.5
110.6
79
68
151
96.1
PFDoA
9
69.5
91
77.8
9
47.5
123.5
88.2
9
71.5
86.5
83.2
9
81
121.5
100.6
79
47.5
123.5
87.8
PFTrDA
9
66
106.5
86.4
9
43.5
100
74.4
9
63.5
81.5
75.1
8
89
109.5
99.1
78
43.5
109.5
84.1
PFTeDA
9
65.5
79.5
71.7
9
59
93.5
74.7
9
68
87.5
80.8
8
80
118.5
93.4
78
59
118.5
85.1
PFBS
9
57.5
87
72.8
9
85.2
103
92.5
9
89.4
98.6
93.9
9
100.5
116.5
108.2
81
57.5
166.3
92.8
PFPeS
9
62.4
96.5
74.3
9
81.7
102
94.3
9
82.2
101
95.6
9
96.5
135.6
112.3
81
62.4
147
95.5
PFHxS
9
63.3
93.5
77.2
9
86.6
102
92.8
9
83
95.7
90.5
9
83
119.9
99.9
81
63.3
1447.8
109.8
PFHpS
9
60.5
96
79.2
9
105.5
239.5
146.3
9
88
103
98.3
9
98.5
231.5
123.6
77
20.8
239.5
104.9
PFOS
9
65
86
76.3
9
92.5
218
132.6
9
83.7
95.2
90.3
9
98
139
109.8
80
65
1095.1
112.4
PFNS
9
62.4
82.2
72.0
9
58.9
121.8
90.0
9
78.2
92.6
85.7
9
42.8
102.5
89.4
79
42.8
121.8
84.9
PFDS
9
59.1
75.8
65.9
9
33.3
78.8
55.8
9
65.2
82.3
75.7
9
10.9
89.4
73.3
76
10.9
97
73.3
PFDoS
9
31.2
63.8
53.6
9
31.7
55.3
41.6
9
51.8
78.4
61.2
8
58.3
82.9
68.6
78
14.6
100
60.1
4:2FTS
9
55.5
121.2
83.5
9
75.7
95.6
86.8
9
91.2
96.9
94.8
9
85.6
128
104.7
80
55.5
128
92.6
6:2FTS
9
69.2
133.8
98.1
9
79.6
106.4
91.8
9
97.2
103.2
99.7
9
73.6
146.2
117.3
81
15.4
146.2
101.3
8:2FTS
9
65.2
113.8
83.4
9
103.3
204.5
129.6
9
98.2
105.6
102.6
9
110.8
145.5
124.5
80
65.2
204.5
107.6
PFOSA
9
71.5
85
80.3
9
92.5
153
112.6
9
88
211
123.2
9
101.5
141.5
120.7
80
71.5
211
104.3
NMeFOSA
9
68.5
93
79.4
9
75
135.5
101.6
9
86.5
96.5
89.7
9
68
112.5
95.7
79
68
135.5
91.6
NEtFOSA
9
65
86
71.1
9
64
133
94.8
9
76
96.5
88.4
9
81.5
118
96.1
79
64
133
88.2
NMeFOSAA
9
88
191
122.2
9
86
375.5
186.5
9
83
211.5
135.1
9
152.5
665
368.6
80
83
665
170.9
NEtFOSAA
9
74
235.5
127.8
9
70.5
479.5
203.9
9
75
269.5
146.1
9
116.5
785
366.7
79
70.5
785
182.5
NMeFOSE
7
56
80.6
69.4
9
53.5
104.4
78.3
9
64.4
93.1
74.5
8
34.1
87.5
65.4
76
34.1
112.5
79.7
NEtFOSE
6
46.9
96.9
74.9
9
41.2
78.8
61.0
9
59
94.4
73.1
8
24.8
86.2
63.0
72
24.8
110.6
75.1
PFMPA
9
11.7
66
40.2
9
72.2
88.8
79.8
9
13.8
68
46.2
9
66.2
115
89.6
80
10.2
115
67.1
PFMBA
9
65.3
102
81.9
9
93
98.2
95.2
9
92
145.5
105.7
9
88.5
116.8
101.9
80
65.3
145.5
100.5
NFDHA
9
53.8
115
90.1
9
82
94.8
88.8
9
70.5
90
84.3
9
94.8
114.8
104.4
80
53.8
125.7
94.6
HFPO-DA
9
71.9
93.1
82.0
9
84.4
97.2
91.9
9
90.6
96.4
93.6
9
106.4
130
117.4
80
71.9
130
99.0
ADONA
9
65.7
80.3
73.9
9
95.5
112.3
103.2
9
92.3
118.8
99.0
9
103.6
135.9
117.3
80
65.7
135.9
100.5
PFEESA
9
70.3
92.3
81.6
9
86.3
94.3
89.4
9
88.5
96.3
91.3
9
99.3
122.4
108.0
80
70.3
122.4
96.8
9C1-PF30NS
9
68.6
82.8
74.8
9
57
87.3
73.1
9
78.8
124.5
91.6
9
24.9
130.8
100.8
79
24.9
130.8
91.2
1 lCl-PF30UdS
9
47.9
67.7
60.1
9
18.6
42.8
28.5
9
55.1
105.5
70.6
8
76.6
94.9
84.7
78
18.6
110.8
70.3
3:3FTCA
9
49.1
79.9
66.8
9
70.4
89.2
79.6
9
17.5
80.5
60.9
9
76.2
104.2
90.1
80
17.5
104.2
73.6
5:3FTCA
9
72.1
84.2
78.8
9
74.3
90
82.6
9
54.2
90.8
80.1
9
66.3
111.7
89.2
80
54.2
111.7
88.6
7:3FTCA
9
57
74.1
66.3
9
63.4
85
75.9
9
51.4
92.5
75.6
9
30.8
96.7
68.6
80
30.8
102.5
78.9
-------
Table F-4. Summary of surface water spike percent recoveries in high spike samples for each laboratory.
Analyte
Lab 1 spike % recover
y
Lab 2 spike % recover
y
Lab 3 spike % recover
y
Lab 4 spike % recover
y
Lab 5 spike % recover
y
n
Mill
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
6
92.8
99.8
95.9
5
87.3
104
93.4
9
81
101.1
94.6
6
100.2
106.2
103.0
9
86.2
93.9
89.4
PFPeA
9
92
104
97.8
9
90
96.2
93.2
9
90
102
98.3
9
91
96.5
93.8
9
88.9
105
96.8
PFHxA
9
86.6
96.1
91.4
9
96
103
98.5
9
81.2
103.2
93.7
9
92.1
109
99.9
9
75.2
110.4
88.5
PFHpA
9
85.3
103
92.4
9
107
116
111.3
9
89.4
97.3
94.5
9
97.4
106
101.2
9
86.8
111
96.8
PFOA
9
89.3
98.5
94.1
8
102.1
118
110.9
9
91.8
109.1
100.0
9
93.8
110
98.9
9
101.9
126.8
117.3
PFNA
9
85.8
100
92.7
8
100
112
104.9
9
79.6
120
93.5
9
89.3
102
98.1
9
79.1
107
93.6
PFDA
9
86
98.2
91.4
8
93.1
102
98.1
9
93.5
135
107.2
9
90.2
106
97.1
9
74.7
100
90.8
PFUnA
9
79.5
97.6
90.0
8
93.8
101
97.8
9
81
115
94.2
9
84.1
96.3
91.5
9
77
92
84.3
PFDoA
9
72.5
93.5
81.2
8
88.9
98.7
93.5
9
78.1
99.8
86.9
9
88.1
99.7
94.0
9
61.9
101
84.7
PFTrDA
9
75.9
92.5
83.6
8
70.5
90.2
79.8
9
71.4
94.2
84.8
9
85.1
93.6
89.1
9
73.4
93.8
83.0
PFTeDA
9
76
95.7
86.9
8
79.1
94.4
85.5
9
84.1
109
95.9
9
86.5
95.8
92.1
9
74.1
101
85.9
PFBS
9
82.8
94
87.4
9
94.2
102.8
98.0
9
84.1
96.8
88.8
9
94.7
109.1
103.1
9
78.8
85.5
81.8
PFPeS
9
86.3
102.6
94.3
8
97
105
100.4
9
91.5
102
96.0
9
91.1
98.8
95.9
9
85.5
92.1
88.7
PFHxS
9
88.6
101
93.8
8
96.1
107
99.9
9
92.8
101
97.0
9
94.6
102
98.5
9
85.5
89.4
87.6
PFHpS
9
87.7
102
96.2
8
93.1
115
104.5
9
101
146
113.6
9
95.3
122
106.5
9
84.5
95.8
90.7
PFOS
9
90.3
101
97.8
8
102
117
110.5
9
89.9
118
99.9
9
91.2
109
99.0
9
86.7
98.2
92.5
PFNS
9
85.5
97.2
90.5
8
75.4
101
90.0
9
89.8
105
92.9
9
88.6
102
92.6
9
74.2
85.2
80.2
PFDS
9
70.4
86.9
81.8
8
63.2
88
77.4
9
66.6
92.6
77.3
9
79.8
92
85.4
9
80.8
94.7
87.4
PFDoS
9
50
78.9
65.5
8
42
79.3
60.0
9
62.2
98.6
73.2
9
73.3
97.4
83.5
9
42.6
69.5
58.5
4:2FTS
9
82.5
95.8
88.3
9
80.4
100.4
89.1
9
85.8
107.5
93.1
9
89.2
110.8
98.6
9
89.6
100.4
94.7
6:2FTS
9
90.9
101.3
96.7
8
113.4
130.5
119.5
9
95.5
99.2
96.8
9
99.2
114.6
107.0
9
97
137.8
107.6
8:2FTS
9
88.8
108.3
96.4
8
107.1
123.3
115.7
9
95.8
135
111.1
9
97.5
119.6
103.9
9
100.8
109.6
104.5
PFOSA
9
93.2
99.4
96.9
8
94.6
104
98.1
9
91.8
150
118.6
9
93.9
107
100.2
9
87.5
96
90.7
NMeFOSA
9
73.9
91.4
82.1
8
82.1
102
92.7
9
72.4
118
91.7
9
81.5
103
92.0
9
87.9
103
95.7
NEtFOSA
9
75.9
93.6
84.7
8
83.2
96.3
89.4
9
77
104
89.9
9
74.8
104
90.4
9
85.7
102
92.5
NMeFOSAA
9
91.7
117
102.8
8
95.8
134
108.9
9
90.5
151
119.3
9
89.8
128
107.5
9
87.2
116
98.8
NEtFOSAA
9
80.9
126
96.1
8
89.4
153
109.8
9
95.2
135
110.0
9
92.5
146
114.8
9
95.1
150
112.2
NMeFOSE
9
68.5
92.5
83.5
8
75.8
89.5
84.8
9
71.5
87.5
79.2
9
84
93.5
89.4
9
76.5
109.5
97.6
NEtFOSE
9
66
93
81.2
8
74.2
90.2
84.9
9
65.5
93.2
81.7
9
78.2
92
86.1
9
88.5
114
102.2
PFMPA
9
31.2
95
72.7
9
19.9
65.5
39.8
9
80.5
91
87.4
9
13.2
74
46.9
9
74
115.5
95.3
PFMBA
9
90.5
112
100.1
9
93.5
122
107.3
9
81
96.5
89.8
9
95.5
130.5
104.9
9
113.5
142.5
125.6
NFDHA
9
90
98
92.7
9
87
103
95.9
9
68.5
99
84.2
9
85
121
105.6
9
85.5
126.5
97.7
HFPO-DA
9
87.9
101.2
95.9
9
89.6
117.5
105.5
9
83.3
105.4
99.2
9
82.5
105.4
94.5
9
87.1
112.5
106.2
ADONA
9
84.6
99.6
93.0
9
29.4
123.8
100.3
9
82.9
101.2
95.5
9
87.1
102.5
93.4
9
101.7
121.2
112.2
PFEESA
9
84
94.5
87.9
9
47.8
106.5
93.5
9
85.5
103
95.5
9
94.5
106
101.4
9
78.5
109
85.4
9C1-PF30NS
9
87.5
101.2
95.9
8
70
117.5
93.9
9
85
97.9
92.1
9
85
103.3
93.4
9
102.1
118.3
111.9
llCl-PF30UdS
9
67.1
87.9
78.1
8
49.2
90.4
70.0
9
52.5
87.9
67.5
9
73.3
92.9
82.2
9
97.5
114.6
107.1
3:3FTCA
9
23.4
86.8
63.3
9
40.2
79.5
53.9
9
77.5
103.2
92.8
9
52.2
96.2
81.5
9
51.7
88.2
72.9
5:3FTCA
9
70.5
92
83.7
9
73
118
101.5
9
81
96
89.9
9
80.5
103.5
93.7
9
84.5
118.5
93.3
7:3FTCA
9
62
103.5
83.5
9
6.8
115.5
90.4
9
79.5
112.5
98.8
9
65
101.5
87.4
9
80
131.5
95.4
-------
Table F-4. Summary of surface water spike percent recoveries in high spike samples for each laboratory.
Analyte
Lab 6 spike % recover
y
Lab 7 spike % recover
y
Lab 9 spike % recover
y
Lab 10 spike % recovery
All Labs
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
6
95.8
99.8
97.5
9
95
116
99.5
6
94
98
96.4
9
107.4
119.8
112.1
65
81
119.8
98.2
PFPeA
9
80
103.5
87.2
9
99.5
105.5
102.3
9
93.6
100
97.2
9
95.5
129
109.0
81
80
129
97.3
PFHxA
9
84.3
100
94.2
9
93.7
99.7
96.5
9
94
101.5
97.1
9
87.6
128
104.4
81
75.2
128
96.0
PFHpA
9
82.5
90
85.9
9
92
99
94.1
9
92.9
98.6
95.1
9
92.9
114
105.7
81
82.5
116
97.5
PFOA
9
79.8
103.7
92.7
9
93.3
105
100.3
9
90.1
95
92.4
9
100.7
118.9
107.6
80
79.8
126.8
101.5
PFNA
9
85.9
103
97.2
9
93.2
113
101.1
9
92.8
99.5
97.1
9
89
121
105.5
80
79.1
121
98.1
PFDA
9
86.7
112
96.9
9
98
144
112.5
9
96.4
102
98.6
9
106
124
113.7
80
74.7
144
100.7
PFUnA
9
88.3
110
99.1
9
75.9
141
102.8
9
88.3
97.6
93.0
9
95.1
127
111.2
80
75.9
141
96.0
PFDoA
9
67.4
102
84.5
9
46.6
125
83.7
9
76.9
94.7
87.8
9
82.4
115
102.3
80
46.6
125
88.7
PFTrDA
9
86
109
94.3
9
46.1
102
70.6
9
67.7
87.4
80.3
9
83.6
117
101.3
80
46.1
117
85.3
PFTeDA
9
68.8
113
91.8
9
70.3
113
92.1
9
74.7
92.6
85.3
9
71.5
121
95.0
80
68.8
121
90.1
PFBS
9
89.6
113
99.4
9
88.9
104.2
96.9
9
94.7
100.1
98.0
9
83.6
125.8
108.3
81
78.8
125.8
95.7
PFPeS
9
82.5
115
105.0
9
89.5
114
98.6
9
95.2
105
99.2
9
98.7
116
107.4
80
82.5
116
98.4
PFHxS
9
80
103
91.4
9
83.3
107.2
95.9
9
89.8
97.1
93.0
9
78.5
107
97.4
80
78.5
107.2
94.9
PFHpS
9
78.4
109
98.2
9
101
167
129.7
9
95.6
109
101.7
9
95
122
105.1
80
78.4
167
105.1
PFOS
9
80.3
112
97.8
9
96.8
146
114.8
9
90.9
98.5
94.9
9
96.9
114
105.1
80
80.3
146
101.3
PFNS
9
92.2
117
103.5
9
69.2
109
83.7
9
81.7
92.3
86.8
9
91.9
106
97.2
80
69.2
117
90.8
PFDS
9
77.3
104
91.5
9
39.6
63.5
52.3
9
66.2
85.4
76.0
9
78.9
93.4
84.7
80
39.6
104
79.3
PFDoS
9
65
86.7
76.1
9
32.4
56.7
42.4
9
46.1
66.4
58.2
9
60.6
86
72.8
80
32.4
98.6
65.7
4:2FTS
9
72.5
114.2
88.0
9
79.2
101.2
91.9
9
94.2
103.8
98.7
9
92.9
161.2
121.0
81
72.5
161.2
95.9
6:2FTS
9
71.3
168.4
109.0
9
87.1
103.4
98.3
9
100.9
104.2
102.4
9
78.8
135.9
110.5
80
71.3
168.4
105.1
8:2FTS
9
67.9
107.9
90.5
9
95.8
132.9
115.4
9
104.2
108.7
106.7
9
98.8
119.2
107.5
80
67.9
135
105.6
PFOSA
9
83.1
107
92.9
9
92.4
120
103.3
9
95.4
105.9
99.4
9
103
114
109.0
80
83.1
150
101.1
NMeFOSA
9
86
101
94.4
9
77.1
120
100.9
9
90.3
101
95.5
9
96.8
114
104.3
80
72.4
120
94.4
NEtFOSA
9
77.1
94.5
87.4
9
58.6
126
89.8
9
87.8
103
95.0
9
91.4
113
101.0
80
58.6
126
91.1
NMeFOSAA
9
91.1
144
113.2
9
85.1
149
117.4
9
96.1
127
108.8
9
104
272
175.8
80
85.1
272
117.0
NEtFOSAA
9
93.2
161
114.8
9
81.4
177
125.7
9
90.3
139
111.3
9
94
317
184.4
80
80.9
317
120.0
NMeFOSE
9
76.8
102.8
87.5
9
53.8
110.5
76.8
9
67
88
79.4
9
58
97
80.8
80
53.8
110.5
84.3
NEtFOSE
9
68.8
98.5
83.2
9
40.5
86.5
61.6
9
60.8
90.5
81.2
9
47.5
99
79.4
80
40.5
114
82.4
PFMPA
9
15.7
78.5
47.5
9
78
92
84.9
9
12
75
50.1
9
71
105
90.3
81
12
115.5
68.3
PFMBA
9
82.5
117
93.7
9
97.5
103
100.4
9
92.5
131
102.3
9
91
114.5
103.8
81
81
142.5
103.1
NFDHA
9
66.5
123.5
90.5
9
90
98.5
94.5
9
84.5
91.5
87.8
9
77
113
97.3
81
66.5
126.5
94.0
HFPO-DA
9
89.2
113.8
100.3
9
89.6
95
92.5
9
94.2
99.6
96.9
9
103.3
129.6
117.3
81
82.5
129.6
100.9
ADONA
9
62.1
87.1
75.7
9
95
110
103.7
9
102.5
105.8
104.4
9
101.7
141.2
116.5
81
29.4
141.2
99.4
PFEESA
9
76.5
94.5
85.4
9
91
97.5
94.6
9
90.5
100
94.9
9
90.5
116.5
104.2
81
47.8
116.5
93.7
9C1-PF30NS
9
67.5
91.2
75.5
9
65.8
98.8
80.6
9
77.9
92.5
86.7
9
108.3
130.8
117.9
80
65.8
130.8
94.2
1 lCl-PF30UdS
9
57.5
72.1
65.8
9
22.4
55
35.1
9
57.1
77.1
66.9
9
78.8
102.1
89.4
80
22.4
114.6
73.6
3:3FTCA
9
66.8
91
81.1
9
66.8
83.8
74.4
9
58.8
97.5
82.9
9
71.8
112.8
94.2
81
23.4
112.8
77.5
5:3FTCA
9
66.5
84
75.8
9
77.5
97.5
90.2
9
81.5
95
89.2
9
69.5
122.5
100.6
81
66.5
122.5
90.9
7:3FTCA
9
44
85.5
69.4
9
65.5
100
87.4
9
65.5
92.5
82.4
9
44.4
132.5
86.1
81
6.8
132.5
86.7
-------
Table F-5. Summary of surface water EIS percent recovery for each laboratory.
Analyte
Lab 1 % recovery
Lab 2 % recovery
Lab 3 % recovery
Lab 4 % recovery
Lab 5 % recovery
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
13c4-pfba
21
6.95
85
43
21
6.16
24.9
12.9
21
85
113
102
21
1.7
23.6
12.8
21
20.1
68.6
40.4
13C5-PFPeA
21
64
98.7
85.9
21
60.9
106
84.5
21
83
132
99.2
21
56
101
73.9
21
40.8
91.2
70.9
13C5-PFHxA
21
83.2
99.3
88.5
21
39.5
96.2
86.5
21
88
112
100.2
21
63.9
100
75.2
21
45.2
90.4
73.3
13C4-PFHpA
21
83.2
101
88.8
21
12.3
94
79.6
21
87
112
95.4
21
59.6
101
72
21
44
90
72
13C8-PFOA
21
75.4
94.5
87.2
21
2.37
93
74.2
21
86
124
99.6
21
66.6
103
76
21
49.2
99.6
83.1
13c9-pfna
21
73.8
101
85.8
21
0.35
99.8
78.1
21
78
118
97.3
21
65.8
95.1
74.4
21
35.4
95.2
76.9
13c6-pfda
21
70.4
91.9
80.5
21
0.35
100
71.9
21
65
103
85.3
21
61.5
88.3
70.1
21
39.4
94.4
78.5
13C7-PFUnA
21
65.6
90.8
79.3
21
0.01
91.7
63.1
21
50
97
78.5
21
59.1
87.2
69
21
35.4
90.4
76.8
13C2-PFDoA
21
57.2
82.9
70.2
21
0.02
87.2
56.9
21
44
91
72.4
21
54.5
82.4
63.9
21
32.7
87.2
73.3
13C2-PFTeDA
21
50
81.4
62
21
0.02
68.9
47
21
27
78
61.1
21
53
78.3
62.4
21
23.3
72.6
58.3
13c3-pfbs
21
78.3
105
90.6
21
17.7
97.2
83.7
21
94
115
104.9
21
65.8
99.9
76.6
21
39
79.4
66.5
13C3-PFHxS
21
79.6
96.4
87.6
21
0.75
95.2
78.1
21
83
117
100.6
21
63
101
74.6
21
39.7
82.7
74.6
13c8-pfos
21
75.1
92.8
83.3
21
0.04
95.7
68.4
21
61
105
86.3
21
58.2
104
72.5
21
37.8
88.8
79.1
13C2-4:2FTS
21
86.9
120
102.2
21
48.4
187
133.7
21
104
165
131.1
21
59.7
112
76.2
21
45.4
168
122.1
13C2-6:2FTS
21
79.7
93.5
87.4
21
2.61
116
90.1
21
90
114
100.5
21
65.6
105
76.3
21
37.4
157
107.8
13C2-8:2FTS
21
73.2
98.2
86.5
21
0.11
178
96.8
21
70
127
94.5
21
54.7
103
72.8
21
33.3
149
106.9
13c8-pfosa
21
73.8
91.1
81.9
21
0.35
111
74.6
21
59
100
78.6
21
44.9
87.5
63.5
21
36
80
63
Dj-NMeFOSA
21
59.2
77.9
69.2
21
0.11
85.6
60.1
21
54
82
69.4
21
24.1
59.8
40
21
26.3
66.4
48.8
D5-NEtFOSA
21
52
73.5
63.9
21
0.03
74
52
21
48
85
67.5
21
20.5
59.4
37.3
21
23
64.4
45.6
Dj-NMeFOSAA
21
69.3
87.8
78.1
21
0.01
125
77.2
21
57
97
82.8
21
55.1
94.1
67.7
21
35.8
89.8
76.3
D5-NEtFOSAA
21
65.5
84.4
77.2
21
0.04
108
68.4
21
44
94
74.6
21
49.4
96.1
64.2
21
33.6
85.8
74.1
DrNMeFOSE
21
57.2
81.3
67.2
21
0.01
69
46.7
21
50
87
70.4
21
34.5
81.1
50.3
21
26.4
68.8
52.9
D9-NEtFOSE
21
56.4
76.3
64.6
21
0.01
67.2
43.6
21
48
92
69.1
21
31.9
95.8
51
21
17.8
60.8
44.2
13C3-HFPO-DA
21
84
103
90.8
21
42.6
97.7
84.4
21
85
127
99.7
21
65.9
109
77.8
21
39.3
80.7
67
-------
Table F-5. Summary of surface water EIS percent recovery for each laboratory.
Analyte
Lab 6 % recovery
Lab 7 % recovery
Lab 9 % recovery
Lab 10 % recovery
All Labs
n
Mill
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
13c4-pfba
21
2.49
28.6
13.1
21
46
88
60.2
14
14
27
21.2
21
31.7
76.1
54.4
182
1.7
113
40.7
13C5-PFPeA
21
51.2
91
74.2
21
79
100
90.3
21
19
79
65.3
21
74.8
114
89.6
189
19
132
81.5
13C5-PFHxA
21
68.5
104
80.4
21
90
106
97.3
21
58
81
74.7
21
79.3
99.2
87.5
189
39.5
112
84.8
13C4-PFHpA
21
70.5
92.5
80
21
91
108
98.2
21
65
76
71.1
21
72.6
103
86.8
189
12.3
112
82.7
13C8-PFOA
21
56.5
106
80.9
21
77
105
92.2
21
73
85
78.8
21
66.1
97.1
80.4
189
2.37
124
83.6
13c9-pfna
21
63.9
86.4
75.4
21
62
97
83
21
70
80
74.3
21
64.8
97.9
83.4
189
0.35
118
80.9
13c6-pfda
21
61.6
88.3
76.7
21
40
92
68.5
21
64
79
71.4
21
51
91.3
82.2
189
0.35
103
76.1
13C7-PFUnA
21
61.6
97.9
76
21
29
76
51
21
57
73
67.8
21
38.1
90.7
77.2
189
0.01
97.9
71
13C2-PFDoA
21
58.2
91.2
71.5
21
24
57
41.8
21
53
70
63.5
21
19.1
85.9
71.7
189
0.02
91.2
65
13C2-PFTeDA
21
36.1
80.7
61.6
21
22
52
36.4
21
48
71
58.3
21
2.2
71.3
61.8
189
0.02
81.4
56.5
13c3-pfbs
21
70.4
108
90.6
21
84
107
97.9
21
56
81
76.1
21
68.9
103
85.6
189
17.7
115
85.8
13C3-PFHxS
21
61.6
102
79
21
74
109
93.5
21
69
79
74.8
21
69.6
98.9
86.4
189
0.75
117
83.3
13c8-pfos
21
62.5
96.9
76.8
21
33
94
68.2
21
67
80
72.9
21
30.6
94.7
84.4
189
0.04
105
76.9
13C2-4:2FTS
21
67.5
150
105.4
21
88
119
98.4
21
66
116
88.2
21
69.5
116
87.5
189
45.4
187
105
13C2-6:2FTS
21
46.3
99.7
74.9
21
87
115
100.3
21
67
85
76.4
21
63.7
122
88.8
189
2.61
157
89.2
13C2-8:2FTS
21
60.4
91.4
72
21
40
109
75.9
21
57
78
68.2
21
51.4
114
85
189
0.11
178
84.3
13c8-pfosa
21
64
91.5
78
21
47
88
74.9
21
22
74
63.8
21
60.3
99.5
83.5
189
0.35
111
73.6
Dj-NMeFOSA
21
50.5
83
66.5
21
27
64
50.1
21
35
69
56.5
21
37.4
82.6
68.2
189
0.11
85.6
58.8
D5-NEtFOSA
21
52.5
81.5
62.9
21
26
57
44.9
21
35
68
52
21
27
79.3
64.4
189
0.03
85
54.5
Dj-NMeFOSAA
21
63.2
91
75.9
21
42
79
64.8
21
57
70
63.8
21
40.1
85.8
76.2
189
0.01
125
73.6
D5-NEtFOSAA
21
62.2
92.2
75.2
21
32
69
55.2
21
55
69
62.9
21
29
82.6
70
189
0.04
108
69.1
DrNMeFOSE
21
0.339
86
56.6
21
20
48
33.2
21
33
64
47.6
21
8.33
77
63.2
189
0.01
87
54.2
D9-NEtFOSE
21
0.53
79
54.1
21
18
51
33.5
21
24
61
44.9
21
3.13
72.3
59.8
189
0.01
95.8
51.7
13C3-HFPO-DA
21
70.1
97.4
81.3
21
80
108
90.7
21
52
78
71.5
21
70.7
101
84.7
189
39.3
127
83.1
-------
PFAS Multi-Laboratory Validation Study Report
Aqueous Media: Wastewater, Surface Water, and Groundwater
SERDP
Appendix G
Groundwater Supporting
Tables
Date: July 25, 2023
-------
Appendix G: List of Tables
G1 Target analytes detected in unspiked wastewater samples by kaboratory
G2 Minimum and maxium target analytes concentrations in unspiked wastewater samples
G3 Summary of wastewater spike percent recoveries in low spike samples Gor each laboratory.
G4 Summary of wastewater spike percent recoveries in high spike samples Gor each laboratory
G5 Summary of wastewater EIS percent recovery Gor each laboratory.
-------
Table G-l. Target Analytes Detected in Unspiked Groundwater Samples by Laboratory (ng/L)
Analyte
Number of
Labs
Lab 1
Lab 2
Lab 3
Lab 4
Lab 5
Lab 6
Lab 7
Lab 10
Cone | Qual
Cone | Qual
Cone | Qual
Cone | Qual
Cone | Qual
Cone | Qual
Cone | Qual
Cone | Qual
Ml 1 Ml /. initlurM
PFBA
8
10.3
12.6
J
10
6.29
J
9.26
12.1
9.7
11.4
PFPeA
8
11.4
12.7
11.8
11.7
10.7
16.6
10
9.3
PFHxA
8
22.9
24.1
20
22
25
24
19.8
22.6
PFHpA
8
6.59
6.39
6.08
5.86
5.75
7.09
5.5
8.31
PFOA
8
5.55
5.09
4.72
5.6
6.36
5.64
4.2
6.79
PFNA
8
0.657
U
1.06
U
0.504
U
0.29
U
1.24
J
0.25
U
0.61
U
0.493
U
PFBS
8
41.9
48
39.3
47.9
36.6
43.1
45.6
58.7
PFPeS
8
33.4
35.2
30.1
34.1
27.1
36.3
32.2
47.1
PFHxS
8
139
139
123
138
98.9
126
126
131
PFHpS
8
2.96
3.06
U
4.32
2.97
3.31
5.44
4.7
3.17
PFOS
8
78.8
78.5
70.6
62.3
75.8
80
78.4
0.415
U
6:2FTS
8
1.07
U
7.92
u
2.16
U
1.6
U
53.3
1.48
u
3.5
U
2.36
u
NMeFOSA
8
0.453
u
0.822
J
0.696
u
1.21
u
0.341
U
0.199
u
0.64
u
0.35
u
Ml II Ml j". \niiili\ii'\i
PFBA
8
--
X
17
15.1
14.2
13.7
16.2
13.3
16.6
PFPeA
8
--
X
37.7
35.8
33.6
31.9
39.6
33.4
36.7
PFHxA
8
--
X
95.5
73.4
87.2
85.8
93.8
85.6
108
PFHpA
8
--
X
15.3
14.1
14.1
11.3
15.9
12.5
14
PFOA
8
--
X
83
75.8
76.2
78.3
90.1
76.3
96
PFNA
8
--
X
1.06
u
1.12
J
0.72
J
0.792
U
0.922
J
0.61
u
0.849
J
PFBS
8
--
X
37.4
31.3
36.6
27.6
29.5
34
34.5
PFPeS
8
--
X
33.5
30.6
29.6
26.4
32.7
31.4
35.3
PFHxS
8
--
X
369
322
324
244
316
341
308
PFHpS
8
--
X
5.65
6.4
4.29
4.22
8.77
6.9
4.48
PFOS
8
--
X
246
197
200
198
246
240
212
6:2FTS
8
--
X
13.8
J
10.9
13.4
37.3
9.94
11
12
owe cwm
PFPeA
8
0.552
u
1.39
JI
0.856
u
0.533
JI
0.772
u
0.563
u
0.94
u
0.549
u
PFHxA
8
1.22
J
--
X
0.88
JI
1
J
0.944
JI
0.412
u
0.63
J
0.298
u
PFOA
8
1.15
J
--
X
0.696
u
0.651
u
0.547
J
0.29
u
0.46
u
1.03
J
PFBS
8
1.57
J
--
X
1.92
1.53
J
1.36
J
2.04
1.5
J
2.46
PFPeS
8
0.361
J
--
X
0.56
J
0.422
J
0.729
u
0.542
J
1.1
u
0.72
JI
PFHxS
8
1.62
J
--
X
2.4
1.67
J
1.61
J
1.83
1.3
J
1.81
J
PFOS
8
0.441
u
--
X
0.728
u
1.7
u
0.631
J
0.548
J
0.54
u
0.415
u
6:2FTS
8
1.07
u
--
X
2.16
u
1.6
u
3.02
BJ+
1.48
u
3.5
u
2.36
u
PFOSA
8
0.346
u
--
X
0.432
u
1.58
JI
2.17
0.188
u
0.67
u
0.212
u
NEtFOSA
8
0.365
u
--
X
0.736
u
1.07
J
0.521
u
0.0998
u
0.62
u
0.273
u
NEtFOSAA
8
0.554
u
--
X
0.88
J
0.61
u
0.531
u
0.571
u
1.3
u
0.693
u
Compounds undetected in all samples included: PFDA, PFUnA, PFDoA, PFTrDA, PFTeDA, PFNS, PFDS, PFDoS, 4:2FTS, 8:2FTS, NMeFOSAA, NMeFOSE, NEtFOSE, PFMPA, PFMBA, NFDHA,
HFPO-DA, ADONA, PFEESA, 9CI-PF30NS, llCI-PF30UdS, 3:3FTCA, 5:3FTCA, 7:3FTCA.
-------
Table G-2. Minimum and Maximum Detected Values Reported by all Laboratories for
Unspiked Samples
Analyte
Number of
Labs
GWA1
GWB1
GWC1
Min
Max
Min
Max
Min
Max
PFBA
8
6.29 J
12.6 J
13.3
17
0.597 U
1.9 U
PFPeA
8
9.3
16.6
31.9
39.6
0.549 U
1.39 JI
PFHxA
8
19.8
25
73.4
108
0.298 U
1.22 J
PFHpA
8
5.5
8.31
11.3
15.9
0.173 U
0.76 U
PFOA
8
4.2
6.79
75.8
96
0.29 U
1.15 J
PFNA
8
0.25 U
1.24 J
0.61 U
1.12 J
0.25 U
0.792 U
PFBS
8
36.6
58.7
27.6
37.4
1.36 J
2.46
PFPeS
8
27.1
47.1
26.4
35.3
0.729 U
0.72 JI
PFHxS
8
98.9
139
244
369
1.3 J
2.4
PFHpS
8
3.06 U
5.44
4.22
8.77
0.204 U
0.633 U
PFOS
8
0.415 U
80
197
246
0.415 U
0.631 J
6:2FTS
8
1.07 U
53.3
9.94
37.3
1.07 U
3.02 BJ+
NMeFOSA
8
0.199 U
0.822 J
0.199 U
1.21 U
0.199 U
1.21 U
PFOSA
8
0.188 U
0.724 U
0.188 U
0.724 U
0.188 U
2.17
NEtFOSA
8
0.0998 U
1.11 U
0.0998 U
1.11 U
0.0998 U
1.07 J
NEtFOSAA
8
0.531 U
2.26 U
0.531 U
2.26 U
0.531 U
0.88 J
-------
Table G-3. Summary of groundwater spike percent recoveries in low spike samples for each laboratory.
Analyte
Lab 1 spike % recover
y
Lab 2 spike % recover
y
Lab 3 spike % recover
y
Lab 4 spike % recover
y
Lab 5 spike % recover
y
n
Mill
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
6
97.1
100.8
99.5
7
100.8
107.5
104.2
9
93.1
99
95.6
9
96.5
105.4
101.9
9
83.7
94.2
88.2
PFPeA
6
97.3
107
101.4
9
105.3
114.2
109
9
79.5
102.7
95.1
9
95.2
114.5
104
9
86.5
112.8
97.6
PFHxA
3
90.9
101.4
97.7
3
106
116.5
111
6
70
98
86.8
3
91.5
109
100.2
3
82.8
98.8
92.1
PFHpA
6
83
104.5
92
9
101
114
104.6
9
86
97
92.4
9
79.5
104.5
91.4
9
68.2
105.7
90.2
PFOA
6
89.8
97.8
93.7
3
102
111
105.3
6
90.5
109.9
99.4
6
90
100
95.5
6
83.7
124.2
99.2
PFNA
6
87.5
98
94.5
7
99.5
111.5
105.6
9
83.9
109.5
92.2
9
93.5
107.9
99.4
9
74.8
95
86.7
PFDA
6
90.5
108.5
99.4
7
97
111.5
102
9
95.5
115.5
104.2
9
93.5
113
101.2
9
71
107.5
86.6
PFUnA
6
89
99
95.1
7
96.5
103.5
99.9
9
90.5
113.5
101.4
9
95.5
108.5
102.1
9
74
103.5
87.1
PFDoA
6
76
96.5
87
7
99.5
109.5
102.8
9
76.5
103.5
90.8
9
96.5
110
100.9
9
84
100.5
92.6
PFTrDA
6
90.5
111.5
98.1
7
48.4
97.5
83.1
9
70.5
101
85.3
9
90.5
102
94.8
9
78
99.5
88.6
PFTeDA
6
89
107
96.5
6
90.5
94.5
93.1
9
72
113
84.1
9
87.5
100
93.9
9
85
97
90.8
PFBS
3
94.7
99.7
97.9
3
104.5
122
113.8
3
85.4
95.4
88.9
3
99.8
112.4
105.9
3
77.7
86.7
82.7
PFPeS
3
90.8
100.7
94.9
2
103
111.4
107.2
3
89.8
99.7
96.2
3
96.9
107.3
101
3
83.2
90.1
86.6
PFHxS
3
88.5
96.4
93.8
2
106
107.5
106.8
3
86.6
97.5
92.2
3
100.6
116.6
107.3
3
74.6
89
79.7
PFHpS
6
92.5
104.2
96.9
7
99
146.5
123.7
9
101.4
117
108.8
9
85.2
110.5
97.6
9
83.5
119
95.6
PFOS
3
91
100.5
95.2
0
--
--
--
3
99
113
107.7
3
92.5
96
94
3
89.3
123.3
101
PFNS
6
80.7
93.1
86
5
51.5
104
87.4
9
89.6
97
93.2
9
82.7
98
89.5
9
73.3
100
82.9
PFDS
6
71.2
87.4
78.4
5
25.9
91.4
69.5
9
73.7
85.9
79.7
9
75.3
91.4
83.2
9
73.7
111.6
89.7
PFDoS
6
65.8
83.9
76.1
6
44.3
81.9
67
9
51.3
79.4
63.6
9
71.4
92
80.6
9
46
80.9
63.1
4:2FTS
6
84.1
100.5
93.3
9
92.8
106.5
99.9
9
88
99.2
94.5
9
91.7
104.6
98.2
9
92
104
96.7
6:2FTS
6
90.4
100.9
94.7
8
101.9
120.3
111
9
91.5
101.5
94.9
9
89.6
119.3
102.5
9
30
99.6
71.6
8:2FTS
6
98.9
104.6
102.2
5
97.2
117.6
108.7
9
95.2
135.5
111.8
9
97.4
111.2
105.4
9
102.3
115.9
107
PFOSA
6
97
103.5
99.9
5
104.5
113
107
9
95
131
105.3
9
98
115.1
104.4
9
79.6
98
87.8
NMeFOSA
6
87.5
104.5
95.2
5
85.4
97
91.8
9
82.5
98
88.2
9
87
101
96.1
9
91.5
103
97.9
NEtFOSA
6
88
92.5
89.8
5
87.5
104.5
95.7
9
81
94
87.3
9
79.1
98.5
88.6
9
90
101
95.2
NMeFOSAA
6
102
129
112.3
7
94
147
113.9
9
94
215
141.9
9
91
171.5
135
9
82.5
129.5
107.3
NEtFOSAA
6
79.5
160.5
124.3
5
96.5
111.5
105.5
9
89.5
210.1
135.2
9
86.5
210.5
146.3
9
89
180
126.5
NMeFOSE
6
87.5
103.1
94.7
4
92.5
97.5
94.9
9
76.2
88.8
81
9
84.4
98.1
90.6
9
86.9
110.6
98.4
NEtFOSE
6
83.8
89.4
87.1
4
89.4
100
94.4
9
71.2
86.2
76.9
9
78.8
88.1
83.8
9
73.1
116.9
94.3
PFMPA
6
96
105.2
101.2
9
34.8
108.5
67.3
9
85.5
95
89.9
9
78.5
106.5
94.1
9
95.5
130
111.8
PFMBA
6
100.7
106
104.5
9
101.2
122.2
113.1
9
82
98.2
90.1
9
97.2
105.2
101.6
9
106.5
138.8
119.9
NFDHA
6
94.5
109
102.8
9
81.8
110.2
97.7
9
75.5
118.2
100.5
9
92.2
117.5
106
9
99.5
128.2
109
HFPO-DA
6
95.9
102.8
98.9
9
112.4
135
119.9
9
88.9
102.6
95.6
9
82.6
109.4
92.6
9
87.4
112.4
104.7
ADONA
6
90.6
97.9
92.8
9
56.9
132.2
102.4
9
84.4
91.5
88.2
9
83.3
112.3
98.2
9
90.8
114.1
103.6
PFEESA
6
112
121.2
114.7
9
45.6
110.7
90.1
9
86.8
110.5
98.6
9
92.8
114.2
104.3
9
80.8
95.3
87.9
9C1-PF30NS
6
95.9
112.7
103.7
7
49.4
129.5
99.2
9
83.8
102.1
92.8
9
83.9
105.4
97.8
9
94.5
117.8
105.9
llCl-PF30UdS
6
70.8
92.5
81.6
7
9.5
95.3
68
9
59.7
79.4
68.7
9
71.1
93
84.6
9
91.3
118.8
105.3
3:3FTCA
6
74.9
79.3
77.1
9
46.8
97.9
73.2
9
84.2
95.2
89.6
9
92
102.9
98.9
9
73.6
85.5
81.7
5:3FTCA
6
80.2
85.8
82.7
9
78.7
104.2
93.7
9
86.7
95
89.8
9
90
107.5
101.1
9
84.2
99.2
92.8
7:3FTCA
6
81.8
91.7
85.9
8
21.1
101.7
85.4
9
79.7
90.8
83
9
85
100.8
94.7
9
72.3
100.8
83.8
-------
Table G-3. Summary of groundwater spike percent recoveries in low spike samples for each laboratory.
Analyte
Lab 6 spike % recover
y
Lab 7 spike % recover
y
Lab 10 spike % recovery
All Labs
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
9
99.2
105.5
102.9
9
89.5
93
91.5
9
101.7
123.2
112.1
67
83.7
123.2
99.3
PFPeA
9
74.8
122.2
99.6
9
93.5
101.3
97.3
9
106.8
141.2
118.2
69
74.8
141.2
102.9
PFHxA
3
90.5
106.5
100.5
6
89.9
103
96.5
3
90.5
116
105.8
30
70
116.5
97.4
PFHpA
9
91.1
139
110.1
9
88.5
102.5
94
9
90
160.5
128.6
69
68.2
160.5
100.8
PFOA
6
99.5
118.8
108.2
6
91
119
100.3
6
102.8
144
121.2
45
83.7
144
102.7
PFNA
9
85.9
122.4
106.7
9
89.5
132
102.1
9
92.8
124
108.7
67
74.8
132
99.5
PFDA
9
91
113.5
104.3
9
88
166.5
113.9
9
98
119.5
106.8
67
71
166.5
102.4
PFUnA
9
89
121
99.4
9
82
143
109
9
93.5
126.5
115
67
74
143
101.4
PFDoA
9
81
113.5
103.5
9
54
102
87.3
9
85.5
120.5
106.8
67
54
120.5
96.7
PFTrDA
9
76
118
98.8
9
44
90.5
74.4
9
94
114
104.9
67
44
118
90.9
PFTeDA
9
73.5
115.5
95.6
9
39.5
114.5
70.6
9
91.5
111
103.6
66
39.5
115.5
90.7
PFBS
3
92.3
96.8
95
3
84.5
97
92
3
110.2
124.7
119
24
77.7
124.7
99.4
PFPeS
3
93.4
117.1
106.1
3
89.1
118.8
100
3
108.8
132.6
120.5
23
83.2
132.6
101.3
PFHxS
3
88.9
107.8
98.4
3
79.6
111.9
93.4
3
97.5
107.4
101.8
23
74.6
116.6
96.2
PFHpS
9
88.1
126.3
112.1
9
96
226.5
156.3
9
103.5
121.6
110.3
67
83.5
226.5
113
PFOS
3
92.8
95.8
94.6
3
94
189.5
127.5
6
94.5
575
318.9
24
89.3
575
157.2
PFNS
9
88.6
120.3
105
9
77.2
139.6
97.1
9
86.6
125.2
100.3
65
51.5
139.6
93.3
PFDS
9
73.7
114.6
98.3
9
48
100.5
69.7
9
81.8
110.6
97.3
65
25.9
114.6
84.3
PFDoS
9
76.4
103.5
91.1
9
23.1
90.5
55.6
9
84.4
107.5
95.4
66
23.1
107.5
74.3
4:2FTS
9
71.3
117.6
94
9
82.7
99
91.1
9
92.7
129.2
113
69
71.3
129.2
97.8
6:2FTS
9
88.9
137.6
114.6
9
86.6
111.9
95.3
9
115
178.8
133
68
30
178.8
102.4
8:2FTS
9
87
140.5
106
9
103.4
154.3
119.4
9
84.7
134.3
109.7
65
84.7
154.3
109.1
PFOSA
9
99
116
103.7
9
90
155.5
112.4
9
101
148.5
123.8
65
79.6
155.5
105.7
NMeFOSA
9
83.5
98
91.6
9
61
115
94.8
9
76
116
96.6
65
61
116
94.1
NEtFOSA
9
90
98.5
94.2
9
47
95
79.6
9
74
102
90.7
65
47
104.5
89.8
NMeFOSAA
9
96.5
149.5
124.9
9
102
237.5
140
9
102.5
570
328.3
67
82.5
570
153.3
NEtFOSAA
9
92
190
137.7
9
79
230
139.1
9
115.5
655
309.1
65
79
655
157.2
NMeFOSE
9
88.1
101.9
95.7
9
54.4
87.5
76.5
9
50.9
101.9
78.5
64
50.9
110.6
88
NEtFOSE
9
83.8
108.1
98.1
9
43.5
78.1
64.6
9
49
102.5
80.5
64
43.5
116.9
84.1
PFMPA
9
73.2
125.7
100.2
9
88.2
93.2
91.5
9
93.5
113.2
102.1
69
34.8
130
94.5
PFMBA
9
81.8
117.8
104.3
9
89.2
94.8
92.5
9
89
121.8
103.9
69
81.8
138.8
103.7
NFDHA
9
57.8
119
90.6
9
83.5
96.2
88.4
9
95.5
121.8
107.7
69
57.8
128.2
100.2
HFPO-DA
9
93.4
147.5
110.1
9
88.2
94.8
91.4
9
104.4
132.5
118.1
69
82.6
147.5
104.1
ADONA
9
65.7
118
97
9
100.6
107.1
102.8
9
96.1
143.4
119.5
69
56.9
143.4
100.9
PFEESA
9
83.5
109.5
101
9
89.3
94
91.2
9
85.3
122.4
107.5
69
45.6
122.4
98.7
9C1-PF30NS
9
89.7
113.6
100.4
9
56.4
92.3
74.8
9
100.4
142
116
67
49.4
142
98.6
1 lCl-PF30UdS
9
82.9
117.3
99.4
9
26.6
59.2
39
9
91
130.9
108
67
9.5
130.9
82.3
3:3FTCA
9
91.2
120.8
102.7
9
90
101
94.5
9
81
104
91.2
69
46.8
120.8
89.1
5:3FTCA
9
88.3
105.8
96.7
9
83.3
95
89.8
9
80.6
124.2
101.9
69
78.7
124.2
94
7:3FTCA
9
83.3
98.3
91.9
9
72.6
90.8
84.7
9
60.4
122.5
93.2
68
21.1
122.5
87.9
-------
Table G-4. Summary of groundwater spike percent recoveries in high spike samples for each laboratory.
Analyte
Lab 1 spike % recover
y
Lab 2 spike % recover
y
Lab 3 spike % recover
y
Lab 4 spike % recover
y
Lab 5 spike % recover
y
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
6
93.8
102.7
98.1
6
99.8
107
104.6
9
92.7
100.2
95.6
9
102.4
109.2
106.5
9
83.6
93.4
89.4
PFPeA
6
92
100.3
97.1
9
106.8
111.2
108.6
9
88.1
107
98
9
92.2
96.7
94.7
9
90.2
106
96.5
PFHxA
6
88.5
96.9
93
9
98.9
110.5
105.6
9
81
97.3
89.8
9
90.8
105
98.3
9
53.2
101.1
84.6
PFHpA
6
88
96.8
93
9
99.4
106.7
102.4
9
88.5
98.5
92.3
9
95.9
103
100.1
9
86.8
101
92.4
PFOA
6
87
94.4
90.9
6
93
117
102.8
9
76.2
107.2
91.2
9
89.8
102
96.1
9
95.4
144.7
120.8
PFNA
6
85.6
98.9
92
8
102
119
108.3
9
79.1
114
90.4
9
89.9
103
96
9
72.8
93
84.4
PFDA
6
80.8
105
91.4
8
105
112
108.5
9
86.8
137
104.4
9
93.1
107
98.5
9
64.7
109
87.5
PFUnA
6
83.2
98.7
87.5
8
103
120
108.1
9
91.8
123
100.6
9
84
99.8
93.1
9
74.1
109
89
PFDoA
6
78.1
91.9
85.5
8
97.8
109
103.2
9
78.4
102
89.7
9
92
105
97.1
9
78.7
103
88.5
PFTrDA
6
86
96.3
92.1
8
80.7
95.3
87.6
9
67.8
97.5
86.8
9
84.7
98
91.6
9
78.8
101
87.6
PFTeDA
6
82.9
105
94.9
8
91.9
97.3
94.9
9
68.6
113
86.9
9
89.6
94.6
92.2
9
79.6
99.5
91.1
PFBS
6
84.8
107.1
94.2
9
100
113.6
107.9
9
75.7
97.7
89
9
90.1
114.1
100
9
76.4
91.4
83
PFPeS
6
82.6
106.6
94.6
8
106
126.5
113.1
9
89.9
102.4
96.1
9
92.9
106.9
99.5
9
81.4
105.6
92.4
PFHxS
3
83.1
97.3
90.2
3
102
104
103.3
3
92.7
104.6
98
3
94.9
100.3
97.3
6
81
123.1
96.9
PFHpS
6
92.5
102
98.8
8
107
133.4
117.5
9
91
131
105.8
9
96.7
108
102
9
87
100.8
93
PFOS
6
95.3
111.2
104.2
5
30.5
106
75.6
6
85.4
112
96.6
6
89.7
116.7
100.9
6
78.2
106.2
91.9
PFNS
6
82.7
94.1
89.2
8
86.6
109
96.4
9
87.2
101
94.2
9
89.2
97.8
93.3
9
78.6
89.9
83.1
PFDS
6
75.1
90.1
83
8
74.6
92.6
83.3
9
75.4
88.1
81.9
9
81.2
92.4
87.9
9
80.9
97.8
90.4
PFDoS
6
68.2
81.5
74.8
8
61.6
77.8
72
9
57
82.4
70.2
9
77.1
88.6
83.6
9
54.5
69.9
63.9
4:2FTS
6
86.7
106.7
95.4
9
91.7
100.8
95.3
9
83.3
90.8
87.4
9
87.5
108.3
97
9
88.8
98.8
93.8
6:2FTS
6
88
99.2
95.2
9
89.2
121.3
111.7
9
85.1
102.5
92.5
9
99.6
116.3
107.5
9
73.2
105
91.2
8:2FTS
6
93.8
104.2
99.3
5
101.2
117.5
107.5
9
94.2
131.7
107.2
9
99.6
119.2
103.7
9
97.5
109.6
105.6
PFOSA
6
95.2
102
98.8
8
101
108
103.4
9
91.4
156
109.4
9
94
110.4
101.8
9
84.2
96
90.5
NMeFOSA
6
82.8
86.5
85.2
8
93.4
101
97.5
9
82
124
96.8
9
83.8
98.6
91.6
9
90.8
101
95
NEtFOSA
6
80.9
92.5
86.4
8
86.1
104
92.7
9
76.3
112
92.1
9
78.3
91.6
83.9
9
89.6
100
93.6
NMeFOSAA
6
88.6
108
97.5
8
95
115
105.6
9
94.9
154
113.7
9
92.3
106
100.3
9
82.9
102
93
NEtFOSAA
6
84.1
97.1
92.2
5
94.9
110
101.8
9
92
164.1
114.7
9
95.9
119
104.7
9
91.8
119
104.6
NMeFOSE
6
87.5
97.5
92.7
5
91.5
96.2
94.7
9
76.5
99.5
89.4
9
89.2
95.5
92.7
9
85.8
118.8
96.4
NEtFOSE
6
86.8
91.8
89.3
5
90.5
96.5
93.9
9
70.5
100.5
81.4
9
86.2
92.8
90.2
9
82.8
123.8
97.7
PFMPA
6
99
106
101.8
9
25.7
100.5
64.8
9
84.5
93
89.4
9
65
93.5
81.6
9
99.5
127
114.7
PFMBA
6
90.5
105.5
99.8
9
106.5
139
116.6
9
76.5
90
85.8
9
95.5
99.5
97.4
9
111.5
134.5
123.9
NFDHA
6
92.5
104.5
100.8
9
90
111
99
9
75.5
113
94.2
9
85.5
112
98
9
79
102
91.2
HFPO-DA
6
89.6
106.2
95.7
9
92.1
116.3
105.7
9
83.3
115
95.9
9
93.8
119.6
103.6
9
90.4
122.1
104.1
ADONA
6
84.6
95
89.3
9
52.5
113.3
98
9
81.7
100.4
88.8
9
92.5
106.7
97.3
9
90
130.4
111.3
PFEESA
6
82
99
90.2
9
61
106.5
96.6
9
85.5
113
93.1
9
98
105.5
102.6
9
71.5
93.5
84.9
9C1-PF30NS
6
91.3
104.6
97.8
8
91.7
107.9
99.6
9
80.4
97.1
87.6
9
93.3
110.4
98.9
9
95.8
130
111.1
llCl-PF30UdS
6
70.8
89.6
79.4
8
68.3
80.8
74.8
9
62.5
76.7
70.3
9
85
95.8
90.5
9
91.7
136.7
111.4
3:3FTCA
6
79
94.8
84.8
9
35
91.5
68.5
9
87.8
98.2
92.1
9
95
98.8
96.8
9
72.2
96.8
86.4
5:3FTCA
6
79.5
86
83.6
9
87.5
105.5
98.7
9
86.5
104
91.1
9
93
103.5
98.5
9
79
105
94.1
7:3FTCA
6
82.5
95.5
88.6
9
16.4
106
90.5
9
88.5
108
96.1
9
91.5
103
97.4
9
86
111
98.4
-------
Table G-4. Summary of groundwater spike percent recoveries in high spike samples for each laboratory.
Analyte
Lab 6 spike % recover
y
Lab 7 spike % recover
y
Lab 10 spike % recovery
All Labs
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
PFBA
9
96.4
103.2
99.4
9
94.6
99.7
97.1
9
98.5
118.3
108.7
66
83.6
118.3
99.8
PFPeA
9
91.2
115.5
98.8
9
97.5
104.8
101.9
9
89.2
122
107
69
88.1
122
100.5
PFHxA
9
64.2
128.2
91.3
9
94.2
112.4
100.9
6
92.4
123.4
106.7
66
53.2
128.2
95.9
PFHpA
9
86.7
113.9
100.2
9
92.3
101.5
96.8
9
94
155
116.2
69
86.7
155
99.4
PFOA
9
76.9
118
99.7
9
96.7
117.7
104.6
9
98
121
111.2
66
76.2
144.7
102.6
PFNA
9
84.4
114
98.3
9
90.1
122
107.2
9
89.2
118
104.7
68
72.8
122
97.8
PFDA
9
87.4
109
98.2
9
99.7
144
117.3
9
97.3
123
107.8
68
64.7
144
102.1
PFUnA
9
88.4
115
98.5
9
96.5
127
110.6
9
90
130
104.5
68
74.1
130
99.4
PFDoA
8
88.1
109
99.8
9
69
103
90.1
9
91.6
108
100.8
67
69
109
94.5
PFTrDA
8
80.3
168
106.5
9
62.7
86
77.7
7
86.5
115
100.8
65
62.7
168
90.8
PFTeDA
8
74.8
107
91.5
9
69
92.7
78
7
84.5
109
95.3
65
68.6
113
90.2
PFBS
9
72.9
96.9
83.5
9
96.3
103
98.9
9
84.3
120.5
103.3
69
72.9
120.5
95
PFPeS
9
67.7
99.3
87.3
9
94.6
118
108.9
9
95.9
131.9
114.6
68
67.7
131.9
100.9
PFHxS
3
78.3
88
84.6
3
99.7
105.7
102
3
92.4
103.2
97
27
78.3
123.1
96.2
PFHpS
9
94
171.2
108.7
9
100.3
185
144
9
103.8
242
136.7
68
87
242
113.9
PFOS
6
82
107.5
97.3
6
91.6
172.6
136.6
6
105
223
157.5
47
30.5
223
108.2
PFNS
9
38.6
105
87.7
9
82.1
131
94.2
9
30.9
111
87.6
68
30.9
131
90.7
PFDS
9
3.9
96.1
79.7
9
57.6
123
74.5
9
8.5
106
77.9
68
3.9
123
82.3
PFDoS
8
48.8
94
75.5
9
43.2
101
60.8
8
2.5
95.7
78.2
66
2.5
101
72.1
4:2FTS
9
87.1
115.8
98
9
82.9
99.2
90.5
9
79.2
123.3
95.8
69
79.2
123.3
94.1
6:2FTS
9
71.7
140.1
107.2
9
83.8
108
96.9
9
78.8
147.1
111.7
69
71.7
147.1
102
8:2FTS
9
86.7
129.6
101
9
108.3
162.9
124.6
9
81.7
148.3
114.1
65
81.7
162.9
108.3
PFOSA
9
85.2
105
94.7
9
92.4
138
114.7
9
98.7
119
106.4
68
84.2
156
102.6
NMeFOSA
9
80.6
95.3
86
9
86.2
103
96
9
82.9
108
98.6
68
80.6
124
93.6
NEtFOSA
8
88.4
94.8
91.7
9
61.2
87.1
78.9
9
77.5
93.7
89.5
67
61.2
112
88.6
NMeFOSAA
8
88.9
128
103.6
9
106
135
114.9
9
106
183
136.1
67
82.9
183
108.7
NEtFOSAA
8
106
132
115.4
9
100
134
110.4
9
89.6
192
127.9
64
84.1
192
110.1
NMeFOSE
6
88.8
97
92
9
60
80.8
75.8
9
66
99.8
87.1
62
60
118.8
89.6
NEtFOSE
6
86.8
99.2
92.6
9
51.5
71.5
64
8
64.5
94
84.5
61
51.5
123.8
85.8
PFMPA
9
55.5
114.5
85.8
9
93.5
101.5
98.8
9
85
111.5
97.1
69
25.7
127
91.3
PFMBA
9
99
124.5
106.1
9
94.5
101
98.8
9
93.5
117
100.5
69
76.5
139
103.8
NFDHA
9
69
111.5
89.6
9
87
95.5
91.6
9
93
115.5
104.4
69
69
115.5
95.9
HFPO-DA
9
74.2
111.2
97.4
9
88.8
99.2
94
9
100
131.2
116.2
69
74.2
131.2
101.8
ADONA
9
63.7
100.4
84
9
97.5
107.5
102.1
9
106.7
144.2
121.7
69
52.5
144.2
99.5
PFEESA
9
82
116.5
93
9
89
100
95.1
9
80
108.5
93.3
69
61
116.5
93.7
9C1-PF30NS
9
32.2
106.7
82.4
9
57.9
85.4
71.1
9
6.4
137.5
90.2
68
6.4
137.5
92
llCl-PF30UdS
9
0.5
85.4
70.3
9
34.1
47.9
40.2
8
1.2
125
93.4
67
0.5
136.7
78.6
3:3FTCA
9
93
131
105.9
9
97.2
104.5
101
9
85.5
106
94.3
69
35
131
91.5
5:3FTCA
9
76.5
108.5
87.9
9
98.5
103.5
101.2
9
90.5
121.5
102.6
69
76.5
121.5
95.2
7:3FTCA
9
74.5
90.5
84.3
9
82.5
103
94.9
9
78
124
96.1
69
16.4
124
93.5
-------
Table G-5. Summary of groundwater EIS percent recovery for each laboratory.
Analyte
Lab 1 % recovery
Lab 2 % recovery
Lab 3 % recovery
Lab 4 % recovery
Lab 5 % recovery
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
13C„-PFBA
21
57.2
95.7
86.1
21
4.73
62.4
24.4
21
93
108
99.3
21
18.8
79.3
40.1
21
58.3
79.5
71.6
13C5-PFPeA
21
78
97.8
88.8
21
34.1
92
79.5
21
86
116
99.2
21
71.7
84.6
78.1
21
62.4
88.2
72.7
13C5-PFHxA
21
80.1
102
88.9
21
4.55
95.1
82.5
21
85
111
97.8
21
64.7
80.7
74
21
66.8
83.6
75.7
13C„-PFHpA
21
75.3
97.1
84.3
21
0.832
94.9
77.5
21
86
107
95.2
21
65
83.4
71.9
21
63.2
92
75.1
13C8-PFOA
21
79.9
94.7
87.6
21
0.0857
95.9
73.7
21
91
112
100.7
21
69.1
88.4
75.7
21
66.8
97.6
81.3
13c9-pfna
21
73.9
99.5
87.3
21
0.157
97.2
72.5
21
78
110
96.2
21
66.8
81.9
73.8
21
60.2
88
76.6
13c6-pfda
21
78.7
102
90.3
20
0.133
94.8
73.6
21
62
116
86.3
21
57.2
79.5
70.5
21
72.7
99.2
84.4
13C7-PFUnA
21
72.9
101
84.2
20
0.0556
81.4
64.8
21
46
104
78.3
21
51.6
80.8
70
21
66.3
99.2
82.9
13C2-PFDoA
21
58.9
90
76.6
20
0.0292
75.6
56.4
21
51
88
70.7
21
52.3
74.1
64.2
21
59
94.4
75.9
13C2-PFT eDA
21
57.3
84.1
70.5
20
0.003
74.9
52.3
21
46
87
63.6
21
51.5
69.6
62.3
21
52
86.4
66.3
13C3-PFBS
21
78.5
89.2
84.2
21
1.47
96.9
79
21
94
112
103.3
21
63.9
87
76.1
21
59.2
79.4
69.5
13C3-PFHxS
21
81.1
91.5
85.5
24
0.0497
90.1
72.8
21
88
111
98.4
21
65.4
85.1
74.2
21
70
82.7
76.9
13Cs-PFOS
21
75.1
95.2
84
21
0.00469
90.1
65.7
21
74
101
89.9
21
63.8
87.4
73.9
21
74.2
86.7
80.2
13C2-4:2FTS
21
81
112
98.4
21
5.22
149
111
21
95
136
116
21
62.5
82.3
72.6
21
81.7
158
119.2
13C2-6:2FTS
21
79
111
96.9
21
0.112
97.8
74.7
21
88
110
99.2
21
64.1
84.3
74
21
69.3
143
108.2
13C2-8:2FTS
21
78.4
107
92.2
21
0.0158
242
116.3
21
73
97
88.1
21
54.9
88.3
72.5
21
69
146
106.5
13Cs-PFOSA
21
67.3
82.8
76.1
21
0.0465
110
71.3
21
56
93
82.5
21
56.2
70.5
63.3
21
57.2
83.6
67.3
D3-NMeFOSA
21
51
74.1
61
21
0.143
83.1
59.6
21
44
77
65.5
21
30.6
41.3
35.5
21
38.8
60.4
49.8
Dj-NEtFOSA
21
45.8
71.2
57.2
21
0.0502
73.6
50.7
21
44
80
65
21
28.6
39
33.1
21
35.4
58
47.2
Dj-NMeFOSAA
21
68.2
90.9
77.8
21
0.0681
101
65.3
21
59
97
79.4
21
59.9
74.8
68
21
72.2
88.2
79.6
Dj-NEtFOSAA
21
62.2
94.7
77
21
0.0885
82.8
60.4
21
52
83
70.5
21
55.8
75.4
64.6
21
67
86.6
78.4
D7-NMeFOSE
21
51.2
80
64.9
21
0.016
68.4
46.2
21
52
85
72.3
21
42.8
60.4
51.2
21
43.2
80.8
63.9
Dg-NEtFOSE
21
49.7
74.6
63.5
21
0.0149
75.8
47.2
21
56
87
73.6
21
38.1
71.6
50.9
21
35.6
67.6
53.6
13C3-HFPO-DA
21
84
106
94.1
21
5.91
96.9
77.9
21
91
119
98.6
21
67.6
90.7
77.9
21
55.8
84.8
69.8
-------
Table G-5. Summary of groundwater EIS percent recovery for each laboratory.
Analyte
Lab 6 % recover
y
Lab 7 % recover
y
Lab 10 % recovery
All Labs Combined
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
n
Min
Max
Avg
13c4-pfba
21
11
39
27.1
21
91
101
97.3
21
54.3
92.5
80.9
168
4.73
108
65.9
13C5-PFPeA
21
53
78
65.7
21
89
98
92.7
21
73.8
110
92.6
168
34.1
116
83.7
13C5-PFHxA
21
58
85
71.6
21
89
100
94.5
21
78.4
105
89.1
168
4.55
111
84.3
13C4-PFHpA
21
61
80
67.7
21
87
100
94
21
68.2
110
86.2
168
0.832
110
81.5
13C8-PFOA
21
56
83
68.7
21
67
102
87.5
21
75.1
98.5
84.4
168
0.0857
112
82.4
13c9-pfna
21
58
96
73.7
21
49
93
76.9
21
74.9
106
87.9
168
0.157
110
80.6
13c6-pfda
21
37
78
68.7
21
33
98
64.9
21
51.6
103
85.5
167
0.133
116
78.1
13C7-PFUnA
21
10
83
67.2
21
29
77
51.1
21
26.1
102
81.6
167
0.0556
104
72.6
13C2-PFDoA
21
1
74
65.5
21
33
59
44.4
21
10.3
94.9
78.4
167
0.0292
94.9
66.6
13C2-PFTeDA
21
0.3
81
58.8
21
29
62
48.5
21
0.138
95.9
75.3
167
0.003
95.9
62.3
13c3-pfbs
21
66
120
87.3
21
89
105
96.5
21
68.7
117
85.2
168
1.47
120
85.1
13C3-PFHxS
21
69
108
81.2
21
68
102
88.7
21
59.4
112
88.2
171
0.0497
112
83.1
13c8-pfos
21
37
80
70
21
32
96
61.8
21
14
98.3
85.3
168
0.00469
101
76.4
13C2-4:2FTS
21
69
116
82.4
21
85
112
97.5
21
71.3
113
91.3
168
5.22
158
98.6
13C2-6:2FTS
21
49
101
75.4
21
77
114
99.2
21
63.3
131
90.2
168
0.112
143
89.7
13C2-8:2FTS
21
36
114
84
21
40
98
70.7
21
50.5
134
92.4
168
0.0158
242
90.4
13c8-pfosa
21
51
85
72.8
21
48
101
74.5
21
49.8
104
87.4
168
0.0465
110
74.4
D3-NMeFOSA
21
11
70
57.1
21
32
66
43.2
21
28.6
90.7
70.5
168
0.143
90.7
55.3
D5-NEtFOSA
21
2
67
52.3
21
30
60
43.3
21
18
90.6
68.6
168
0.0502
90.6
52.2
D3-NMeFOSAA
21
9
77
64.2
21
33
82
57.5
21
30.6
103
84.5
168
0.0681
103
72
D5-NEtFOSAA
21
5
83
63
21
36
70
51.9
21
18.7
116
80.5
168
0.0885
116
68.3
D7-NMeFOSE
21
0.3
82
57
21
26
49
39.5
21
12.3
99
78.3
168
0.016
99
59.2
D9-NEtFOSE
21
0.4
80
53.8
21
26
51
40.3
21
4.71
98.9
75.4
168
0.0149
98.9
57.3
13C3-HFPO-DA
21
60
95
72.9
21
82
96
88.9
21
66.5
120
87.6
168
5.91
120
83.5
-------