A
v>EPA
EPA-910-R-17-005
August 2017
Water Sampling and
Testing for Formaldehyde at
Northwest F sh Hatcheries
Report Finalized August 2017
Prepared for the EPA Region 10 Office of Water and Watersheds
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WATER SAMPLING AND TESTING FOR FORMALDEHYDE
AT NORTHWEST FISH HATCHERIES
Report Finalized August 2017
Prepared for the EPA Region 10 Office of Water and Watersheds by:
Jed Januch, Environmental Protection Specialist
Environmental Services Unit
EPA Region 10 Office of Environmental Review and Assessment
Steve Reimer, Chemist
EPA Region 10 Laboratory
EPA Region 10 Office of Environmental Review and Assessment
Catherine Gockel. Environmental Protection Specialist
EPA Region 10 Office of Water and Watersheds
Siana Wong, Natural Resource Scientist
Washington State Department of Ecology, Toxics Studies Unit
Brandee Era-Miller, Environmental Specialist
Washington State Department of Ecology, Toxics Studies Unit
The authors wish to thank the EPA sampling team members Brent Richmond, Lillian Herger,
and Raymond Wu, and the Ecology sampling team members James Medlen and Debbie
Sergeant for their time and efforts. We also wish to thank QA team members Don Matheny
and Jennifer Crawford for assistance in developing the quality assurance project plan and
environmental data management support. Also, many thanks to Tim Siwiec for GIS support
and Kevin Brown for graphics support.
Cover Photo: Little White Salmon River, Washington
ii
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TABLE OF CONTENTS
EXECUTIVE SUMMARY 1
INTRODUCTION 2
BACKGROUND 2
NPDES Aquaculture Permits 2
Formalin 2
PROJECT DESCRIPTION 4
Selection of Sampling Sites 4
Table 1: Hatcheries Sampled for this Study 4
Figure 1: Locations of fish hatcheries participating in the EPA sampling events 5
EPA Sampling of Hatcheries 5
Ecology Sampling of WDFW Hatcheries 6
METHODS AND MATERIALS 6
1. Field Measurements 6
2. Water Sampling 6
3. Analytical Methods 7
4. Quality Assurance and Quality Control 7
RESULTS OF ANALYSIS 7
EPA Sampling 7
Table 2 8
Figure 2 9
Figure 3 10
Table 3 10
Additional Information Collected 10
Ecology Sampling 11
Table 4 12
Figure 4 12
Figure 5 13
Figure 6 13
Additional Information Collected 14
CONCLUSION 14
Technical Notes/Recommendations 15
Appendices 16
Appendix 1 17
Appendix 2 18
Appendix 3 23
Appendix 4 37
Appendix 5 65
Appendix 6 70
Appendix 7 99
Appendix 8 109
ill
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
EXECUTIVE SUMMARY
In 2016, the U.S. Environmental Protection Agency (EPA) Region 10's Office of
Environmental Review and Assessment (OERA) and the Washington State Department
of Ecology (Ecology) conducted water sampling and field analysis at 10 federal and state
fish hatcheries in Washington and in Idaho. The objective was to provide data on the
concentrations of formaldehyde being discharged from hatcheries after applications of
formalin, which is used by the hatcheries to control external parasites on hatchery fish and
their eggs.
Formalin is a generic term that describes a solution of 37% formaldehyde gas dissolved
in water. The Food and Drug Administration (FDA) requires a 10-fold dilution of finfish
treatment water and a 100-fold dilution of finfish egg treatment water, which should lead to
a discharge concentration of no more than 25 parts per million (ppm), equivalent to 25 (.iL/L
formalin, or 10 ppm formaldehyde (active ingredient). According to the FDA, additional
in stream dilution, infrequent use, and rapid degradation should render the discharged
formalin below a level that causes significant environmental effects on aquatic animals.1
In a recent risk assessment of hatcheries covered by the EPA National Pollutant Discharge
Elimination System (NPDES) General Permit for Federal Aquaculture Facilities and
Aquaculture Facilities in Indian Country within Washington State, EPA Region 10 concluded
that formalin use at hatcheries covered that NPDES General Permit is not likely to affect
salmonids listed under the Endangered Species Act (ESA) in concentrations below 10 ppm
formaldehyde in the receiving water.2 Therefore, the EPA has used 10 ppm formaldehyde as
the level of concern for this study, against which formaldehyde concentrations detected in
samples were compared.
The EPA and Ecology worked with staff and managers at U.S. Fish and Wildlife Service
and Washington State Department of Fish and Wildlife to identify which hatcheries in the
Northwest use the most formalin, and to ensure that sampling included a range of formalin
use scenarios (i.e., egg, juvenile, and adult treatments). By sampling formaldehyde in the
effluent at facilities that use the most formalin across Washington and Idaho, and by sampling
during peak formalin use, this study intended to capture a reasonable worst-case scenario for
estimating formaldehyde concentrations in Pacific Northwest hatchery effluent.
Sampling was performed in accordance with an approved quality assurance project plan
(QAPP) at a minimum of three locations per fish hatchery: 1) the influent raw water; 2)
the effluent water; and 3) the receiving water. Samples from facility outfalls where treated
effluent would be discharged were collected as both grab samples collected by hand and
discrete interval samples collected with an automated sampler. Grab samples were collected
after at a period when it was believed that the plume with the highest likely concentration
of formaldehyde was being discharged through the outfall. The analytical parameters for
influent raw water and effluent, are applicable field measurements (temperature, total
chlorine, ammonia, dissolved oxygen, conductivity, turbidity, pH, and formaldehyde
screening) and laboratory analysis for formaldehyde. The EPA Region 10 Laboratory
performed all of the analytical chemistry required for this study.
In all of the hatcheries sampled for this study, the maximum concentration of
formaldehyde measured did not exceed the FDA and EPA Region 10 level of concern of 10
ppm
1 http://water.epa.gov/scitech/wastetech/guide/aqu\aeulture/upload/2005 09 01 guide aquaculture EEBA
EEBA-Cfaapter-7.pdf accessed 12/5/2014
2 https://www3.epa.gov/regionl0/pdf/permits/npdes/wa/WA Hatchery (IP WAG130000 BE.pdf
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Based on data collected at the hatcheries that participated in this study, as well as the
available toxicological data for threatened and endangered salmonids and an EPA risk
assessment for formalin in Washington hatcheries, the EPA believes that current levels of
formalin use are generally protective of aquatic life and ESA listed salmonids in Pacific
Northwest waters.
INTRODUCTION
In 2016, the U.S. Environmental Protection Agency (EPA) Region 10's Office of
Environmental Review and Assessment (OERA) and the Washington State Department
of Ecology (Ecology) conducted water sampling and field analysis at 10 federal and state
fish hatcheries in Washington and in Idaho. The objective was to provide data on the
concentrations of formaldehyde being discharged from hatcheries after applications of
formalin used by the hatcheries to control disease among hatchery fish. The data resulting
from this study will be used by the EPA Region 10 Office of Water and Watersheds (OWW)
to inform the development of aquaculture permits issued under the National Pollution
Discharge and Elimination System (NPDES). This report details the sample collection
techniques used by EPA and summarizes the results of analysis for samples collected by EPA
and Ecology.
BACKGROUND
NPDES Aquaculture Permits
The EPA and Ecology issue permits under the National Pollutant Discharge Elimination
System (NPDES) to establish conditions for the discharge of pollutants in wastewaters
to waters of the United States. In order to ensure protection of water quality and human
health, the NPDES permits place limits on the types and amounts of pollutants that can
be discharged and places other conditions on such activity, such as monitoring and best
management practices.
At 40 CFR §122.24, the EPA defines concentrated aquatic animal production (GAAP)
facilities as point sources subject to the NPDES permit program. In Idaho, EPA Region 10
is the NPDES permitting authority for GAAP facilities.3 In Washington, EPA is the NPDES
permitting authority for federal aquaculture facilities (i.e.. National Fish Hatcheries), and
for aquaculture facilities in Indian Country within the State of Washington.4 Ecology is the
NPDES permitting authority for all other hatchery and aquaculture facilities."
Formalin
Formalin is a generic term that describes a solution of 37% formaldehyde gas dissolved in
water. The Parasite-S formulation is administered in a bath treatment to control external
protozoa (Chilodonella spp., Costia spp., Epistylis spp., Ichthyophthirius spp., Scyphidia
spp. and Trichodina spp ), and the monogenetic trematode parasites (Cleidodiscus spp..
Dactylogyrus spp., and Gyrodactylus spp.) on all finfish. It is also used for the control of
fungi of the family Saprolegniaceae on all finfish eggs (Western Chemical Label, no date).
3 https://yosemite.epa. gov/rlO/water.iisf/npdes+penmts/general+iipdes+permits# Aquaculture
4 https://yosemite.epa.gov/rlO/water.nsf/npdes+permits/general+npdes+permits#fedaqua
5 http://www.ecy.wa.gov/Programs/wq/permits/fin fish/index.html
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Formalin is administered to salmon and trout as a bath treatment for prolonged or short
periods of time. The standard dosage recommended in the INAD #9013 Protocol to prevent
or control fungus on fish and eggs is to administer formalin as a static-bath or flow-through
treatment at 15 - 2000 |iL/L (ppm) active drug. Eggs are treated daily or every other day until
hatch. Fish are treated every other day to weekly for 30 to 60 minutes, and then transferred
to clean water. The formalin concentration is water temperature dependent and 50°F is the
cutoff for the two treatment concentrations. Salmon and trout are treated up to 170 |iL/L at
water temperatures above 50°F and 250 |iL/L at temperatures below 50°F. All other finfish
are treated up to 250 |iL/L regardless of temperature. Treatment is not recommended to
exceed 1.0 hour.
In the finding of no significant impact for Parasite-S, the Food and Drug Administration
(FDA) requires a 10-fold dilution of finfish treatment water and a 100-fold dilution of finfish
egg treatment water, which should lead to a discharge concentration of no more than 25 ppm
(equivalent to 25 |iL/L or 10 ppm formaldehyde).' The FDA contended that additional in-
stream dilution, infrequent use, and rapid degradation would render the discharged formalin
below a level that causes significant environmental effects on aquatic animals (formaldehyde,
the active ingredient in formalin, is oxidized in the aquatic environment into formic acid
and ultimately into carbon dioxide and water; the estimated half-life of formaldehyde in
water is approximately 36 hours). Directions for dilution of treatment water and additional
environmental precautions are described on the labeling of the product. An example of the
Parasite-S labeling is displayed in Appendix 1.
As part of its Biological Evaluation for EPA's NPDES General Permit for federal aquaculture
facilities and aquaculture facilities in Indian Country within Washington State, and in
compliance with the Endangered Species Act (ESA)7, the EPA performed risk assessments
to determine whether formalin use at EPA-permitted aquaculture facilities in Washington
and Idaho have the potential to affect threatened or listed species or their critical habitat.
These risk assessments used the best available science and toxicological information. The
EPA's risk assessments likely resulted in unrealistically conservative assumptions, and did
not account for in-stream dilution. Based on the available toxicological data for threatened
and endangered salmonids, the EPA believes that the FDA's dilution requirement (10 ppm
formaldehyde) will be protective of aquatic life in Pacific Northwest waters. Therefore, the
EPA has used 10 ppm formaldehyde as the level of concern for this field study, against which
formaldehyde samples were compared.
There have been very few studies examining the amounts of formaldehyde discharged
from fish hatcheries after formalin treatments. Some of the hatcheries participating in this
study provided anecdotal information on unpublished or informal studies. One published
study which did focus on measuring the formaldehyde concentration in effluent outfalls at
freshwater aquaculture facilities in Nova Scotia was done by Environment Canada in 2011.
Formaldehyde was applied at an effective rate of 250 (.iL/L to a 10-meter diameter pond with
a water temperature of 50° Fahrenheit (F). Samples were collected at the effluent outfall and
at another location 100 meters downstream of the effluent outfall. Samples were collected
with the aid of automated I SCO® samplers set to obtain 100 milliliters (ml) of water every
5 minutes over a 3-hour period. The I SCO® samples were composited in a glass container
through Teflon tubing. Additional grab samples were also collected at three otheraquaculture
facilities at different times, with one effluent sample collected from an outfall 72 hours after
treatment. The results of the study revealed the formaldehyde concentrations in samples
6 http://water.epa.gov/scitech/wastetech/guide/aquaculture/upload/20Q5 09 01 guide aquaculture EEBA
EEBA-Chapter-7.pdf accessed 12/5/2014
7 https://www3.epa.gov/regionl0/pdf/permits/npdes/wa/WA Hatchery (IP WAG130000 BE.pdf
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
collected at the outfall location during treatments ranged from 1.8 to 7.1 milligrams per
liter (mg/L). The analysis of the sample collected 72 hours after treatment revealed 0.2
mg/L formaldehyde. The analysis of samples collected at the downstream locations varied
in formaldehyde concentration of 0.9 to 1.9 mg/L. The study concluded that formaldehyde
concentration downstream of land based aquaculture facilities could cause an adverse chronic
impact to aquatic organisms.8
PROJECT DESCRIPTION
Selection of Sampling Sites
In order to select hatcheries at which to sample, the EPA and Ecology worked with staff
and managers at U.S. Fish and Wildlife Service (U.S. FWS), Idaho Department of Fish and
Game (1DFG), and Washington State Department of Fish and Wildlife (WDFW) to identify
hatcheries that use the most formalin, and to ensure that sampling included a range of
formalin use scenarios (i.e., egg, juvenile, and adult treatments). By sampling formaldehyde
in the effluent at facilities that use the most formalin, and by sampling during peak formalin
use, this study intended to capture a reasonable worst-case scenario for estimations of
formaldehyde concentrations in Pacific Northwest hatchery effluent. The hatcheries at
which sampling was conducted are covered under NPDES aquaculture permits by the EPA
or Ecology. A list of all the hatcheries participating in this study is included in Table 1. The
locations are displayed on the map in Figure 1.
Table 1: Hatcheries Sampled for this Study.
Formalin Consumption
Sampling
Growth
Hatchery Name
Ownership
Gallons Per Year
Sampled By
Date
Stage Treated
Carson National Fish Hatchery
U.S. FWSa
516
EPA/OERA
7/13/2016
Adults
Clearwater Fish Hatchery
IDFGb
1,650
EPA/OERA
7/20/2016
Adults
Cowlitz Salmon Hatchery
WDFWC
6,000
Ecology
9/30/2016
Adults
Dworshak National Fish Hatchery
U.S. FWS
2,680
EPA/OERA
7/18/2016
Adults
Hoodsport Fish Hatchery
WDFW
1,155
Ecology
12/7/2016
Eggs
Kalama Falls Fish Hatchery
WDFW
1,554
Ecology
9/12/2016
Adults & Eggs
Leavenworth National Fish Hatchery
U.S. FWS
4,400d
EPA/OERA
8/17/2016
Adults
Little White Salmon National Fish Hatchery
U.S. FWS
370
EPA/OERA
7/11/2016
Adults
Priest River Fish Hatchery
WDFW
2,310
Ecology
11/4/2016
Adults
11/30/2016
Eggs
Wallace River Fish Hatchery
WDFW
2,575
Ecology
9/19/2016
Adults & Eggs
3 United States Department of Fish and Wildlife Service
b Idaho Department of Fish and Game
c Washington State Department of Fish and Wildlife
d Not including treatment of egg, juvenile, and adult Coho Salmon done by the Yakama Nation
8 Lalondc BA, Earnest W, Garron C, (2015) Formaldehyde Concentration in Discharge from Land Based
Aquaculture Facilities in Atlantic Canada. Bulletin of Environmental Contamination and Toxicology 94:444-
447
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Figure 1: Locations of fish hatcheries participating in the EPA sampling events
PUFCELL MOUNTAINS K
Wallace River Hatchery
ra
^3tMc Leavenworth National Fisto..Hatchery
Hoodsport Hatchery_ A
Cowlitz Salmon Hatchery PnelR|Pids Hatchery Clearwater Fish Hatchery (State)
H Carson National Fish Hatchery
Kalama Falls Hatchery A
U»m Little White Salmon National Fish Hatchery
Dworshak National Fish Hatchery
BITTEftROOT RANQE
IDAHO
J G K E A r SANDY DESERT
HARNEY B AS I
Legend
Ecology collected samples at WDFW hatcheries
EPA collected samples at USFWS hatcheries
Fish Hatchery Sampling 2016
EPA and Ecology
v»EPA GISTeam
EPA Sampling of Hatcheries
Between July 11, 2016 and August 17, 2016, OERA conducted site visits at five hatcheries
to obtain samples for analysis and associated supporting data to determine the concentrations
of formaldehyde being discharged through hatchery outfalls following formalin treatments.
Prior to visiting the sites, the managers of the hatcheries were interviewed by phone to
discuss the logistics of the planned site visits. Appendix 2 includes contact information
and aerial photographs showing the sampling locations at each of the hatcheries visited by
OERA. Appendix 3 includes a collection of digital images showing examples of the sampling
and field measurements taken during the site visits.
Sampling was performed in accordance with an approved quality assurance project plan
(QAPP) at a minimum of three locations per fish hatchery: 1) the influent raw water; 2) the
effluent water; and 3) the receiving water. A copy of the QAPP is included in Appendix 4.
Samples from facility outfalls where treated effluent would be discharged were collected
as both grab samples collected by hand and discrete interval samples collected with an
automated sampler. The grab samples were collected after at a period when it was believed
that the plume with the highest likely concentration of formaldehyde was being discharged
through the outfall. The analytical parameters for influent raw water and effluent, are
applicable field measurements (temperature, total chlorine, ammonia, dissolved oxygen,
conductivity, turbidity, pIT, and formaldehyde screening) and laboratory analysis for
formaldehyde. Ammonia reacts with formaldehyde thus the presence of ammonia will result
in a low bias for formaldehyde. Chlorine reacts with ammonia to create chloramines and will
slowly oxidize the formaldehyde to formic acid.
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
While significant concentrations of formaldehyde in the influent water were not expected,
it was possible that at certain locations, formaldehyde occurs naturally or that other
contaminants from upstream (including but not limited to pesticides and fertilizers used in
agricultural or forestry operations) may interfere with formaldehyde analysis. The composite
downstream sample was collected to reveal the concentration of formaldehyde downstream
of the facilities after mixing the effluent with the receiving water.
Ecology Sampling of WDFW Hatcheries
Between September 12, 2016, and December 7, 2016, Ecology collected samples during
six events from five fish hatcheries managed by the WDFW (Table 1). Appendix 5 includes
contact information and aerial photographs showing the sampling locations at each of the
hatcheries visited by OERA. At the Priest Rapids Hatchery, sampling was conducted once
during adult treatment, and on a separate date during egg treatment in order to capture any
differences in formaldehyde concentrations during the two treatment types. At the other four
hatcheries, one site visit was performed, in which adults and eggs were concurrently being
treated, only adults were being treated, or only eggs were being treated. Ecology's sampling
was performed in accordance with Ecology's QAPP for this project based on the original
EPA QAPP. Differences between Ecology and EPA sampling included minor variations in the
equipment used for sampling and field screening. Copies of Ecology's QAPP, field notes, and
results of analysis have already been provided to the NPDES Permits Unit. Ecology's QAPP
is included in Appendix 6.
EPA staff participated in one of Ecology's field sampling events, assisting with sampling
performed at the Kalama Falls Hatchery. EPA also provided supplies including sample
containers and field test kits. All of the samples collected by Ecology were analyzed for
formaldehyde by the EPA Region 10 Laboratory.
METHODS AND MATERIALS
1. Field Measurements
Chlorine measurements were performed on site using a glass sample cell designed for use
with a HACH® Chlorine Colorimeter with the quality control verification performed with the
aid of a HACH® Chlorine DPD Secondary Standard Kit. Measurements of pH, temperature,
turbidity, conductivity, and dissolved oxygen were made in-situ with a Horiba® model U53
water quality meter during collection of the physical samples. Ammonia screening was
performed with the aid of a HACH® ammonia test strip kit and the formaldehyde screening
was performed with the aid of a Quantofix® formaldehyde test kit.
2. Water Sampling
Water samples were collected with portable Sigma® model 900 composite water samplers.
The samplers were deployed to three locations at each hatchery: the influent point, the
effluent point, and downstream. The samplers were programmed to obtain a timed composite
sample from the influent and downstream locations and set for timed discrete samples from
the effluent location. The samples were collected over a facility specific sampling period
that bracketed the application of formalin. The sample collection containers were iced
during sample collection and preserved, stored, and shipped with wet ice as the coolant. The
temperature of each cooler containing samples were checked with an infrared thermometer
upon arrival at the laboratory. The formaldehyde sample containers were QC-Class 125
milliliter (ml) glass jars with Teflon lids.
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
EPA Health and Safety Considerations
OERA field work performed during this project was done according to health and safety
guidelines approved by OERA Management. There were no adverse health and safety
incidents identified by the sampling team during sample collection or field analysis. Special
care was taken to disinfect equipment between facilities in an effort to avoid potential spread
of contamination or pathogens from one facility to another.
3. Analytical Methods
The water samples were analyzed for formaldehyde at the U.S. EPA Region 10 Laboratory
using method EPA 1667a titled Formaldehyde, Isobutyraldehyde, and Furfural by
Derivatization Followed by High Performance Liquid Chromatography. This method is
for surveying and monitoring under the Clean Water Act. Method sensitivity can be varied
depending upon the expected concentration. At the start of this project it was decided
to pursue the lowest range of sensitivity to capture concentrations well below the target
maximum of 10 ppm. Doing so required that most of the positive samples were analyzed at a
10:1 dilution. A short holding time and only a single container of each sample precluded re-
extraction or duplicate analysis for any sample except the field duplicates.
4. Quality Assurance and Quality Control
One field blank and one field duplicate sample was collected during most of the sampling
events. The field blank sample consisted of laboratory-grade deionized (DI) water that was
prepared for formaldehyde analysis by running approximately five gallons of DI water
through the Sigma® automatic composite samplers prior to initial use and before moving to
the next sample location. Samples were shipped to the laboratory under chain of custody with
coolers sealed shut with application of custody seals. Signed copies of the chain of custody
documentation showing the condition of samples upon receipt at the laboratory are included
in Appendix 7. Copies of Ecology chain of custody documentation is included in Appendix 8.
RESULTS OF ANALYSIS
EPA Sampling
The results of the formaldehyde analysis of effluent samples collected from four of the
facilities are summarized in Figure 2. The graph displays the results for samples collected at
ten minute intervals at the Little White Salmon National Fish Hatchery, the Carson National
Fish Hatchery, the Dworshak National Fish Hatchery, and the Clearwater Fish Hatchery. In
all cases the maximum, concentration of formaldehyde measured did not exceed the FDA
Acceptable Formaldehyde Discharge Concentration of 10 parts per million (ppm), which
is equivalent to 10 mg/L. Effluent samples collected from the Leavenworth National Fish
Hatchery were collected at 20 minute intervals. The results of the formaldehyde analysis of
effluent samples collected from the Leavenworth National Fish Hatchery are summarized in
Figure 3. The results reported are expressed in micrograms per liter (|ig/L).
The results of the OERA field measurements taken during sampling events at the hatcheries
are summarized in Table 2. The water quality measurements, including the results of
ammonia and chlorine analysis, did not impact the analysis of water samples tested for
formaldehyde in the laboratory.
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Table 2.
Summary of OERA Field Measurement Data
Hatchery
Measurement
Temp.
Temp.
PH
Turbidity
Conductivity
Dissolved 02
Ammonia
Chlorine
Formaldehyde
Name
Location
°C
°F
NTU
Ms
ppm
test strip ppm
ppm
test strip ppm
Little White Salmon NFH
Influent
7.91
46.24
7.08
0.82
0.043
12.83
ND
0.03
ND
Effluent
7.73
45.91
6.48
1.85
0.043
11.05
ND
0.01
10
Receiving Water
8.27
46.89
6.99
0.85
0.043
11.24
ND
0.05
ND
Carson NFH
Influent
9.36
48.85
5.79
0.18
0.049
12.79
ND
0.08
ND
Effluent
9.23
48.61
5.93
2.04
0.049
11.27
0.25
0.01
10
Receiving Water
11.58
52.84
5.81
0.76
0.058
8.96
0.25
0.01
10
Dworshak NFH
Influent
7.34
45.21
6.76
0.7
0.032
14.73
ND
0.05
ND
Effluent
7.59
45.66
6.27
0.76
0.032
16.62
ND
0.09
10
Receiving Water
7.54
45.57
6.72
0.8
0.032
16.62
ND
0.09
ND
Clearwater FH
Influent
10.73
51.31
6.34
0.75
0.032
14.73
ND
0.07
ND
Effluent
12.58
54.64
6.64
1.15
0.035
14.82
0.25
0.11
10
Receiving Water
7.36
45.25
6.29
1.04
0.033
13.77
ND
0.06
ND
Leavenworth NFH
Influent
14.62
58.32
7.26
No Meas
0.035
11.94
ND
ND
ND
Effluent
14.73
58.51
7.36
2.04
0.076
8.05
0.25
ND
ND
Receiving Water
15.58
60.04
7.53
0.19
0.041
15.39
0.25
ND
ND
Analysis of the influent water at all of the hatcheries resulted in no formaldehyde detected.
In addition, there were no detectable interferences noted, these would be seen as absorbing in
the near-ultraviolet and interfering with the quantitation of the derivatized formaldehyde. The
results of analysis of the receiving waters collected as composite samples revealed varying
concentrations of formaldehyde ranging from an estimated 96 |ig/L downstream from the
Clearwater Hatchery to 1000 |ig/L downstream from the Carson Hatchery. Analysis of the
grab samples collected at four of the fish hatcheries revealed concentrations of formaldehyde
ranging from none detected (<20 |ig/L) at the Clearwater Fish Hatchery to 2000 |ig/L at the
Little White Salmon National Fish Hatchery.
Analysis of the field blanks collected at the hatcheries revealed no formaldehyde detections.
Also, the results of analysis for field duplicates showed variable reproducibility. The field
duplicate results are summarized in Table 3. For the most part, there was pretty good
agreement between field duplicates with the relative percent difference ranging between 0
and 32.3%. The one exception was for the field duplicate collected at the Clearwater fish
hatchery where the initial sample had 32 |ig/L and the duplicate was < 20 |ig/L.
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Figure 2: Concentrations of formaldehyde for hatchery effluent sampled at 10-minute
intervals.
10000
8000
6000
o
CO
0
o
O 4000
O
2000
Blue Line = 10 ppm FDA Acceptable Formaldehyde Discharge Concentration
OERA Sampling Result of Analysis
Formaldehyde\Fish Hatchery Study
Little White Salmon NFH - Blue
Carson NFH - Red
Dworshak NFH - Green
Clearwater FH - Purple
Little White Salmon NFH
Dworshak NFH
Carson NFH
Cleawater Fish Hatchery
10 20 30 40 50 60 70 80 90 100 110 120
Time (every ten minutes)
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Figure 3: Concentrations of formaldehyde for hatchery effluent sampled at 20-minute
intervals.
10000
8000
6000
4000
2000
Blue Line = 10 ppm FDA Acceptable Formaldehyde Discharge Concentration
OERA Sampling Results of Analysis
Formaldehyde\ Fish Hatchery Study
Leavenworth National Fish Hatchery - Orange
Leavenworth NFH
60 80 100 120 140 160 180 200 220 240 260
Time (every 20 minutes)
Table 3.
Summary of Field Duplicate Measurments
Hatchery
Name
Measurment Sample Duplicate
Location Number Result jig/L Number
Result ^g/L RPD
Little White Salmon NFH Effluent
Carson NFH Effluent
Clearwater FH Effluent
Leavenworth NFH Effluent
16284107
16284124
16294128
16334105
1300
120
32
490
16284116
16284135
16294136
16334118
1800
140
<20
490
32.3
15.4
50 -200
0
The relative percent difference (RPD) for the Clearwater fish hatchery duplicate samples is
expressed as a range given the detection limit of 20 |ig/L.
Additional Information Collected
During the site visits, the field team collected additional information on the species of fish
being treated with formalin, the type of formalin being applied, and the conditions under
which it was being applied. The aquatic species being treated during all of the site visits was
10
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Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
adult spring Chinook salmon (Oncorhynchus tshawytscha). The formulation of formalin
used at all of the federal hatcheries was Parasite-S, New Animal Drug Application (NADA)
number 140-989, manufactured by Western Chemical, Inc. In the case of the Clearwater fish
hatchery, the fish were being treated with a generic version of Parasite-S containing 37%
formaldehyde called Formacide-B, Abbreviated New Animal Drug Application (AN AD A)
number 200-414, distributed by Georgia Pacific.
During the field visits, the sampling team noted there was variation in the layout of the
facilities and the methods used to measure water flow and administer formalin. All the
facilities were using a flow-through method of treatment which typically lasted for 60
minutes. The target concentration of formalin applied ranged between 150-200 ppm. In
each case, it appears the facilities were making a good effort to follow the formalin label
instructions. One minor discrepancy noted was at the Leavenworth National Fish Hatchery.
The treatment was applied at a rate of 200 ppm (|.ig/L), but the water temperature measured
by EPA was 14.62°C (58.32°F) for the influent water and 14.73oC (58.51°F) for the effluent
water. The formalin label states that in water greater than 50°F (10°C) the concentration of
formalin should be up to 170 (.ig/L. It would appear the formalin is being over applied for the
temperature conditions at this facility.
One observation made at the Little White Salmon National Fish Hatchery was that the
outfall used for routine monitoring under the NPDES permit appears to be different from
the water channel used to discharge formalin treated water into the Little White Salmon
River. Another complication encountered at this facility was an apparent power outage
during sampling that caused the pump administering formalin to stop during treatment. This
resulted in an incomplete and relatively distorted data displayed as the blue plot in Figure
2. As the sampling was terminated at 110 minutes, we do not know if the concentration
of formaldehyde exceeded the highest level measured which was 3700 |ig/L for sample
16284112.
Ecology Sampling
Results of analysis for the Ecology samples were similar to the results of analysis from the
samples collected by EPA, and the concentration of formaldehyde did not exceed the 10 ppm
acceptable threshold set by FDA.
Data resulting from analysis of the Ecology samples are displayed in Figures 4, 5, and 6. The
only potential discrepancy noted is shown in Figure 10 representing the data from analysis of
samples from the Cowlitz Hatchery. There is a steep decline (from 2100 |ig/L) in the curve to
none detected (<20 |ig/L) at 180 minutes and then a steep incline (to 1700 |ig/L) afterward.
This means that formaldehyde, if any, was below the detection limit for sample 16395258, a
discrete sample collected at 1:00 PM. It is likely that this was an error caused by a mislabeled
container.
The results of the Ecology field measurements taken during sampling events at the hatcheries
are summarized in Table 4. The water quality measurements including the results of ammonia
and chlorine analysis, did not impact the analysis of water samples tested for formaldehyde
in the laboratory.
11
-------
Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Table 4.
Summary of Ecology's Field Measurement Data
Hatchery Name
Measuremen
t Location
Temp (deg C)
Temp (deg F)
pH
Specific
Conductance
(uS/cm)
Dissolved
Oxygen (ppm)
Ammonia Test
Strip (ppm)
Chlorine (ppm)
Formaldehyt
Test Strip
(ppm)
Cowlitz Salmon Hatchery
Influent
12.29
54.122
7.62
49.1
10.51
ND
ND
ND
Effluent
12.17
53.906
7.55
49.6
11.04
ND
ND
ND
Receiving
Water
11.94
53.492
7.5
49.2
10.49
ND
0.07
ND
Hoodsport Hatchery
Influent
6.94
44.492
7.6
72.2
12.13
ND
0.03
ND
Effluent
6.83
44.294
7.43
72.2
11.52
ND
0.015
10
Receiving
Water
6.81
44.258
7.62
83.5
12.18
ND
0.02
0-10
Kalama Falls Hatchery
Influent
11.94
53.492
7.53
60.5
11.1
ND
0.01
ND
Effluent
12.38
54.284
7.76
61.4
10.42
ND
ND
ND
Receiving
Water
12.4
54.32
7.61
60.7
11.06
ND
0.09
ND
Priest Rapids Hatchery
Influent
15.85
60.53
7.78
227.4
9.72
ND
ND
ND
(Visit 1)
Effluent
14.5
58.1
7.87
142.8
10.11
ND
0.02
10
Receiving
Water
14.68
58.424
8
141.4
10.34
ND
ND
10
Priest Rapids Hatchery
Influent
13.31
55.958
7.9
135.1
10.56
ND
0.07
0-10
(Visit 2)
Effluent
10.88
51.584
8
138.4
11.01
ND
0.06
0-10
Receiving
Water
10.94
51.692
8.01
137.9
11.32
ND
0.04
ND
Wallace River Hatchery
Influent
13.2
55.76
7.3
30.1
NA
ND
ND
ND
Effluent
13.16
55.688
7
33.1
NA
0.25
ND
10
Receiving
Water
12.89
55.202
7.19
27.3
NA
ND
0.06
ND
Figure 4: Concentrations of formaldehyde for hatchery effluents sampled at 20-minute
intervals (Ecology).
10000
Blue Line =10 ppm FDA Acceptable Formaldehyde Discharge Concentration
Ecology Sampling Results of Analysis
Formaldehyde\Fish Hatchery Study
Wallace River Fish Hatchery - Pink
8000 — Kalama Falls Hatchery - Green
Priest River 1 (adult treatment sampling) - Red
Priest River 2 (egg treatment sampling) - Blue
6000
4000
2000
Wallace River Fish Hatchery
Kalama Falls Hatchery
Priest River 2
Priest River 1
80 100 120 140 160 180 200 220 240
Time (every 20 minutes)
12
-------
Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Figure 5: Concentrations of formaldehyde for hatchery effluent sampled at 30-minute
intervals (Ecology).
Blue Line = 10 ppm FDA Acceptable Formaldehyde Discharge Concentration
10000
8000
Ecology Sampling Result of Analysis
Formaldehyde\Fish Hatchery Study
Cowlitz Fish Hatchery - Brown
^ 6000
3
C
o
ro
c
O)
o
O 4000
O
2000
Cowlitz Fish Hatchery
0 30 60 90 120 150 180 210 240 270 300 330 360
Time (every 30 minutes)
Figure 6: Concentrations of formaldehyde for hatchery effluent sampled at 10-minute
intervals (Ecology).
Blue Line = 11) ppm hUA Acceptable hormaldehyde Discharge Concentration
10000
Ecology Sampling Results of Analysis
Formaldehyde\Fish Hatchery Study
Hoodsport Fish Hatchery - Aqua Blue
8000
6000
4000
2000
Hoodsport Fish Hatchery
0
0 10 20 30 40 50 60 70 80 90 100 110 120
Time (every 10 minutes)
13
-------
Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
Additional Information Collected
At the five WDFW hatcheries sampled, both adults and eggs were treated using Parasite-S
from Western Chemical. Among the hatcheries, adult treatments lasted 1 -2 hours, while egg
treatments lasted 15 minutes. Differences in treatment types among the hatcheries (adults,
eggs, or adults & eggs) during the time of sampling were noted. At the Kalama Falls and
Wallace River Hatcheries, both adults and eggs were on station and treated during sampling.
At the Cowlitz Hatchery, only adults were being treated during sampling. During the first
Priest Rapids Hatchery sampling event, both adults and eggs were on station, but only adults
were treated during the time of sampling. During the second Priest Rapids Hatchery sampling
event, only eggs were on station and treated. The Hoodsport Hatchery typically only treats
eggs, unless adult treatments become necessary. During the sampling the typical formalin
concentration used for adults was 1:6000 ( -166 ppm), while the concentration used for eggs
was 1:600 ( -1666 ppm).
The physical layout of each facility was unique to each hatchery. At the Wallace River
Hatchery, adult and egg treatment effluents had separate discharge points. At the Cowlitz
Hatchery, adult and egg treatment effluents had a single common discharge point. At the
Priest Rapids Hatchery, hatchery effluent was mixed with river water in a long concrete canal
structure before being discharged into Jackson Creek, which eventually empties into the
Columbia River. At the Hoodsport Hatchery, sampling was timed to coincide with a low/ebb
tide to minimize the influence of saltwater at the receiving water site.
CONCLUSION
In all of the hatcheries sampled for this study, the maximum concentration of formaldehyde
measured did not exceed the FDA and EPA Region 10 level of concern of 10 ppm.
Based on data collected at the hatcheries that participated in this study, as well as the
available toxicological data for threatened and endangered salmonids and an EPA risk
assessment for formalin in Washington hatcheries, the EPA believes that current levels of
formalin use are generally protective of aquatic life and ESA listed salmonids in Pacific
Northwest waters.
14
-------
Water Sampling and Testing for Formaldehyde at Northwest Fish Hatcheries
TECHNICAL NOTES/RECOMMENDATIONS
EPA should consider repeat sampling and analysis at the Little White Salmon National Fish
Hatchery to clarify the location of the permitted outfall in relation to where the effluent
containing formaldehyde was being discharged. In addition, because the pump used to
administer formalin failed during a power disruption, there is uncertainty about the highest
concentration of formaldehyde in the effluent. Repeat sampling and analysis would result in
more complete data for this site.
EPA should also consider repeat sampling and analysis at the Leavenworth National
Fish Hatchery to help confirm the question of water temperature and how it relates to the
concentration of formalin being administered to fish being treated at this facility. In addition,
due to ease of access, this facility would be a good candidate for testing the concentration of
formaldehyde downstream. An automated sampler could be used to collect discrete samples
at the downstream location to provide data on the highest concentration present in the
Wenatchee River downstream from the Leavenworth National Fish Hatchery outfall.
EPA should consider adjusting the analytical method parameters to better reflect the expected
concentrations. At the same time the quality assurance could be modernized by adding a
surrogate to monitor derivatization and extraction efficiency.
15
-------
A
Appendices
16
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Appendix 1
PARASITE-S
Formalin (aqueous formaldehyde solution)
|For control of External Protozoa and Monogenetic Trematodes on all Finfish and External
Protozoans on Penaeid Shrimp; and for control of Fungi on all Finfish eggs.
DESCRIPTION
PARASITE-S is the aqueous solution of formaldehyde gas (this is equivalent to formalin 37% or
37 grams of formaldehyde in 100 mL of solution). U.S.P grade PARASITE-S contains not less
than 37% (by weight) of formaldehyde gas per weight of water and 6 to 14% methanol. In solution,
formaldehyde is present chiefly as H0(CH30)H. Its molecular weight is 30.93. PARASITE-S is
readily miscible with water, methanol, and ethanol and is slightly soluble in ether. It is a clear,
colorless liquid (Heyden Newport Chemical Corporation, 1961).
FISH AND SHRIMP TOXICITY STUDIES
The toxicity of PARASITE-S was measured by standard methods in laboratory bioassays with
rainbow trout Atlantic salmon, lake trout, black bullhead, channel catfish, green sunfish, bluegill,
smallmouth bass, largemouth bass and striped bass. The 3,6,24 and 96-hour LCso (lethal con-
centration for 50% of the animals) values for trout range from 1,230 to 100 pL/L (455 to 37 ppm
formaldehyde); for catfish, from 495 to 65.8 |jl_/L (183 to 24 ppm formaldehyde); for bluegill, from
2,290 to 100 |jl_/L (847 to 37 ppm formaldehyde); for largemouth bass, the values for 6 to 96-hour
LCjq range from 1,030 to 143 |jL/L (381 to 53 ppm formaldehyde) (Bill et al. 1977) and for striped
bass the values for 6 to 96-hour LCsq range from 940 to 30 |jL/L (347 to 11 ppm formaldehyde)
(Bills, Marking & Howe-1993). The 24, 48, 72, and 96-hour LC^ values for penaeid shrimp
range from 712 to 235 |jl_/L (ppm) (Johnson, 1974 and Williams, 1980).
INDICATIONS FOR USE:
1. Parasiticide for Finfish: for the control of external protozoa (Chilodonelta spp., Ichthyobodo
spp, Epistylisspp., Ichthyophthinus spp., Ambiphiyaspp. and Ttichodina spp.), and the mono-
genetic trematode parasites {Cteidodiscusspp., Dactyiogyrus spp., and Gyrodactylus spp).
2. Parasiticide for Penaeid Shrimp: for the control of external protozoan parasites {Bodo
spp., Epistylis spp., and Zoothamnium spp.).
3. Fungicide for Finfish Eggs: for the control of fungi of the family Saprolegniaceae.
DIRECTIONS FOR USE:
1. Parasiticide for Finfish
Concentrations of Formalin
Aquatic species
Administer in Tanks & Race-
ways for up to 1 hr (pL/L)*
Administer in Earthen
Ponds Indefinitely (pL/L)*
Salmon & Trout
above 50°F
up to 170
15-25"""""
below 50 °F
up to 250
15-25" "*
All other finfish
up to 250
15-25" *"
* Microliter per liter (pL/L) = parts per million (ppm).
" Use the lower concentration when ponds, tanks or raceways are heavily loaded with phyto-
plankton, or fish, to avoid oxygen depletion due to the biological oxygen demand created by
decay of dead phytoplankton. Alternatively, a higher concentration might be used if dissolved
oxygen is strictly monitored.
"* Although the indicated concentrations are considered safe for cold and warm water finfish, a
small number of each lot or pond to be treated should always be used to check for any unusual
sensitivity to formalin before proceeding.
2. Parasiticide for Penaeid Shrimp
Concentrations of Formalin
Aquatic species
Administer in Tanks & Raceways
for up to 4 hours (pL/L)*
Administer in Earthen
Ponds Indefinitely (pL/L)*
Shrimp
50 to 100"
k Microliter per liter (pL/L) = parts per million (ppm).
' Treat for up to 4 hours dai ly. Treatment may be repeated daily until parasite control is achieved.
Use the lower concentration when ponds, tanks or raceways are heavily loaded with phyto-
plankton, or shrimp, to avoid oxygen depletion due to the biological oxygen demand created by
decay of dead phytoplankton. Alternatively, a higher concentration might be used if dissolved
oxygen is strictly monitored.
' Treatment may be repeated in 5 to 10 days, if needed
3. Fungicide for Finfish Eggs
Concentrations of Formalin
Aquatic species
Administer in Hatchery Systems (pL/L)*
Eggs of all finfish except Acipenseriformes
1000-2000 for 15 minutes'*
Eggs of Acipenseriformes
up to 1500 for 15 minutes"
* Microliter per liter (pL/L) = parts per million (ppm).
" Apply in constant flow water supply of incubating facilities. A preliminary bioassay should be
conducted on a small subsample of fish eggs to determine sensitivity before treating an entire
group. This is necessary for all species because egg sensitivity can vary with species or strain
and the unique conditions at each facility.
METHODS OF APPLICATION
APPLICATION TO TANKS AND RACEWAYS -Turn off water supply, provide aeration, apply
appropriate amount of PARASITE-S, and thoroughly dilute and mix to assure equal distribution of
PARASITE-S. Treat for up to 1 hour for fish and up to 4 hours for penaeid shrimp, then drain the
solution and refill the tank with fresh, well-aerated water. While tank is under treatment, adequate
oxygen must be present to maintain the fish or shrimp. If needed, aeration should be provided to
prevent oxygen depletion. Treatments may be repeated daily until parasite control is achieved.
APPLICATION TO PONDS - Apply greatly diluted PARASITE-S to the pond evenly using a pump,
sprayer, boat bailer, or other suitable device to assure even distribution. Allow PARASITE-S to
dissipate naturally. Single treatments usually control most parasites, but may be repeated in 5 to 10
days if needed. Treatments for Ichthyophthinus should be made at 2-day intervals until control is
achieved.
APPLICATION TO EGG INCUBATORS - Apply PARASITE-S into a constant water supply flowing
around the eggs. A drip or pressure system should be used and timed. Apply PARASITE-S under
the surface of the water flow
WITHDRAWAL TIME
Zero days.
WARNING
Striped bass have been demonstrated to be hypersensitive to formalin; lethal toxicity has been
noted to occur at levels approximately 2-3 times the recommended therapeutic concentration.
DANGER POISON
USER SAFETY WARNINGS
Exposure to high concentrations of formaldehyde vapor causes severe respiratory irritation
which can be life-threatening. Lower vapor levels can cause irritation to the eyes, respiratory
tract, and skin. Swallowing formaldehyde can be life-threatening. Formaldehyde is an irritant
when splashed on skin or Into the eyes. It can cause severe eye damage, even blindness.
Keep out of reach of children.
Use only with adequate ventilation.
Keep container tightly closed when not in use.
May aggravate a pre-existing asthmatic condition and allergic rhinitis.
Moderate fire and explosion hazard exists when exposed to heat or flame.
Contains methanol - cannot be made non-poisonous. Prolonged exposure to methanol has
been associated with reproduction disorders.
Potential Cancer Hazard; Formaldehyde vapor may be carcinogenic if inhaled. Use
applicable safety protection. (Note; This drug, used as labeled, does not cause
formaldehyde tissue residues in fish).
Employers; Refer to Occupational Safety and Health Administration (OSHA) regulation 29
CFR 1910.1048 for human safety guidance that may be applicable to your specific
operation. OSHA's "action level" concentration for airborne formaldehyde is 0.5 pail per
million (ppm), calculated as an 8 hour time-weighted average (TWA). Use respiratory, skin,
and eye protection when needed (refer to OSHA's regulation 29 CFR 1910.1048). OSHA's
airborne exposure limits (without use of a respirator) for formaldehyde shall not exceed 1)
0.75 part per million (ppm) as an 8-hour, time-weighted average (TWA) or 2) 2 parts per
million (ppm) as a 15-minute, short term exposure limit (STEL). NOTE: The odor of
formaldehyde in the air can generally be detected at about 0.5 to 0.8 ppm (range about 0.05
to 1 ppm).
USER EXPOSURE EMERGENCY AID
INHALATION (Breathing); Get medical aid immediately Remove victim from exposure
wearing protective clothing and respiratory protection appropriate to the type and degree of
contamination. Move victim to fresh air immediately. If breathing is difficult, give oxygen. DO
NOT use mouth-to-mouth respiration. If breathing has ceased, induce artificial respiration
with the aid of a pocket mask equipped with a one-way valve or other proper respiratory
medical device
INGESTION (Swallowing): DO NOT induce vomiting. If the person is conscious, dilute,
inactivate, or absorb the formaldehyde by giving milk, activated charcoal, or water, Get
medical help immediately. If vomiting occurs, keep head lower than hips.
EYE CONTACT: ImmPliately flush eye(s) with large amounts of water for at least 15
minutes, lifting the lower and upper eyelids occastonally, until no evidence of chemical
remains. Seek medical attention immediately DO NOT allow victim to rub eyes or keep
eyes closed for burns to eyes may have a delayed effect.
SKIN CONTACT: Remove contaminated clothing (including shoes) immediately. Wash
affected area of body with soap and large amounts of water until no evidence of chemical
remains (at least 15 minutes). If there are chemical burns, or appreciable eye or respiratory
irritation, get medical help immediately.
PRECAUTIONS
Store PARASITE-S indoors away from direct sunlight, heat, sparks, and open flames, and
ventilate storage area. Do not subject PARASITE-S to temperatures below 40°F (4.4°C).
PARASITE-S subjected to temperatures below 40°F causes the formation of
paraformaldehyde, a substance which is toxic to fish. Paraformaldehyde can be
recognized as a white precipitate at the bottom or on the walls of the container.
Tolerance to PARASITE-S may vary with strain arid species of fish, eggs and shrimp. While
the indicated concentrations are considered safe for the indicated use, a small number of
each lot to be treated should be used to check for any unusual sensitivity to PARASITE-S
before proceeding.
Under some conditions, fish or penaeid shrimp may be stressed by normal treatment
concentrations. Heavily parasitized or diseased fish or penaeid shrimp often have a greatly
reduced tolerance to PARASITE-S. Such animals do not tolerate the normal tank treatment
regimen the first time they are treated. Therefore, time and dosage may need to be reduced.
If they show evidence of distress (by piping at the surface), the solution should be removed
and replaced with fresh, well aerated water. Careful observations should always be made
throughout the treatment period whenever tank or raceway treatments are made. Treatment
should never exceed 1 hour for fish or4 hours for penaeid shrimp (even if they show no sign
of distress), nor should it exceed 15 minutes for fish eggs.
Do not apply PARASITE-S to fish ponds, tanks or raceways with water warmer than 80°F
(27X) when a heavy bloom of phytoplankton is present, or when the concentration of dis-
solved oxygen is less than 5 mg/L (ppm). Do riot apply to penaeid shrimp ponds when the
concentration of the dissolved oxygen is less than 3 to 4 mg/L (ppm). PARASITE-S may kill
phytoplankton and can cause depletion of dissolved oxygen. If an oxygen depletion occurs,
add fresh, well-aerated water to dilute the solution and to provide oxygen.
Because formalin may harm a biofiIter, biofilters should be bypassed during treatment, and
the system should be flushed and replaced with untreated water before reconnecting the
biofi Iter.
Do not use PARASITE-S in a tank, pond or raceway in which methylene blue, or other dyes
which are absorbed, have been recently used.
ENVIRONMENTAL PRECAUTIONS
Do not discharge the contents of fish treatment tanks into natural streams or ponds without
thorough dilution (greater than or equal to 10X). Do not discharge the contents of egg
treatment tanks without a 100X dilution. This will avoid damage to PARASITE-S sensitive
phytoplankton, zooplankton, and fish populations and avoid depletion of dissolved oxygen.
Formaldehyde is identified by the U.S. Environmental Protection Agency (EPA) as a toxic pol-
lutant and hazardous substance and is required by regulation (40 CFR, Pail 122) to be identi-
fied as a discharge for NPDES permits for aquatic animal production facilities, a qua culture
projects and other facilities. Formaldehyde is subject to SARA Title III, Section 313 reporting.
Use, storage, and disposal of this product must be handled in accordance with applicable
local, state arid Federal laws.
STORAGE
Recommended storage temperature 59°F (15°C). DO NOT EXPOSE TO DIRECT SUN-
LIGHT. Store PARASITE-S indoors away from direct sunlight, heat, spark, and open flame,
and ventilate storage area. Do not subject PARASITE-S to temperatures below 40°F (4.4°C).
Manufactured for:
Western Chemical Inc.
VV II 1269 Lattimore Road, Femdale. WA98248
Chemical, Inc. (360)^t5®98
- -- • ver. 020513
NADA 140-989, Approved by FDA
Western
17
-------
Appendix 2
1. Little White Salmon National Fish Hatchery
56961SR14, Cook, WA 98605 BohTurik (509)538-2755
Little White Salmon National Fish Hatchery ^ 4>EPA oisT«m
—"¦.¦yj.-rjj*""'"' l | | | | | | | | * Attar73 -Mm USSSIHI
18
-------
Appendix 2
2. Carson National Fish Hatchery
14041 Wind River Hwy. Carson, WA 98610 Larry Zeigenfuss (509) 427-5905
AR/E^F
Region 10
GISTeam
19
-------
Appendix 2
3. Dworsh ak Nati onal Fi sh Hatchery
4147 Ahsahka Rd. Ahsahka, ID 83520 Mark Drobish (208) 512-9151
Timed discrete sample f
Dworshak National Fish Hatchery »EFA
Regt&fi 10
GIS Team
20
-------
Appendix 2
4. Clearwater Fish Hatchery
118 Hatchery Rd. Ahsahka, ID 83520 TonyFolsom (208)476-3331
H": . ,
Nrvth Fiifir Clrnrwiter
ftiVSf
Region 10
GISTeam
21
-------
Appendix 2
5. Leavenworth National Fish Hatchery
12790 Fish Hatchery Rd. Leavenworth, WA 98826 Chris Foster (509) 548-7641
Region 10
GISTeam
22
-------
Appendix 3
Little White Salmon National Fish Hatchery
July 11, 2016
Jed Jariuch
2 - Automatic sampler deployed at LWSNFH influent
1 - LWSNFH Influent water location location
23
-------
Appendix 3
Little White Salmon National Fish Hatchery
July 11, 2016
Jed Jariuch
3- Automatic sampler deployed at LWSNFH downstream
4- Automatic sampler deployed at LWSNFH outfall
24
-------
Appendix 3
Little White Salmon National Fish Hatchery
July 11, 2016
JedJariuch and Brent Richmond
5 - Brent Richmond measuring water quality parameters
6 - Screening for formaldehyde with test kit downstream
25
-------
Appendix 3
Little White Salmon National Fish Hatchery
July 11, 2016, Jed Januch and Brerit Richmond
7 - Screening effluent water with a formaldehyde test kit
26
-------
Appendix 3
Carson National Fish Hatchery
July 13, 2016
JedJariuch arid Brent Richmond
8- Automatic sampler deployed at CNFH influent location
9- Automatic sampler deployed at CNFH outfall location
27
-------
Appendix 3
Carson National Fish Hatchery
July 13, 2016
JedJariuch arid Brent Richmond
10- Automatic sampler deployed at CNFH downstream
location 11- Screening for formaldehyde with test kit downstream
28
-------
Appendix 3
Carson National Fish Hatchery
July 13; 2016, Jed Januch and Brerit Richmond
12 - Screening effluent water with a formaldehyde test kit
29
-------
Appendix 3
Dworshak National Fish Hatchery
July 18, 2016
Jed Jariuch and Lilian Merger
IB- DNFH influent location
14- Automatic sampler deployed at CDNFH effluent
location
¦ ' ,y
CLLL
"{717(7(7,
, • ^ .
30
-------
Appendix 3
Dworshak National Fish Hatchery
July 18, 2016
Jed Jariuch and Lilian Merger
15- Grab sample outfall location
16- Automatic sampler deployed at DNFH downstream
location
31
-------
Appendix 3
Clearwater Fish Hatchery
July 20, 2016
Jed Jariuch arid Lilian Merger
17- Automatic sampler deployed at CIWFH influent
location
18 - Lilian Herger measuring water quality parameters
32
-------
Appendix 3
Clearwater Fish Hatchery
July 20, 2016
Jed Jariuch arid Lilian Merger
20- Automatic sampler deployed at CIWFH downstream
19- Chlorine test kit - effluent location location
33
-------
Appendix 3
Leavenworth National Fish Hatchery
August 17, 2016
Jed Jariuch arid Raymond Wu
21- Automatic sampler deployed at LNFH influent location
22- Automatic sampler deployed at LNFH effluent location
34
-------
Appendix 3
Leavenworth National Fish Hatchery
August 17, 2016
Jed Jariuch arid Raymond Wu
24- Automatic sampler deployed at LNFH downstream
23- Automatic sampler bottle configuration and wet ice location
35
-------
Appendix 3
Leavenworth National Fish Hatchery
August 17, 2016
Jed Januch and Raymond Wu
23- Automatic sampler bottle configuration and wet ice
36
-------
Appendix 4
QUALITY ASSURANCE PROJECT PLAN (QAPP)
FOR
Water Sampling and Testing for Formaldehyde
at Northwest Aquaculture Facilities
Date: June 2016
Prepared by:
Office of Environmental Review and Assessment
U.S. EPA Region 10
37
-------
Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 2
PROJECT MANAGEMENT
Title and Approval Page
Title; Water Sampling and Testing for Formaldehyde at Northwest Aquaculture Facilities
Approvals;
. - , Digitally signed by Fiiippini,
Filippini, Mario*
1 ~ * Date: 2C16.06.06 16:01:20 -07 00' Date.
Mark Filippini, Manager
Environmental Services Unit
Office of Environmental Review and Assessment
U.S. EPA Region 10
'^/¦v / ' "\ ~ 1 - ¦ ' - Date: v~ /?
Michael Lidgard, Manager >•-'*
NPDES Permits Unit
Office of Water and Watersheds
U.S. EPA Region 10
Digitally signed by JENNIFER CRAWFORD
j - /' " DN: c-US, o-U.S. Government, ou=USEPA.
. , \ , {,,,r -1 ' I ou=5taff, cr=JENNtFER CRAWFORD,
. i \ ( ' v \ dnQuaIifier--0000024857
- ***" Date: 2016,06.07 09:15:28 -G?'00' Date'
Donald Brown, Regional Quality Assurance Manager
Office of Environmental Review and Assessment
U.S. EPA Region 10
38
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0QAPP
June 2016
Page 3
Table of Contents
PROJECT MANAGEMENT 2
Title and Approval Page 2
Table of Contents 3
Acronyms 5
Introduction 6
Distribution List 6
Project/Task Organization 7
Problem Definition/Background 8
Project /Task Description and Schedule 11
Quality Objectives and Criteria for Measurement Data 12
Special Training Requirements/Certification 14
Documentation and Records 15
MEASUREMENT/DATA ACQUISITION 15
Sampling Process Design (Experimental Design) 15
Sampling Methods Requirements 16
Sample Handling and Custody Requirements 18
Analytical Methods Requirements 18
Quality Control Requirements 18
Instrument/Equipment Testing, Inspection, and Maintenance Requirements 19
Calibration Procedures and Frequency 19
Inspection/Acceptance Requirements for Supplies and Consumables 19
Data Acquisition Requirements (Non-Direct Measurements) 19
Data Management 19
ASSESSMENT/OVERSIGHT 20
Assessments and Response Actions 20
Reports to Management 20
DATA VERIFICATION AND USABILITY 20
Data Review and Verification Requirements 20
Review and Verification Methods 20
Reconciliation with User Requirements 21
References Cited 21
Sample Alteration Form 23
Corrective Action Form 24
Site Visit Information Form 25
Data Quality Objectives 27
39
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0QAPP
June 2016
Page 4
Table 1. Project Document Distribution List 6
Table 2. Roles & Responsibilities 7
Table 3. Schedule of Tasks 12
Table 4. Hatchery Information 15
Table 5 Sample Numbers, Types and Locations 17
Table 6. Sample Bottles, Preservation & Date Quality Indicators 22
Figure 1. Organization Chart 8
40
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
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PageS
Acronyms
COC Chain of Custody
DMP Data Management Plan
DQO Data Quality Objective
EPA U.S. Environmental Protection Agency
IDOC Initial Demonstration of Capability
GPS Global Positioning System
LCS Laboratory Control Sample
MEL EPA Region 10 Manchester Environmental Laboratory
MS matrix spike
MSD matrix spike duplicate
NELAC National Environmental Laboratory Accreditation Conference
QA Quality Assurance
QAM Quality Assurance Manager
QAPP Quality Assurance Project Plan
QC Quality Control
RPD relative percent difference
RSCC Regional Sample Control Coordinator
SOP Standard Operating Procedures
TNI The NELAC Institute
41
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
June 2016
PageS
Introduction
This Quality Assurance Project Plan (QAPP) was developed in accordance with the EPA QA guidance (EPA
240-R-02-009)'1'and data quality objective guidance (EPA 240-B-06-001)(2). The sections herein describe
the necessary planning elements for the EPA to conduct sampling and analytical activities at
representative aquaculture facilities within the Region that utilize formaldehyde as a disease treatment
for fish and eggs.
Distribution List
The list of project personnel and their respective contact information is provided in Table 1. The
documentation generated in support of this study and its distribution is also indicated.
Table 1. Project Document Distribution List
Name
Title / Project Role
Organization-Affiliation
Address
Phone
Email
Document Distribution
Catherine Gockel, Permit Writer
Principal Investigator
NPDES Permits Unit
Office of Water and Watersheds
1200 Sixth Ave., Suite 900, OWW-191
Seattle, WA 98101, (206) 553-0325
Gockel.Catherine@epa.gov
QAPP (e-copy) - maintains
official signed e-copy in
project file
Data (QC reports & e-copy)
Dirk Helder, Permit Writer (ID)
NPDES Permits Unit
Office of Water and Watersheds
950 W Bannock, Suite 900
Boise, ID 83702, (208)378-5749
Helder.Dirk@epa.gov
QAPP (e-copy)
Jed ianuch,
Environmental Protection Specialist
Principal Investigator; Scribe Project
Manager
Environmental Services Unit
Office of Environmental Review and
Assessment
7411 Beach Drive East
Port Orchard WA 98366, (360) 871-8731
Januch.Jed@epa.gov
QAPP (e-copy)
Data (QC reports & e-copy)
Donald M. Brown
Regional QA Manager
Office of Environmental Review and
Assessment
1200 Sixth Ave., Suite 900, OERA-140
Seattle, WA 98101, (206) 553-0717
Brown.DonaldM@epa.gov
QAPP (e-copy)
Jennifer Crawford, Chemist
Regional Sample Control Coordinator
Office of Environmental Review and
Assessment
1200 Sixth Ave., Suite 900, OERA-140
Seattle, WA 98101, (206) 553-6261
CrawfordJennlfer@epa.gov
QAPP (e-copy)
42
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 7
Don Matheny, Chemist
QA; Alternate RSCC
Office of Environmental Review and
Assessment
1200 Sixth Ave., Suite 900, OERA-140
Seattle, WA 98101, (206) 553-2599
Matheny.Don@epa.gov
QAPP (e-copy)
Gerald Dodo
Supervisory Chemist
EPA Region 10 Laboratory (MEL)
7411 Beach Drive East
Port Orchard WA 98366, (360) 871-8728
Dodo.Gerald@epa.gov
QAPP (e-copy)
Project/Task Organization
The project organization and lines of authority for this sampling event are provided in Figure 1 with the
roles and responsibilities shown below in Table 2. The information produced by this project is limited
to a summary report describing field observations, measurements, laboratory analytical data and
interpretation for future permitting. Data obtained by this field work will be used to ascertain the
concentration of formaldehyde in Pacific Northwest aquaculture effluent and receiving water. While
evaluation of the final data is the responsibility of the OWW Principal Investigator, other project
personnel may be consulted to provide a scientific perspective on its technical validity, usability and
relevance.
Table 2. Roles & Responsibilities
Project Personnel
Responsibility
Authorities
Principal Investigator,
Office of Water and Watersheds
Provides data interpretation from the perspective of
a potential data user for the purpose of supporting
NPDES permit decisions. Coordinates enrollment
and study logistics with participating facilities.
OWW Programmatic Lead
Principal Investigator,
Office of Environmental Review
and Assessment
Develops QAPP, manages field operations, collects
samples and performs direct fie d measurements.
Coordinates logistics with participating facilities.
OERA Technical Lead
Regional QA Manager
Provides overall QA Program oversight. Delegates
QAPP review/approval to EPA Project QA Staff.
Regional QA Program
Authority
Regional Sample Control
Coordinator (RSCC),
Project QA Staff
Schedules EPA lab support services, coordinates
sample shipments to labs, resolves issues with lab
analyses, and consults on Scribe usage. Provides
unique EPA Sample IDs and Reg onal Project Code.
Reviews and approves QAPP. Reviews Scribe
submissions for completeness.
Authorizes sample
shipments to EPA RIO Lab,
Delegated QAPP Approval
43
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Appendix 4
Formaldehyde fn Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 8
Scribe Project Manager
Data entry or upload into Scribe in accordance with
the Region 10 DMP (EPA Region 10,2014) and QAPP
requirements. Coordinates with RSCC for sample
shipment notification, prints sample labels, exports
electronic COC records to lab. Finalizes and archives
Scribe project file with lab data to Scribe.net.
Custodian of official Scribe
Project File
Region 10 (MEL) Lab Chemistry
Supervisor
Serves as the mair contact between the laboratory
and project personnel. Coordinates with lab team
leaders on sample analysis, data review and
reporting.
Authorizes acceptance of
samples into MEL and the
release of final reviewed
data
Figure 1. Organization Chart
RSCC/Project OA Staff
EPA Region 10
)
Jennifer Crawford
OA Manager
Don Matheny (Alt. RSCC)
Donald M. Brown
Principal Investigators
Catherine Gockel(OWW)
Jed Januch (OERA)
EPA RIO Lab (MEL)
Gerald Dodo
EPA RIO Fieid Staff
Lead:Jed Januch
Staff: Raymond Wu, others
TBO
Scribe Project Manager
Jed Januch
Problem Definition/Background
NPDES Aquaculture Permits
The U.S. Environmental Protection Agency (EPA) and the Washington State Department of Ecology
(Ecology) issue permits under the National Pollutant Discharge Elimination System (NPDES) to establish
conditions for the discharge of pollutants in wastewaters to waters of the United States. In order to
ensure protection of water quality and human health, the NPDES permits place limits on the types and
amounts of pollutants that can be discharged and places other conditions on such activity, such as
monitoring and best management practices.
44
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 9
At 40 CFR §122.24, the U.S. Environmental Protection Agency (EPA) defines concentrated aquatic animal
production (GAAP) facilities as point sources subject to the National Pollutant Discharge Elimination
System (NPDES) permit program and further defines such a facility as a hatchery, fish farm, or other
facility that contains, grows, or holds:
Cold water fish species or other cold water aquatic animals in ponds, raceways, or other similar
structures which discharge at least thirty days per year, but does not include:
a. Facilities that produce less than 20,000 harvest weight pounds of aquatic animals per
year, and
b. Facilities that feed less than 5,000 pounds of food during the calendar month of
maximum feeding.
Warm water fish species or other warm water aquatic animals in ponds, raceways, or other
similar structures which discharge at least 30 days per year, but does not include;
a. Closed ponds which discharge only during periods of excess runoff; or
b. Facilities which produce less than 100,000 harvest weight pounds of aquatic animals per
year.
Cold water aquatic animals include, but are not limited to, the Salmonidae family of fish, e.g. trout
and salmon. Warm water aquatic animals include, bu' are not limited to, the Ameiuride,
Centrarchidae and Cyprinidae families offish, e.g., respectively, catfish, sunfish and minnows.
EPA Region 10 is the NPDES permitting authority for CAAP facilities in Idaho3. In Washington, EPA is the
NPDES permitting authority for federal aquaculture fac lities (i.e., National Fish Hatcheries), and for
aquaculture facilities in Indian Country within the State of Washington5. Ecology is the NPDES permitting
authority for all other hatchery and aquaculture facilities'.
Formalin
Formalin is a generic term that describes a solution of 37% formaldehyde gas dissolved in water. The
Parasite-S formulation is administered as a treatment to control for external protozoa {Chilodonella spp.,
Costia spp,, Epistylis spp., Ichthyophthirius spp., Scyjhidia spp. and Trichodina spp.}, and the
monogenetic trematode parasites (Cleidodiscus spp., Dactylogyrus spp., and Gyrodactylus spp.) on all
finfish. It is also used for the control of fungi of the famil / Saprolegniaceae on all finfish eggs (Western
Chemical label, no date)d.
Formalin is administered to salmon and trout as a bath treatment for prolonged or short periods of time.
The standard dosage recommended in the INAD #9013 Protocol to prevent or control fungus on fish and
eggs is to administer formalin as a static-bath or flow-through treatment at 15 - 2000 (il/L (ppm) active
" liitffs://vosemile.cpa.nov/rlO/water.nsf/iipdcs+permits/general+nt)dc ;+r>eri«iis#Aquaculture
b l)ltps:/A'Oi;emitc.epa.gov/r 10/water.ns£'nodcs ^ermits/mteral+nndc»' oennils^fcdaqua
c IntpMvwv.ecv Ava.gov/PrograrosAvq/permMs/fin tlsMnricx.html
d hUP'.//www.\vchenucal.com/product.s/fish-cgt!-trcalmcnts/parasiie-s- Ponrmlin/parasiie-s.html
45
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0QAPP
June 2016
Page 10
drug. Eggs are treated daily or every other day until hatch. Fish are treated every other day to weeklye
for 30 to 60 minutes, and then transferred to clean water. The formalin concentration is water
temperature dependent and 50°F is the cutoff for the two treatment concentrations. Salmon and trout
are treated up to 170 nL/L at water temperatures above 50°F and 250 |iL/L at temperatures below 50°F.
All other finfish are treated up to 250 |iL/L regardless of temperature. Treatment is not recommended
to exceed 1.0 hour.
In the finding of no significant impact for Parasite-S, the FDA requires a 10-fold dilution of finfish
treatment water and a 100-fold dilution of finfish egg treatment water, which should lead to a discharge
concentration of no more than 25 ppm.f "Hie FDA contended that additional in-stream dilution,
infrequent use, and rapid degradation would render the discharged formalin below a level that causes
significant environmental effects on aquatic animals (formaldehyde, the active ingredient in formalin, is
oxidized in the aquatic environment into formic acid and ultimately into carbon dioxide and water; the
estimated half-life of formaldehyde in water is approximately 36 hours). Directions for dilution of
treatment water and additional environmental precautions are described on the labeling of the product.
For product label information see:
http://www.wchemical.com/downloads/dl/file/id/45/parasite s package insert.pdf.
As part of its Biological Evaluation in compliance with the Endangered Species Act6, the EPA performed
risk assessments to determine whether formalin use at EPA-permitted aquaculture facilities in
Washington and Idaho have the potential to affect threatened or listed species or their critical habitat.
These risk assessments used the best available science. The EPA's risk assessments likely resulted in
unrealistically conservative assumptions, and did not account for in-stream dilution. Based on the
available toxicological data for threatened and endangered salmonids, the EPA believes that the FDA's
dilution requirement will be protective of aquatic life in Pacific Northwest waters.
However, calculating the maximum concentration of water-borne treatments in hatchery effluent can
be challenging. Formalin presents a particularly complicated case because many facilities send their
formalin-treated water to a holding tank, from which it is slowly metered out and mixed with hatchery
water that does not contain formaldehyde. The EPA does not currently have the data inputs to calculate
the formalin concentration in the effluent for individual facilities because we do not have information
on holding tank size, flow and internal dilution rates, facility retention times, etc. for each treatment.
The EPA is undertaking this study to ascertain the concentration of formaldehyde in Pacific Northwest
aquaculture effluent.
Based on many discussions with permittees, USFWS, Ecology, USGS, and the Northwest Indian Fisheries
Commission, the EPA expects that this study will confirm that formalin use in Northwest aquaculture
facilities does not present an ecological risk to listed species or the aquatic environment. If, however,
"http://www.fws.gov/fisheries/aadap/summarvHistorvFornialin.htiTi accessed 8/12/2014
f http://water.eDa.gov/scitech/wastetech/guide/aauacultiire/uDload/2005 09 01 guide aquaculture EEBA EEBA-Chapter-
7.pdf accessed 12/5/2014
8https.7/www3.epa.gov/regionlO/pdfirpermits/npdes/waWA Hatchery GP WAG130000 BE.pdf
46
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 11
the study results suggest that formaldehyde estimated environmental concentrations are unacceptably
high, the EPA will take steps to work with permittees to adjust their formalin use (e.g., treat a smaller
subset of the hatchery at a time, provide more internal dilution prior to discharge, route formalin-treated
water to an offline settling basin, or hold treated water for a longer period of time to allow for
degradation). If the results of this field study demonstrate that formaldehyde estimated environmental
concentrations are higher than allowed on the approved label or higher than acceptable levels to ESA
listed species, formalin will be addressed in future NPDES permits.
Other Background Information/Literature Review
A study focused on measuring the formaldehyde concentration in effluent outfalls at freshwater
aquaculture facilities in Nova Scotia was done by Environment Canada in 2011 and published in the
Bulletin of Environmental Contamination and Toxicology in 2015. Formaldehyde was applied at an
effective rate of 250 microliters per liter (nL/L) to a 10 meter diameter pond with a water temperature
of 50° Fahrenheit (F). Samples were collected at the effluent outfall and at another location 100 meters
downstream of the effluent outfall. Samples were collected with the aid of automated ISCO® samplers
set to obtain 100 milliliters (ml) of water every 5 minutes over a 3-hour period. The ISCO® samples were
composited in a glass container through Teflon tubing. Additional grab samples were also collected at
three other aquaculture facilities at different times, with one effluent sample collected from an outfall
72 hours after treatment. The results of the study revealed the formaldehyde concentrations in samples
collected at the outfall location during treatments ranged from 1.8 to 7.1 milligrams per liter (mg/L). The
analysis of the sample collected 72 hours after treatment revealed 0.2 mg/L formaldehyde. The analysis
of samples collected at the downstream locations varied in formaldehyde concentration of 0.9 to 1.9
mg/L The study concluded that formaldehyde concentration downstream of land based aquaculture
facilities could cause an adverse chronic impact to aquatic organisms.'4'
Project /Task Description and Schedule
The proposed study will monitor the concentration of formaldehyde discharged from fish hatchery
outfalls during treatment of fish and eggs during the summer and fall of 2016. The following list of
samples and field analyses are required:
Samples collected for laboratory analyses may be analyzed for:
• Formaldehyde
Sample analyses and field measurements may be conducted in the field for:
• Flow
• Temperature
• Chlorine (Total)
• Ammonia
• Dissolved Oxygen (DO)
• pH
• Formaldehyde Screening (test kits)
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
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Page 12
See Table 6 for the specific analytical methods, QA/QC, and container and preservation requirements
applicable to this study. Table 3 includes a schedule for conducting tasks related to this project. It is
intended as a guideline only as it is possible that unforeseen circumstances and conditions will require
adjustment to some or all of the following dates and timeframes proposed. Site visits will be planned
during a timeframe when facilities are performing formaldehyde treatments and able to accommodate
EPA access to facilities. EPA will schedule visits with aquaculture facility managers prior to traveling to
the site. In the event that changes are required to travel schedules, field staff will consult their manager
on contingencies.
Table 3. Schedule of Tasks
Activities
Due Dates
QAPP review/approval
June 10, 2016
Sample Collection
July 1 through November 1,2016
Analysis/data Review Completion
Analysis within the technical holding times required by 40 CFR Part 136. Generally,
reviewed data will be provided within 8 weeks of sampling.
Report Preparation
Initial draft within 90 days of receiving the final reviewed analytical results.
Site Sampling Constraints
Time of sample collection is coordinated with the facility manager. Problems with coordinating the
timing of facility treatment with the sample collection are not likely but are possible due to daily facility
conditions. For example, EPA crew is available to do the sampling but the facility does not need to treat
(discharge formaldehyde) on the assigned day. This could result in delay that would either require more
travel time/funds or cause the site to not be sampled.
Quality Objectives and Criteria for Measurement Data
Data quality objectives (DQOs) are statements that define the type, quality, quantity, purpose, and use
of data to be collected. EPA uses a seven-step process for establishing DQOs and developing QAPPs to
help ensure that data collected during a study will be adequate to support reliable decision-making. For
this project the DQOs shown in Attachment 4 and their subsequent data quality indicators and
acceptance criteria were developed.
Data will determine if the concentration of formaldehyde being discharged from Northwest aquaculture
facility outfalls is significant enough to impact aquatic organisms downstream. The LCso for the most
sensitive non-target aquatic species, such as certain crustaceans, is >1.0 mg/L formaldehyde based on
96-hour static LC50 tests.'31 The data should be of sufficient quality to aid in making NPDES permit
decisions. The following is a compilation of the major data quality indicators used to evaluate data quality
for this project.
48
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Appendix 4
Formaldehyde In Fish Hatcheries
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Precision is the measure of agreement among repeated measurements of the same property under
identical or substantially similar conditions. Approximately 5-10% (1 per facility with <20 field samples)
of the field measurements will be made in duplicate by collecting co-located field duplicate samples (or
by collecting well mixed field split samples from a butter churn type mixer) and analyzing both samples
separately. In addition, approximately 5% of the samples will be analyzed in duplicate (analytical
duplicate). For this project, precision will be measured by the relative percent difference of duplicates.
The required precision is specified in Table 6. The calculation for relative percent difference (RPD) is
given as follows:
(Ri - R2) x 100%
RPD =
(R1 + R2)/2
RPD = Relative percent difference
Ri = Matrix spike result
R2 - Matrix spike duplicate result
Accuracy is a measure of the overall agreement of a measurement to a known value; includes a
combination of random error (precision) and systematic error (bias) components of both sampling and
analytical operations. For this project accuracy will be evaluated based on the use of laboratory control
samples (LCS) and matrix spike(s) recoveries. The required accuracy criteria are specified in Table 6. The
calculation for percent recovery of matrix spikes is given as:
(Sm - N)
%Rec= x 100%
Sa
% Rec = Percent recovery
Sm = Spike result
N = Native concentration in the un-spiked sample
Sa = Concentration of Spike Added
For laboratory control samples (LCS) the percent recovery calculation will be determined as follows:
Mv
% Rec= x 100%
7V
% Rec = Percent recovery
Mv = Measured Value in LCS
Tv = True (certified) Value in LCS
49
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
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Page 14
Representativeness is a qualitative term that expresses the degree to which data accurately and
precisely represent a characteristic of a population, parameter variations at a sampling point, a process
condition, or an environmental condition. For this project, samples intended for analysis in the
laboratory will be both composites of influent and outfall waters collected at timed intervals and discrete
grab samples that will be collected following the application of formaldehyde in the facility.
Comparability is a qualitative term that expresses the measure of confidence that one data set can be
compared to another and can be combined for the decision(s) to be made. For this project sample
processing, and the methods for extraction and analysis of Formaldehyde will utilize accepted EPA
methodologies.
Sensitivity is the capability of a method or instrument to discriminate between measurement responses
representing different levels of the variable of interest. For this project, the sensitivity for the
measurement of formaldehyde will be 100 ug/L (ppb). This concentration range is expected to allow for
dilution of the drug through the facility and still allow for a quantitative determination to be made. The
reporting limits for all measurement parameters are provided in Table 6.
Completeness is the measure of the amount of valid data needed to be obtained from a measurement
system. A complete data set will be free of field and laboratory errors and accidents such as broken
sample containers, non-preserved samples when it is required, misidentified samples, and calibration
errors. For this project, a completeness objective of 100% valid laboratory measurements is the goal.
The completeness calculation is given as:
Nv
% Completeness = x100%
Nm
Nv = Number of Valid Measurements
Nm = Total Number of Measurements
Special Training Requirements/Certification
Field samplers will have at a minimum 24-hour Basic Health and Safety training and/or the Hazardous
Materials Incident Response Course and will be in compliance with regional health and safety
requirements such as attending an 8-hour safety training refresher course every year after the basic
training and participation in the medical monitoring program. The field sampling personnel involved
with this project are senior EPA employees with extensive training and experience relevant to the type
of sampling and field analysis required for this project.
50
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Appendix 4
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Page IS
Chemists/analysts performing the analytical work for this project have extensive knowledge, skill and
demonstrated experience in the execution of the analytical methods being requested.
The Scribe Project Manager has been trained in the requirements for regional documentation as
identified in the Region 10 Data Management Plan (2014) document and associated appendices.
Documentation and Records
A field log notebook, photos, GPS locational data, and chain of custody (COC) form generated by Scribe,
will be used to document the sampling and inspection activities. Scribe is a software tool developed by
the USEPA's Environmental Response Team (ERT) to assist in the process of managing environmental
data. This includes sampling/laboratory, locational, observational, and monitoring field data. Scribe is
required for all samples submitted to the EPA Region 10 Laboratory and the EPA CLP.
For each sample location, the following will be recorded in the notebook: facility name and address,
sample numbers, date, time of each sample collection, physical description of each sample collection
point, locational data, weather conditions, color, sample appearance, sample identifier, and
measurements. Scribe documentation will include all required R10 template fields and valid values as
defined in the R10 DMP, including locational data, sample collection information, COCs, labels,
monitoring data, and final validated laboratory results when available. Field duplicates and any field QC
(blanks) will be identified in the Scribe Sample Type field. For fixed laboratory analyses, field duplicates
will be assigned a separate unique sample identifier. Analytical duplicate and matrix spike / matrix spike
duplicate results will be reported with the appropriate laboratory identifier as defined in the lab SOP and
the RIO Universal EDD Data Dictionary (DMP appendix B).
Photographs will be managed in accordance with the R10 SOP OEAFIELDSOP-022.
The laboratory will store all sample receipt, sample login, sample preparation documentation, and
laboratory instrument documentation per the applicable SOPs.
Validated laboratory results and interpretation (if necessary) will be appended to the final report along
with photographs and other supporting documentation.
MEASUREMENT/DATA ACQUISITION
Sampling Process Design (Experimental Design)
Sampling will be done at the following fish hatcheries shown in Table 4 which includes the name of the
hatchery, the location, and a description of the treatment/outfall. Additional information for each
facility will be provided in the site specific inspection plan (SSIP) included in Attachment 3.
Table 4. Hatchery Information
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formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
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Page 16
Name
Location
Estimated Gallons Formalin
Used Per Year
Description of Treatment/Outfall
Leavenworth National Fish Hatchery
leaveriwath, WA
4,400
flow through treatment, 1 outfall
Carson National Fish Hatchery
Carson, W \
516
1 outfall
Little White Salmon National Fish Hatchery
Cook, WA
370
Flow through treatment, 2 outfalls
Dworshak National Fish Hatchery
Ahsahka, D
2,630
Flow through treatment, 1 outfall
Clearwater Fish Hatchery (Idaho Fish and
Same)
Ahsahka, 13
1,650
flow through treatment, 1 outM !
Sampling will be done at the following point .sources: influent raw water, effluent and receiving water
location. Analytical parameters for influent rrw water and effluent, are applicable field measurements
(flow, temperature, total chlorine, ammonia, DO, pH, and formaldehyde screening) and laboratory
analysis for formaldehyde. Ammonia reacts w th formaldehyde thus the presence of ammonia will result
in a low bias for formaldehyde. Chlorine reacts with ammonia to create chloramines and will slowly
oxidize the formaldehyde to formic acid. Dechlorination is required if chlorine is detected.
Sampling Methods Requirements
Field samplers visiting fish hatchery facilities reed to be aware of and be sensitive to bio-security issues
and/or procedures related to the potential disease transmission from one facility to another facility. Fish
hatchery operators may deny access to a faciity because of the existence of a disease or illness at the
facility. In addition, there is a real potential that field samplers may be the vector that transmits a disease
from one facility to another if proper precaut ons are not taken. To the extent possible, field samplers
will adhere to facility specific bio-security measures recommended by hatchery operators. Minimal
recommendations are that visitors to farms wear freshly laundered clothing and clean footwear, or
disposable booties and gloves if appropriate Some aquaculture facility operators may request that
samplers not visit other aquaculture facilities on the day of the visit to their facility. Other options for
decontamination of shoes, clothing, and vehicles (e.g., wearing rubber boots and cleaning them with hot
water and disinfectant before and after an inspector visits a facility or adjacent property) should be used
by field samplers. The USDA-APHIS Veterinary Service /Emergency Program maintain lists of
disinfectants (such as Virkon®) that will help prevent the spread of disease causing bacteria, viruses, and
other microorganisms. Field samplers may need to contact their local USDA-APHIS Office to obtain a
copy of the latest list and follow the recommended disinfection and/or decontamination procedures
before visiting an aquaculture facility.
Samples from the facility outfall will be collected as both grab and composite samples. A single grab
sample will be manually collected after treatment at a period when the plume with the highest likely
concentration of formaldehyde is discharging through the outfall. Three Sigma® composite samplers will
be deployed to the facility influent, effluent and receiving water locations. Samplers will be programed
to obtain composite samples from the influent and receiving water, and timed discrete samples from
the effluent (outfall). Both discrete and composite samples will be collected at 10 minute intervals over
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Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 17
a 2 hour period following formaldehyde treatment. Table 5 below shows the number of samples by
location and sample type. While significant concentrations of formaldehyde in the influent water is not
expected, it is possible that in certain locations it occurs naturally or that other contaminants from
upstream (including but not limited to pesticides and fertilizers used in agricultural or forestry
operations) may interfere with formaldehyde analysis. The samples will be collected over a facility
specific sampling period that will bracket the application of formalin. The sample collection containers
will be iced during sample collection and will be preserved, stored and shipped with ice as the coolant
according to Table 6. The temperature of each cooler containing samples will be checked with an
infrared thermometer upon arrival at the laboratory.
Table 5. Sample Numbers, Types and Locations
Sampling Location
Sample Type
Number of
Samples
Description
Influent
Composite
1
12:1 composite collected at 10 minute intervals
with a Sigma® sampler over a 2 hour period
Effluent
Grab
1
Grab sample manually collected at a time when
the formaldehyde concentration is expected to
be highest
Effluent
Grab
12
12 discrete samples collected at 10 minute
intervals with a Sigma® sampler over a 2 hour
period
Receiving Water
Composite
1
12:1 composite collected at 10 minute intervals
with a Sigma® sampler over a 2 hour period
Samples collected for both composites and grabs will be analyzed as follows:
(1) Formaldehyde laboratory measurements,
(2) One un-preserved container for total chlorine, ammonia, and formaldehyde screening field
measurements.
The formaldehyde sample containers will be QC-Class glass jars with Teflon lids. Chlorine measurements
will be made on site using a glass sample cell designed for use with a chlorine colorimeter. Ammonia
measurements will be made in situ with ammonia test strips such as HACH Ammonia (Nitrogen) Test
Strips, 0-6.0 mg/L, or equivalent. Where applicable, pH, temperature and dissolved oxygen will be
measured in-situ with Horiba® model U53 water quality meters during collection of the physical samples.
Total chlorine and formaldehyde screening measurements will be conducted at each facility, at the
discretion of the field team lead in terms of frequency and location necessary. Flow measurements will
be calculated from measurements taken on-site or will be documented from facility measurements.
At least one blank bottle sample will be obtained and submitted for selected analyses. One or more
facilities will also have field rinsate blanks obtained and submitted for selected analyses. Sigma®
53
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 18
automatic composite samplers will require at least one rinsate blank be obtained for analysis. If
composite samplers are used in more than One location, the Sigma® sampler will be rinsed with blank
water by flushing approximately 5 gallons through the sampler. A field rinsate blank sample will be
collected by running Dl water through the composite sampler, prior to initial use and before moving to
the next sample location.
Depending on the number of facilities to be sampled, the field duplicate ratio of one per facility. Lab QC
will be assigned at a frequency of 5% (1/20 samples).
See the SSIP for approximate sampling numbers, specific analyses, containers, preservation, volumes,
and holding times. All alterations or deviations from this QAPP shall be documented using attachment
1 - Sample Alteration Form.
Sample Handling and Custody Requirements
Sample custody is critical to establishing and maintaining the integrity of samples. Samples are
determined to be in the custody of the designated EPA sample custodian when they are:
• in the physical possession,
• in plain sight,
• secured or locked in a manner that restricts access.
Samples will be kept in the custody of EPA project personnel. Region 10 Chain of Custody procedures
and Chain of Custody forms generated by Scribe will be used. Custody seals (2) will be placed on all
shipping containers/coolers.
Packaging, marking, labeling, and shipping of samples will comply with RIO requirements and all
regulations promulgated by the U. S. Department of Transportation (DOT) in the Code of Federal
Regulations, 49 CFR171 -177 and International Air Transport Association (IATA) regulations.
Analytical Methods Requirements
Monitoring shall be conducted in accordance with accepted analytical procedures (Standard Methods or
other EPA approved methods). See Table 6 for specific methods, reporting limits, etc. applicable to each
facility.
Quality Control Requirements
Quality Control procedures will be implemented per the analytical methods and laboratory standard
operating procedures (SOP's). Data quality indicators are provided in Table 6. Prior to analysis a full
initial demonstration of capability will be performed by the lab.
54
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0QAPP
June 2016
Page 19
Instrument/Equipment Testing, Inspection, and Maintenance Requirements
Field maintenance will be performed where appropriate prior to use of the instruments. The laboratory
will follow their SOP's for any preventative maintenance required on laboratory instruments or systems
used for this project.
Calibration Procedures and Frequency
Field calibration will be performed where appropriate prior to use of the instruments. The Horiba multi-
meter will be calibrated and verified with each day of use in accordance with EPA SOP "Calibration and
use of the Horiba U-53G Multi Water Quality Checker" - OEAFIELDSOP-1QO. Field measurement for total
chlorine and formaldehyde screening will be conducted according to the manufacturer's procedure and
EPA field SOP where applicable.
Laboratory instrumentation and other equipment will be calibrated in accordance with the applicable
analytical procedure, laboratory quality manual and standard operating procedures. Laboratory
instrumentation will be maintained in accordance with the instrument manufacturer's specifications
and/or the Laboratory standard operating procedures.
inspection/Acceptance Requirements for Supplies and Consumables
All sample jars used for this project will be new certified clean and supplied by MEL. These will consist
of glass 12S mL containers for formaldehyde. The field samplers will make note of the information on
the certificate of analysis that accompanies sample jars to ensure that they meet the specifications and
guidance for contaminant free sample containers.
Data Acquisition Requirements (Non-Direct Measurements)
Where recent historical data for QAPP parameters exist from each facility inspected, it may be used for
trends analysis and comparison of results. Facility generated flow data may be acquired at the time of
sample setup and collection.
Data Management
Critical data for this project will consist of field logbook entries, field measurements, sample
identification information (facility identification and sample IDs), locational data, and laboratory sample
results. Field logbooks and photographs will be maintained by the OERA principal investigator and the
information maintained in a project file. All required project data (EPA, 2014 DMP) will be managed in
Scribe and archived to Scribe.net upon project completion. All supportive laboratory documentation will
be kept at MEL in hardcopy format until archived to the federal records center in accordance with the
55
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 20
lab SOP. Prior to final release, an independent check of the laboratory results will be performed internal
to the laboratory.
ASSESSMENT/OVERSIGHT
Assessments and Response Actions
An internal assessment of the data and results may be conducted by the appropriate supervisors and
the Laboratory QA Coordinator. MEL routinely participates in EPA's water pollution performance
evaluation studies (WP Studies). No U.S. EPA system audit is planned for the aquaculture monitoring
activities.
Corrective action procedures that might be implemented from QA results or detection of unacceptable
data will be developed if required (See Attachment 2- Corrective Action Form).
Reports to Management
Besides data verification reports to be provided to the principal investigators, no other QA reports are
planned. If, for any reason, the schedules or procedures above cannot be followed, the appropriate
person must complete the "Sample Alteration Form" (attachment 1) for each element changed and have
the element(s) verified and reviewed by the Project Manager and the QA Office.
DATA VERIFICATION AND USABILITY
Data Review and Verification Requirements
The summary of all analytical results will be reported to the project managers and staff as identified in
Table 1. The raw data for this project shall be maintained by the laboratory. Data verification will also
be performed by MEL for all the analyses prior to the release of data at a level equivalent to 100% Stage
4 Validation Manual (S4VM, EPA 2009). The laboratory will archive the analytical data into their
laboratory data management system.
Review and Verification Methods
All laboratory data generated will be reviewed in accordance with the analytical methods specified in
the QAPP and the MEL data review procedures. All data generated by the laboratory will be reported to
the principal investigators.
The OERA principal investigator will be responsible for reviewing field log notebooks for accuracy and
completeness upon return from the field. Sample results will be appended to the final report. The Scribe
data manager will spot check 10% of the electronic data against the hardcopy results prior to and after
uploading the final laboratory data into Scribe.
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 21
Reconciliation with User Requirements
The principal investigators will review the formaldehyde and flow data in order evaluate if there is
sufficient information to determine whether the dilution criteria for formalin usage within each facility
has been achieved. This will involve evaluating if the reporting limit goals have been achieved and if the
data collection approach was adequate.
References Cited
(1) EPA 240-R-02-009, Guidance for Quality Assurance Project Plans, EPA QA/G-5, December, 2002
(2) EPA 240-B-06-001, Guidance on Systematic Planning Using the Data Quality Objectives Process
- EPA QA/G-4, February, 2006
(3) U.S. EPA Region 10. Biological Evaluation - Federal Aquaculture Facilities and Aquaculture
Facilities Located in Indian Country within the Boundaries of Washington State. December 2015
(4) Lalonde BA, Earnest W, Garron C, (2015) Formaldehyde Concentration in Discharge from Land
Based Aquaculture Facilities in Atlantic Canada. Bulletin of Environmental Contamination and
Toxicology 94:444-447
(5) EPA Region 10,2014, Data Management Plan for Environmental Monitoring and Associated
Geospatial Data, Appendix H, EPA Region 10 Quality Management Plan, January, 2014
(6) EPA Region 10,2015, Quality Assurance Manual for the U.S. EPA Region 10 Environmental
Laboratory, April, 2015
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 22
Table 6. Sample Bottles, Preservation & Data Quality Indicators
Analytical
Group
Number of
Samples'
# of QA
Samples:
Field Dups/
Blanks1
Matrix
EPA
Method
Reporting
Limits
Accuracy
Precision
(RPD)
Complete-
ness
Preservation
Volume,
Container
Holding
Time2
(days)
Laboratory Measurements
Formaldehyde
IS
1/2
Water
1667A
100 ng/L
50-150%
30%
100%
Cool4°C
1x125 mL Glass
Tall / 4xl25mL for one
sample from each facility for
labQC
5 days
Field Measurements
Flow
continuous
1/NA
Water
SOP
Cf/mln
NA
NA
100%
NA
NA
NA
Chlorine
Total*
4
1
Water
DPD
0-4.5 mg/L
+/-0.02 mg/L
NA
100%
NA
NA
Analyze
Immed.
Ammonia
4
1
Water
Test Strip
0-6.0 mg/L
+/- 0.5 color
block
NA
100%
NA
NA
Analyze
Immed.
PH
4
1/NA
Water
150.1
NA
± 0.1 pH
Unit
±0.1 pH
Unit
100%
None
Required
Analyze
Immed.
Temperature
4
1/NA
Water
170.1
NA
0.1°C
NA
100%
None
Required
Field Sample Container
Analyze
Immed.
Dissolved
Oxygen (DO)
4
1/NA
Water
360.1
0.05 mg/L
±2%
30%
100%
None
Required
Analyze
Immed.
1 Number of field arid QC samples represents the estimated number of samples for the influent, receiving water, and outfall per facility. The total number of
samples including field QC will not exceed 20 per facility.
2 For the timed discrete samples, the holding time begins at completion of the collection of the last sample. Formaldehyde derivatization must occur within
5 days of collection and analyzed within 3 days of derivatization. Field measurements indicated as 'analyze immediately' are within a holding time of 15
minutes from collection.
3 Where total chlorine is detected at a point of sample collection, the result must be indicated in the Scribe COC comments / special instructions so that the
lab staff is alerted.
58
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Appendix 4
Attachment 1
Sample Alteration Form
(QAPP Addendum - SPAF # NN)
QAPF Title, Author (company), Revision, and Approval Date of standing 'parent* QAPP:
Project Name and assigned Region 10 Project Code:
Material to be Sampled:
Measurement Parameters:
Standard Procedure for Field Collection and Laboratory Analysis (cite references):
Season for Change in Field Procedure or Analytical Variation:
Variation from Field or Analytical Procedure (reference specific QAPP sections):
Special Equipment, Materials, or Personnel Required:
CONTACT
APPROVAL SIGNATURE
DATE
Initiator:
First and Last Name, Title
EPA Project Manager:
First and Last Name, Title
EPA RIO QA Manager:
First and Last Name
Other project designee (title):
First and Last Name
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 23
59
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 24
Attachment 2
Corrective Action Form
QAPP Title, Author (company), Revision, and Approval Date of standing 'parent' QAPP:
Project Name and assigned Region 10 Project Code:
Sample Dates Involved:
Measurement Parameters:
Acceptable Data Range:
Problem Areas Requiring Corrective Action:
Measures Required to Correct Problem:
Means of Detecting Problems and Verifying Correction:
CONTACT
APPROVAL SIGNATURE
DATE
Initiator:
First and Last Name, Title
EPA Project Manager:
First and Last Name, Title
EPA RIO QA Manager:
First and Last Name
Other project designee (title):
First and Last Name
60
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 25
Attachment 3
Site Visit Information Form
Site Name/Facility Type:
Address:
NPDES Permit Number:
Contact Person:
E-mail Address /Phone Number:
EPA Project Code:
SamDle Numbers:
FacMitv Entrv - Date:
Start Time:
End Time:
GPS Sample Location Influent
Longitude:
Date/Time:
Datum:
Latitude:
WavDoint #:
Effluent
Loneitude:
Date/Time:
Latitude:
WavDoint #:
Receiving Water
Longitude:
Date/Time:
Latitude:
WavDoint #:
Aauatic SDecies treated:
Eggs ~ Juveniles ~
Adults ~
Name of Chemical:
NADA Number:
Other Chemical Treatments with the Last 5 Days: No ~ Yes ~, If yes, list chemicals and concentrations.
Influent Sample
Sampler S/N: Advanced Program-Number of Bottles:
Bottle Volume= Time Between Samples
Tubing Length= Number of Intake Rinses
In-Situ Measurements: pH DO Temperature
(record in Horiba
where applicable) CI Flow Formaldehyde
Effluent Samples
Sampler S/N: Advanced Program-Number of Bottles:
61
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Appendix 4
Formaldehyde In Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 26
Bottle Volume= Time between Samples
Tubing Length= Number of intake rinses
In-Situ Measurements: pH DO Temperature
CI Flow Formaldehyde
Effluent Grab SamplesCollected:
Receiving Water Sample
Sampler S/N: Advanced Program - Number of Bottles:
Bottle Volume= Time between Samples
Tubing Length= Number of intake rinses
In-Situ Measurements: pH DO Temperature
CI Flow Formaldehyde
Treatment Type - Bath ~ Duration: minutes Flow-Through ~ Duration: minutes
Static Bath Treatment
Tank Volume
Liters
Desired Treatment Concentration
|ig/L
Volume of Formalin Needed Per Treatment
Liters
Flow-Through Treatment
Tank Volume
Liters of water treated with formalin
Calculated Flow Rate
Liters/Minute
Duration of Treatment
Minutes
Flow-Through Concentration
|ig/L
Amount of Formalin Added Initially
Liters
Amount of Formalin Added During Treatment
mL/Minute
Volume of Formalin Needed Per Treatment
Liters
Maximum percent Facility Discharge Treated:
Maximum Volume of Water Discharged per Day:
Attachment 4
62
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Appendix 4
Data Quality Objectives
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 27
The Environmental Protection Agency (EPA) has established policy which states that before
information or data are collected on Agency-funded or regulated environmental programs and
projects, a systematic planning process must occur during which performance or acceptance
criteria are developed for the collection, evaluation, or use of these data. To meet this planning
requirement the Agency has developed a 7 step planning process for the development of these
data quality objectives. For this study the results of these planning efforts are documented in
the following sections:
Stepl: State the problem
Describe the problem -
Formaldehyde (formalin) is currently used as a drug at specific aquaculture facilities with
permitted discharges under the NPDES program. However even though there are labelling
requirements that govern its use, there are no effluent limitations nor is there any monitoring
data available on the formalin concentrations at these outfalls or receiving waters. The FDA
recommends that the discharge concentration of formalin not exceed 25 mg/L and the receiving water
concentration not exceed 1 mg/L after dilution. We need to determine if formaldehyde is being
discharged from Northwest aquaculture facilities at concentrations of ecological concern.
Planning Team -
Planning team consists of Catherine Gockel, Program lead from the Office of Water and
Watersheds and Jed Januch, Technical lead from the Office of Environmental Review Assessment.
Other technical consultation was received from EPA Chemists, Steve Reimer and Theresa McBride
(Manchester Lab), Don Matheny (Quality Assurance) and Jennifer Crawford (Quality Assurance &
Sampling) Brent Richmond (Field Services), and Lillian Herger (Environmental Characterization
Unit).
Data Needs and Use -
Data on formalin concentrations at the outfalls and receiving waters of aquaculture facilities who
are actively applying the drug are needed. This information would be used to inform the
aquaculture facility managers on the use and management of this drug in addition to informing
permit writers on possible additions to the future permits.
Resources, Constraints, and Deadlines -
Data collection would be contingent on the timeframes when formalin is being applied at these
facilities and the likely time that the drug would be reaching the facility outfall and receiving
water.
Step 2: Identify the study goals and decisions
The goal of this study is to inform the EPA and Ecology NPDES permit authorities and aquaculture
facility managers on the potential effects of formalin usage within the facilities that apply this
drug.
63
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Appendix 4
Formaldehyde in Fish Hatcheries
Revision 1.0 QAPP
June 2016
Page 28
Step 3: Identify the type of data needed
The type of data needed for this study are formaldehyde concentrations in water samples that
are representative of permitted discharge locations at a time spanning after formalin application
has occurred within the facility.
Step 4: Define the study boundaries
The boundaries of this study are limited to influent, permitted outfalls and downstream locations
at aquaculture facilities that are actively aoplying formalin.
Step 5: Define the analytic approach
Collect samples that represent the highest concentration of formalin being flushed through the
outfall and at a downstream location during and immediately following formalin treatment
(depending on whether the treatment was flow-through or static bath). As a baseline check, co-
collect water flowing into the facility at the same time period. Data on chemical interferences
that are likely to be present include ammonia (via test strip) which also requires analysis of
chlorine. Timeframes for sample collection are dependent on the timing and type of treatment
(eggs, juveniles, etc.) being conducted. Woterflow at the outfall during sample collection and the
amount of formalin used for treatment are also needed to determine if the dilution requirement
of the label is being achieved.
Step 6: Define the acceptance criteria
For this study, acceptance criteria for Formalin data are defined by the analytical method
requirements. This includes testing for possible interferences (e.g., ammonia and chlorine). The
Acceptance criteria are quantitative rules which specify how accurate or how precise the results
of an analytical method must be to be considered acceptable.
Step 7: Optimize the study design
Number of facilities - 5
Number of samples - Total number anticipated will not exceed 90.
Sample specifications - A combination of automated sampling and hand collected grab samples
will be done after treatment at a period when the plume with the highest likely concentration
of formaldehyde is discharging. The estimated time it takes for water at each facility to move
from the treatment area to the outfall was provided by hatchery managers.
64
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Appendix 5
Wallace River Fish Hatchery
14418 383rd Ave SE, Sultan, WA 98294 Bradley Hosteller (360) 793-1382
Wallace Rfver Hatchery
influent
47.865530
-121,717000
Wallace River Hatcher/
Wallace River Hatcnery
Effluent
121.717640
-121.717960
Receiving Water
4 7.S6S898
Region 10
GISTeam
Meters
Das; 6
-------
Appendix 5
Kalama Falls Fish Ffatchery
3900 Kalama River Rd, Kalama, WA 98625 Brian Gale (360)673-4825
Kaldina Falls Hatchery
Influent
40.015840
46.016730
46.01/690
•322.733340
122.732060
•122.732450
Kalama foils Motchery
Kalama falls Hatchery
Effluent
Receiving Water
Region 10
GISTeam
66
-------
Appendix 5
3. Cowlitz Fish Hatchery
125 Salmon Ln, Salkum, WA 98582 Laroria Newhouse (360) 985-7424
influent
Cowlitz Salmon Hatchery
Cowlitz Salmon Hatchery
Cowlitz Salmon Hatchery
46.510000
-122.529970
Effluent
Receiving Water
46.531460
46.512570
122.531540
-122.632430
Region 10
GISTeam
67
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Appendix 5
4. Priest Rapids Fish Hatchery
P.O. Box 937 Mattawa, WA 99349 Glen Pearson (509) 932-4481
Priest Rapids Hatchery (Visit 1 and 2) Influent
Priest Rapids Hatchery (Visit land 2) Effluent
Priest Rapids Hatchery (Visit l and 2) Receiving water
4G.547000
46.537000
46.636679
Priest Rapids Hatchery
(Visit 1 and 2)
Region 10
GISTeam
68
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Appendix 5
5. Hoodsport Fish Hatchery
P.O. Box 606, Hoodsport, WA 98548 Jorge Villarreal (360) 877-6408
F^chCreoK
N Schoolhousc-Hill Rd
Hcodsport Hatchery
Hoodsport Hatchery
Hoodsport Hatchery
influent
47.40W87
Effluent
Receiving Water
47.406960
47.406670
-123.140090
-123.139790
Region 10
GISTeam
69
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Appendix 6
DEPARTMENT OF
ECOLOGY
State of Washington
Quality Assurance Project Plan
Water Sampling for Formaldehyde
at Five Fish & Wildlife Hatcheries
in Washington State: Screening Study
March 2017
Publication No. 17-03-108
70
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Appendix 6
Publication Information
This document is an addendum to the U.S. Environmental Protection Agency's Quality
Assurance Project Plan (QAPP) entitled "Quality Assurance Project Plan for Water Sampling
and Testing for Formaldehyde at Northwest Aquaculture Facilities'" (EPA 2016). The QAPP
describes the objectives of the study and the procedures to be followed to achieve those
objectives.
This document, Quality Assurance Project Plan: Water Sampling for Formaldehyde at Five Fish
& Wildlife Hatcheries in Washington State: Screening Study, is available at:
https://fortress.wa.gov/ecv/publications/SummaryPages/1703108.html
Ecology's Activity Tracker Code for this study is 17-013.
Author and Contact Information
Siana Wong and Brandee Era-Miller
Toxics Studies Unit
Environmental Assessment Program
Washington State Department of Ecology
P.O. Box 47600
Olympia, WA 98504-7710
Communications Consultant: phone 360-407-6764.
Washington State Department of Ecology - www.ecv.wa.gov
o Headquarters, Lacey 360-407-6000
o Northwest Regional Office, Bellevue 425-649-7000
o Southwest Regional Office, Lacey 360-407-6300
o Central Regional Office, Union Gap 509-575-2490
o Eastern Regional Office, Spokane 509-329-3400
Any use ofproduct or firm names in this publication is for descriptive purposes only and does not
imply endorsement by the author or the Department of Ecology.
Accommodation Requests: To request ADA accommodation including materials in a format for the
visually impaired, call Ecology at 360-407-6834. Persons with impaired hearing may call
Washington Relay Service at 711. Persons with speech disability may call TTY at 877-833-6341.
71
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Appendix 6
Quality Assurance Project Plan
Water Sampling for Formaldehyde
at Five Fish & Wildlife Hatcheries
in Washington State: Screening Study
March 2017
Approved by:
Signature:
Date:
Mike Hepp, Compliance Specialist, WQP, Eastern Regional Office
Signature:
Date:
Donald Matheny, Chemist, EPA Region 10
Signature:
Date:
Siana Wong, Author / Project Manager, EAP
Signature:
Date:
Brandee Era-Miller, Author / EAP
Signature:
Date:
Debby Sargeant, Author's Unit Supervisor, EAP
Signature:
Date:
Jessica Archer, Author's Section Manager, EAP
Bill Kammin, Ecology Quality Assurance Officer
Signatures are not available on the Internet version.
EAP: Environmental Assessment Program
WQP: Water Quality Program
72
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Appendix 6
1.0 Table of Contents
Page
2.0 Abstract 7
3.0 Background 7
3.1 Introduction and problem statement 7
3.2 Study area and surroundi ngs 7
3.2.3 Parameters of interest and potential sources 8
3.2.4 Regulatory criteria or standards 8
3.3 Water quality impairment studies 9
3.4 Effectiveness monitoring studies 9
4.0 Project Description 10
4.1 Project goals 10
4.2 Proj ect obj ectives 10
4.3 Information needed and sources 10
4.4 Tasks required 10
4.5 Systematic planning process used 11
5.0 Organization and Schedule 12
5.1 Key individuals and their responsibilities 12
5.2 Special training and certifications 12
5.3 Organization chart 12
5.4 Proposed project schedule 13
5.5 Budget and funding 13
6.0 Quality Objectives 14
6.1 Data quality objectives 14
6.2 Measurement quality objectives 14
6.2.1 Targets for precision, bias, and sensitivity 14
6.2.2 Targets for comparability, representativeness, and completeness 14
6.3 Acceptance criteria for quality of existing data 15
6.4 Model quality obj ectives 15
7.0 Study Design 15
7.1 Study boundaries 15
7.2 Field data collection 15
7.2.1 Sampling location and frequency 15
7.2.2 Field parameters and laboratory analytes to be measured 17
7.3 Modeling and analysis design 17
7.3.1 Analytical framework 17
7.3.2 Model setup and data needs 17
7.4 Assumptions in relation to obj ectives and study area 17
7.5 Possible challenges and contingencies 17
7.5.1 Logistical problems 17
7.5.2 Practical constraints 17
7.5.3 Schedule limitations 17
8.0 Field Procedures 18
8.1 Invasive species evaluation 18
73
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Appendix 6
8.2 Measurement and sampling procedures 18
8.3 Containers, preservation methods, holding times 19
8.4 Equipment decontamination 21
8.5 Sample ID 21
8.6 Chain-of-custody 21
8.7 Field log requirements 21
8.8 Other activities 21
9.0 Laboratory Procedures 21
9.1 Lab procedures table 21
9.2 Sample preparation method(s) 21
9.3 Special method requirements 21
9.4 Laboratories accredited for methods 22
10.0 Quality Control Procedures 22
10.1 Table of field and laboratory quality control 22
10.2 Corrective action processes 22
11.0 Management Procedures 23
11.1 Data recording and reporting requirements 23
11.2 Laboratory data package requirements 23
11.3 Electronic transfer requirements 23
11.4 EIM/STORET data upload procedures 23
11.5 Model information management 23
12.0 Audits and Reports 23
12.1 Field, laboratory, and other audits 23
12.2 Responsible personnel 23
12.3 Frequency and distribution of report 23
12.4 Responsibility for reports 23
13.0 Data Verification 24
13.1 Field data verification, requirements, and responsibilities 24
13.2 Laboratory data verification 24
13.3 Validation requirements, if necessary 24
13.4 Model quality assessment 24
14.0 Data Quality (Usability) Assessment 24
14.1 Process for determining project objectives were met 24
14.2 Treatment of non-detects 24
14.3 Data analysis and presentation methods 24
14.4 Sampling design evaluation 24
14.5 Documentation of assessment 24
15.0 References 25
16.0 Appendix. Glossaries, Acronyms, and Abbreviations 26
74
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Appendix 6
List of Figures and Tables
Page
Figures
Figure 1. Location of participating WDFW hatcheries 9
Tables
Table 1. Participating WDFW hatcheries for this study, estimated formalin used per
year, WDFW contacts for sampling coordination, sampling dates, and
treatment types 8
Table 2. Organization of Ecology staff and project responsibilities 12
Table 3. Proposed schedule for completing field work and data management tasks 13
Table 4. Measurement quality objectives for Hydrolab calibration checks 14
Table 5. Summary of water samples/measurements collected at each hatchery
location 16
Table 6. Summary of sample collection information, laboratory and field methods,
QC objectives, preservation, and holding times 20
75
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Appendix 6
2.0 Abstract
The U.S. Environmental Protection Agency (EPA) is conducting a study to measure the
concentrations of formaldehyde in effluent from aquaculture facilities in Washington and Idaho
(EPA, 2016). In Washington State, EPA is the National Pollutant Discharge Elimination System
(NPDES) permitting authority for federal aquaculture facilities and aquaculture facilities in
Indian Country. The Washington State Department of Ecology (Ecology) is the NPDES
permitting authority for all other aquaculture facilities.
EPA conducted sampling and field analysis at five National Fish Hatcheries as documented in
the EPA Formaldehyde in NWAquaculture Facility Water Study Quality Assurance Project Plan
(QAPP) (EPA, 2016). In coordination with EPA, Ecology conducted sampling and field analysis
at five Washington Department of Fish & Wildlife (WDFW) hatcheries that use formalin.
This report documents Ecology's sampling and field analysis for this project, which is adapted
from EPA's QAPP for the study and the subsequent Addendum to the QAPP (Sample Plan
Alteration Form #2) documenting the addition of Ecology-sampled facilities.
3.0 Background
3.1 introduction and problem statement
Formalin, a 37% by mass aqueous solution of formaldehyde gas, is commonly used to treat and
reduce introduction of external parasites in fish hatcheries. This study is being conducted to
collect empirical data on formaldehyde concentrations in hatchery effluents in Washington State.
The data will be used to determine if concentrations are at levels that pose ecological risk to
threatened species or their critical habitat (EPA, 2016).
Ecology's sampling at state-operated hatcheries was intended to supplement EPA's sampling at
federally operated hatcheries. The addition of state hatcheries provides further empirical data for
the overall study. Details and background about the overall project can be found in EPA's
QAPP (EPA, 2016).
3.2 Sti s
Five WDFW state fish hatcheries that use formalin during treatments were selected for this study
(Table 1, Figure 1). These hatcheries were selected by Ecology based on their relatively high use
of formalin. Formalin use is reported to Ecology by each NPDES-permitted facility in an
Annual Disease Control Chemical Use report.
76
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Appendix 6
Table 1. Participating WDFW hatcheries for this study, estimated formalin used per year,
WDFW contacts for sampling coordination, sampling dates, and treatment types.
I'ii rtici
1 liilchcrv
Ksliiiiiilod
l-'oniiiilin I soil
per Yesir
(Ciillons)
Wm-'W Conlncl
S:im plini>
Ditlc
Type
Kalama Falls
Hatchery
1554
Sam Gibbons
Manager
(360) 673-4825
Sam.Gibbons@dfw.wa.gov
Sept 12,2016
Adults & eggs
Wallace River
Hatchery
2575
Brad Hostetler
FHS4
(360)793-1382
Bradley.Hostetler@dfw.wa.gov
Sept 19,2016
Adults & eggs
Cowlitz Salmon
Hatchery
6608
Larona Newhouse
FHS4
(360) 673-4825
Sam.Gibbons@dfw.wa.gov
Sept 30, 2016
Adults
Priest Rapids
Hatchery
2310
Glen Pearson
FHS4
(509) 932-4481
Glen. Pearson@dfw .wa.gov
Nov 4,2016
Nov 30, 2016
Adults (Nov 4)
Eggs (Nov 30)
Hoodsport
Hatchery
1155
Jorge Villarreal
FHS4
(360) 877-2737
Jorge.Villarreal@dfw.wa.gov
Dec 7,2016
Eggs
* Based on formalin use reported to Ecology by each facility in 2014.
3.2.3 Parameters of interest and potential sources
The parameter of interest is formaldehyde. The potential source is the hatchery performing
formalin treatments as part of typical daily operations.
Ancillary data - including ammonia concentration, chlorine concentration, dissolved oxygen
concentration, pH, and water temperature - were also collected.
3.2.4 Regulatory criteria or standards
Under Washington's Upland Fin-Fish Hatching and Rearing General NPDES Permit,
aquaculture facilities that use formalin are required to follow chemical label instructions and
report use and concentration information. Parasite-S by Western Chemical, Inc., is the
commonly used chemical for formalin treatments. In the finding of no significant impact for
Parasite-S, the Food and Drug Administration (FDA) requires a "10-fold dilution of finfish and
penaeid shrimp treatment water and a 100-fold dilution of finfish egg treatment water." This
should lead to a discharge concentration of no more than 25 ppm. According to the FDA, a
77
-------
Appendix 6
discharge concentration <25 ppm, in stream dilution, infrequent use, and rapid degradation of
formalin in water will cause no significant aquatic impact (EPA, 2015)
I E,«" 9
Wallace River Hatchery
9
Hoodsport Hatchery
Olympla
9
Cowlitz Salmon Hatchery
Priest Rapids Hatchery
9
Kalama Falls Hatchery
Figure 1. Location of participating WDFW hatcheries.
3.3 Water quality impairment studies
Not Applicable.
3.4 Effectiveness monitoring studies
Not Applicable.
78
-------
Appendix 6
4.0 Project Description
This section describes the specific objectives and tasks required for Ecology's sampling and field
analysis at participating WDFW hatcheries. More information about the overall project can be
found in EPA's QAPP (EPA 2016). No report or data interpretation will be provided by Ecology
for this project.
4.1 Project goals
The goal of this study was to sample on behalf of EPA to provide an assessment of formaldehyde
concentrations at WDFW hatcheries using the methods outlined in EPA (2016) as closely as
possible.
4.2 Project objectives
The objectives for Ecology's sampling and field analysis were to:
• Collect water samples for laboratory analysis of formaldehyde concentration at each hatchery
sampling site using an ISCO automated composite sampler (ISCO).
• Measure chlorine, ammonia, and formaldehyde concentration using test screening kits at
each hatchery sampling site.
• Measure in-situ water chemistry (temperature, pH, dissolved oxygen) at each hatchery
sampling site.
4 J Information needed and sources
Not Applicable.
4.4 Tasks required
Pre-Sampling Tasks
• Coordinate with EPA staff prior to each sampling event.
• Schedule and verify sampling dates with hatchery managers.
• Print samples labels and obtain Chain of Custody form sent by EPA.
• Calibrate Hydrolab.
• Test ISCOs and charge ISCO batteries.
• Pre-wash sampling equipment.
Field Tasks
• Set up and program ISCOs to collect water samples for laboratory analysis of formaldehyde
at each hatchery sampling site.
• Collect one grab sample per hatchery sampling site for measurement of chlorine, ammonia,
and formaldehyde concentration using test screening kits.
• Measure water temperature, pH, and dissolved oxygen using Hydrolab at each hatchery
sampling site.
• Collect information about formaldehyde treatment from hatchery staff.
79
-------
Appendix 6
Post-Sampling Tasks
• Send copy of Chain of Custody form, water quality data, and GPS coordinates to EPA staff.
• Ship samples to EPA Region 10 Laboratory.
• Perform Hydrolab post-calibration check.
Field Equipment Checklist
• ISCO water sample collection
o ISCO automated samplers x 3
o Pre-washed 1-L wedge-shaped polyethylene bottles x 24
o Pre-washed 10-L glass jug x 2
o 3/8" ID (1/2" OD) polyethylene/vinyl tubing for ISCOs (-50 feet total)
o Clamps for attaching suction line to pump tube
o 3 charged 12-volt batteries + chargers
o 3 cables for connecting 12-volt batteries to ISCOs
o Graduated cylinder for calibration (1000 mL)
o 3 strainers for end of suction line
• GPS for documenting sample locations
• 125-mL glass jars for formaldehyde samples
• Hach Chlorine 46700-00 CL2 Test Kit with Pocket Colorimeter
• Hach AquaCheck Ammonia Test Strips
• QUANTOFIX® Formaldehyde Test Kit
• Calibrated Hydrolab, connection cable, & handheld meter
• Pre-washed 1-L polyethylene bottle for grab samples
• Extended pole for grab samples
• Cooler(s) with ice for water samples
• DI water for field equipment blank
• Field notebook
• EPA-Scribe preprinted labels and Chain of Custody forms (printed copy)
• Other
o
Writing utensils
o
Bubble wrap for sample jars
o
Packaging tape for sample labels
o
Ziploc bags- gallon size for water samples
o
Miscellaneous tools
o
Laboratory gloves
o
Boots, waders, rain gear
4.5
Systematic planning process used
This QAPP and the EPA QAPP (EPA, 2016) represent the systematic planning process for this
project.
80
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Appendix 6
5.0 Organization and Schedule
5.1 Key individuals and their responsibilities
Key Ecology personnel (in addition to those EPA personnel identified in EPA's QAPP) are
summarized in Table 2.
5.2 Special training and certifications
Not Applicable.
5 J Organization chart
See Table 2.
Table 2. Organization of Ecology staff and project responsibilities.
siarr
Title
Responsibilities
Siana Wong
Toxics Studies Unit
Statewide Coordination Section
Environmental Assessment Program
Phone: 360-407-6432
Email: swon461@ecy.wa.gov
Project Manager
Leads field operations. Coordinates logistics
and activities with EPA and participating
WDFW hatcheries.
Brandee Era-Miller
Toxics Studies Unit
Statewide Coordination Section
Environmental Assessment Program
Phone: 360-407-6771
Email: bera461@ecy.wa.gov
Field Lead
Leads field operations. Reviews Ecology's
QAPP.
Debby Sargeant
Toxics Studies Unit
Statewide Coordination Section
Environmental Assessment Program
Phone: 360-407-6775
Email: dsar461@ecy.wa.gov
Unit Supervisor for
the Project Manager
Provides internal review, approves Ecology's
final QAPP, manages budget and staffing
needs
William R. Kammin
Phone: 360-407-6964
Email: wkam461@ecy.wa.gov
Ecology Quality
Assurance
Officer
Reviews and approves the draft and final
QAPP addendum.
81
-------
Appendix 6
5.4 Proposed project schedule
Five WDFW hatcheries that perform formalin treatments were selected for this study (Table 1).
A one-time sampling event at each hatchery was coordinated with each of the hatchery facility
managers during formalin treatment periods between September-December 7, 2016. The Priest
Rapids Hatchery was sampled during two sampling events: once during adult treatments, and a
second time during egg treatments. Contact information and sampling dates for each hatchery
are shown in Table 1. Detailed schedules for each facility were determined in coordination with
the EPA Region 10 lab staff, Principal Investigators, and Regional Sample Control Center prior
to sample collection.
Ecology's sampling was also coordinated with EPA to ensure that similar sampling methods and
procedures were used, and that samples were not submitted to EPA's laboratory during the same
weeks in order to avoid overloading the laboratory's capacity. Ecology staff followed the EPA
Region 10 sample shipment/delivery notification and coordination requirements with the EPA
Regional Sample Control Center and lab staff.
Table 3. Proposed schedule for completing field work and data management tasks
T;isk
Due dale
Lead Mali'
Field work completed
Dec 2016
Siana Wong
All in-situ and grab sample data and site
coordinate information sent to EPA for
entry into Scribe
Dec 2016
Siana Wong
Copies of field notes & files sent to EPA
Project Manager
Jan 2017
Siana Wong
6.5 Budget and funding
Laboratory budget and funding for this project was provided by the EPA.
To complete Ecology's sampling, the EPA provided the following equipment:
• Pocket Colorimeter™ II, Chlorine (Free and Total).
• DPD Total Chlorine Reagent Powder Pillows for a 10 mL sample size.
• Free & Total Chlorine Test Strips, 0-10 mg/L.
• Ammonia (Nitrogen) Test Strips, 0-6.0 mg/L.
• Formaldehyde sample bottles, 125 mL.
All other equipment and staff time was provided by Ecology.
82
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Appendix 6
6.0 Quality Objectives
ctives
See EPA (2016).
6.2 Measurement quality objectives
See EPA (2016) for discussion on Measurement Quality Objectives (MQOs) for this study.
MQOs for Ecology's Hydrolab measurements are shown in Table 4.
Table 4. Measurement quality objectives for Hydrolab calibration checks.
Parameter
Units
Accept
Qualify
Reject
pH
std. units
< or = + 0.2
> + 0.2 and < or = + 0.8
>±0.8
Conductivity*
uS/cm
< or = + 5
> + 5 and < or = + 15
>±15
Temperature
°C
< or = + 0.2
> + 0.2 and < or = + 0.8
>±0.8
Dissolved Oxygen
mg/L
< or = + 0.3
> + 0.3 and < or = + 0.8
>±0.8
* Criteria expressed as a percentage of readings; for example, buffer = 100.2 uS/cm and Hydrolab = 98.7 uS/cm;
(100.2-98.7)/100.2 = 1.49% variation, which would fall into the acceptable data criteria of less than 5%.
6.2.1 Targets for precision, bias, and sensitivity
6.2.1.1 Precision
See EPA (2016).
6.2.1.2 Bias
See EPA (2016).
6.2.1.3 Sensitivity
See EPA (2016).
6.2.2 Targets for comparability, representativeness, and completeness
6.2.2.1 Comparability
See EPA (2016).
6.2.2.2 Representativeness
See EPA (2016).
6.2.2.3 Completeness
See EPA (2016).
83
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Appendix 6
6.3 Acceptara ita
See EPA (2016).
6.4 Model quality objectives
Not Applicable.
7.0 Study Design
The study design follows EPA's study design as described in EPA (2016).
7.1 Study boundaries
See Section 3.2 of this document.
7.2 Field data collection
7.2.1 Sampling location and frequency
At each hatchery, sampling occurred at the influent, effluent (discharge), and receiving water.
Table 5 shows the site location at each hatchery, analyte to be collected/measured at each site,
sample/measurement type, and general collection description.
84
-------
Appendix 6
Table 5. Summary of water samples/measurements collected at each hatchery location.
Siiinplin^
l ocution ;ii
I nch Ihilchcn
An;il.Mc
Coiled ion Tj pc -
# Siiinpk's/
Mc.isii mucins
( oiledion Description
Influent
Formaldehyde
Composite - 1
Automated ISCO sampler set up to collect sample at
20-minute intervals for 4 hours following formaldehyde
treatment (12:1 composite)
Chlorine (Total)
Grab - 1
Hach Chlorine 46700-00 CL2 Test Kit with Pocket
Colorimeter
Ammonia
Grab - 1
Hach AquaCheck Ammonia Test Strips
Temperature
Measurement - 1
Hydrolab MiniSonde
Dissolved Oxygen
Measurement - 1
Hydrolab MiniSonde
pH
Measurement - 1
Hydrolab MiniSonde
Formaldehyde
Screening
Grab - 1
QUANTOFIX® Formaldehyde Test Kit
Effluent
Formaldehyde
Grab - 13
Automated ISCO sampler set up to collect 12 discrete
samples at 20-minute intervals for 4 hours following
formaldehyde treatment.
One grab sample will also be collected manually during
estimated peak formalin discharge.
Chlorine (Total)
Grab - 1
Hach Chlorine 46700-00 CL2 Test Kit with Pocket
Colorimeter
Ammonia
Grab - 1
Hach AquaCheck Ammonia Test Strips
Temperature
Measurement - 1
Hydrolab MiniSonde
Dissolved Oxygen
Measurement - 1
Hydrolab MiniSonde
pH
Measurement - 1
Hydrolab MiniSonde
Formaldehyde
Screening
Grab - 1
QUANTOFIX® Formaldehyde Test Kit
Receiving water
Formaldehyde
Composite - 1
Automated ISCO sampler set up to collect sample at
20-minute intervals for 4 hours following formaldehyde
treatment (12:1 composite)
Chlorine (Total)
Grab - 1
Hach Chlorine 46700-00 CL2 Test Kit with Pocket
Colorimeter
Ammonia
Grab - 1
Hach AquaCheck Ammonia Test Strips
Temperature
Measurement - 1
Hydrolab MiniSonde
Dissolved Oxygen
Measurement - 1
Hydrolab MiniSonde
pH
Measurement - 1
Hydrolab MiniSonde
Formaldehyde
Screening
Grab - 1
QUANTOFIX® Formaldehyde Test Kit
85
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Appendix 6
7.2.2 Field parameters and laboratory analytes to be measured
The following parameters were measured/sampled at each hatchery as documented in the EPA
QAPP:
• Formaldehyde - Lab
• Chlorine (Total) - Field
• Ammonia - Field
• Water Temperature - Field
• Dissolved Oxygen - Field
• pH - Field
• Formaldehyde Screening (test kits) - Field
7.3 Modeling and analysis design
No modeling or data analysis were conducted for this project.
7.3.1 Analytical framework
Not Applicable.
7.3.2 Model setup and data needs
Not Applicable.
7.4 Assumptions in relation to objectives siufJv ^rea
Not Applicable.
7.5 Possible ^kiiienyes arid ^oiitiiKfeicies
7.5.1 Logistical problems
Field work was coordinated with hatchery staff to ensure that sampling occurred on treatment
days during peak formalin treatment periods. Field schedules were also coordinated with EPA
laboratory staff to ensure that the lab could process the samples during the targeted sampling
dates. Each hatchery was visited prior to sampling day to determine sampling sites and identify
any logistical challenges.
7.5.2 Practical constraints
Not Applicable.
7.5.3 Schedule limitations
Not Applicable.
86
-------
Appendix 6
8.0 Field Procedures
8.1 Invasive species evaluation
Not Applicable.
8.2 Measurement and sampling pr> rUine*
Measurement and sampling procedures followed EPA's QAPP (EPA, 2016) as closely as
possible to ensure that data are comparable. No deviations occurred, with the exception of the
type of instruments used for collecting samples (ISCO vs. Sigma automated sampler; Hydrolab
vs. Horiba multi-probe instrument). Calibration of the Hydrolab followed Ecology's SOP
(Anderson, 2016).
Formaldehyde
Formaldehyde samples for laboratory analysis were collected using automated ISCO (Model
6712) samplers. Three ISCO samplers were programmed to collect samples at the influent,
effluent, and receiving water at each hatchery. Prior to sampling, ISCO samplers were calibrated
at each hatchery location to ensure that the accurate volumes were collected.
Each ISCO was programmed to collect the first sample -15 minutes before treatment started and
the last sample ~1 hour after treatment ended. This helped ensure that the pulse of formalin
running through the system was captured.
At the influent and receiving water, a composite sample was collected at 20-minute intervals
over a four-hour period during the formalin treatment application. The composite consisted of
12x250-mL aliquots collected into a single 10-L pre-washed (soap + water followed by
deionized water rinse) glass jug. The internal compartment of the ISCO sampler was filled with
ice to keep the 10-L jug cold during the sampling. After the composite was collected, water
from the 10-L jug was mixed and poured into a single 125 mL glass sample jar, and then stored
in a cooler on ice. The remaining water in the 10-L jug was discarded.
At the effluent, the ISCO sampler was set up to collect 12 discrete samples over a four-hour
period during the formalin treatment. Each discrete sample was comprised of 450-mL water
collected in a pre-washed wedge-shaped 1-L polyethylene bottle. At the end of discrete
sampling, water from each polyethylene bottle was mixed and poured into a 125 mL glass
sample jar (12 total samples). One grab sample for laboratory analysis of formaldehyde was also
collected at the effluent during estimated peak formalin discharge.
All formaldehyde samples were stored in a cooler with ice in the field, and then shipped
overnight to EPA's laboratory for further processing and analysis.
Chlorine (Total)
Chlorine samples were taken from an aliquot of a grab sample collected at each of the influent,
effluent, and receiving water sites. Total chlorine was analyzed on-site using a Hach Chlorine
46700-00 CL2 Test Kit with Pocket Colorimeter. Results were recorded in the field notebook.
87
-------
Appendix 6
Ammonia
Ammonia samples were taken from an aliquot of a grab sample collected at each of the influent,
effluent, and receiving water sites. Ammonia was analyzed on-site using Hach AquaCheck
Ammonia Test Strips, 0-6.0 mg/L. Results were recorded in the field notebook.
Temperature, Dissolved Oxygen, and pH
A calibrated Hydrolab MiniSonde was used to measure in-situ water temperature, dissolved
oxygen, and pH at the influent, effluent, and receiving water sites. The Hydrolab was calibrated
on the day prior to sampling following Ecology's SOP (Anderson, 2016). A post-calibration
check was performed following each sampling event. Table 4 shows the MQOs for post-
calibration checks. Results were recorded in the field notebook.
Formaldehyde screening kit
Formaldehyde screening samples were taken from an aliquot of a grab sample collected at each
of the influent, effluent, and receiving water sites. QUANTOFIX® Formaldehyde Test Strips
were used to analyze formaldehyde concentrations on-site. Results were recorded in the field
notebook.
Flow
Flow information was obtained from facility staff.
Other hatchery facility information
Hatchery facility and formalin treatment information will be obtained from hatchery staff:
• Static Bath Treatment
o Tank volume
o Desired treatment concentration
o Volume of formalin needed per treatment
• Flow-Through Treatment
o Tank volume
o Calculated flow rate
o Duration of treatment
o Flow-through concentration
o Amount of formalin added initially
o Amount of formalin added during treatment
o Volume of formalin needed per treatment
• Maximum percent facility discharge treated
• Maximum volume of water discharged per day
8.3 Containers, preservation methods, holding tsnws
Table 6 summarizes the number of samples collected, QC samples, matrix, laboratory method,
reporting limit, accuracy and precision, completeness, container, preservation, and holding time
for each analyte collected. All formaldehyde samples will be sent to the EPA Region 10
Laboratory for analysis.
88
-------
Appendix 6
Table 6. Summary of sample collection information, laboratory and field methods, QC objectives, preservation, and holding times.
Table is adapted from EPA (2016).
Aiiiil.Mc
#
Siimples
per
link-hen
#<„)C
Siimples:
l-ielri
Dups/
ISIiinks per
lliilehen
M;i(ri\
( olleelion
1 'j pe
Method
Repor-
ting
Limits
Aeeur;ie\
Preeision
tRPI»
( omplele-
ness
( onliii-
ner
Preser-
\ ;il ion
Holding
lime
Formalde
-hyde
15
1/1
Water
Lab Sample
EPA
1667A
100
Hg/L
50-150%
30%
100%
125 mL
Certified
Clean
Glass with
Teflon Lid
Liner
Cool
to
4 C
5 days
Chlorine
(Total)
3
1/NA
Water
Field
Measurement
EPA
330.5
0-4.5
mg/L
±0.02
mg/L
NA
100%
NA
NA
Analyze
Immediately
Ammonia
3
1/NA
Water
Field
Measurement
NA (Test
Strip)
0-6.0
mg/L
± 0.5 mg/L
color block
NA
100%
NA
NA
Analyze
Immediately
Tempera-
ture
3
1/NA
Water
Field
Measurement
EPA
170.1
NA
0.1 C
NA
100%
NA
NA
Analyze
Immediately
Dissolved
Oxygen
3
1/NA
Water
Field
Measurement
EPA
360.1
0.05
mg/L
±2%
30%
100%
NA
NA
Analyze
Immediately
pH
3
1/NA
Water
Field
Measurement
EPA
350.1
NA
0.1
pH unit
0.1
pH unit
100%
NA
NA
Analyze
Immediately
Formalde
-hyde
Screening
(Test Kits)
3
1/NA
Water
Field
Measurement
NA (Test
Strip)
NA
NA
NA
100%
NA
NA
Analyze
Immediately
89
-------
Appendix 6
ation
Prior to sampling, equipment used for collecting samples was washed with hot tap water and
Liquinox soap, followed by tap water rinse and de-ionized water rinse. The specific procedure
for decontaminating equipment can be found in Ecology's SOP (Friese, 2014).
8,5 Sample ID
Ecology coordinated with EPA staff to assign unique sample IDs prior to sampling at each
hatchery.
stody
Chain-of-custody was maintained for all samples throughout the project. As Ecology was acting
as the sampling entity only, with EPA being the data recipient and data user, all samples and
associated field/lab and locational data were managed in a single Scribe file by EPA Office of
Environmental Review and Assessment Environmental Services Unit staff. At minimum,
Ecology hand-entered the sample collection date and time onto pre-printed Scribe sample labels
and Chain of Custody forms for each facility. Immediately after each sampling event, Ecology
scanned the completed printed copy of the Chain of Custody form and completed field form
(EPA, 2016) to the EPA Regional Sample Control Center so that field data could be entered into
Scribe and the lab Chain of Custody XML generated for sample receipt/login.
8.7 Field log requirements
Field data was recorded in a bound, waterproof notebook on Rite in the Rain paper. Attachment
3 of the EPA's QAPP for this project will be used as Ecology's template (EPA, 2016).
8.8 Other activities
Not Applicable.
9.0 Laboratory Procedures
9.1 Lab procedures table
See Table 5 of this document.
S^nipl^ preparation method* s)
Methods for formaldehyde analysis in water samples are documented by EPA Method 1667A.
9.3 Special method requirements
Not Applicable.
90
-------
Appendix 6
9.4 Laboratories accredited iods
All water sample analyses for formaldehyde concentration were performed by the EPA Region
10 Laboratory.
10.0 Quality Control Procedures
10.1 Table ot firiti and lahoratoiv quality renvoi
Table 5 summarizes field duplicate and blank sample collections for each analyte.
Field Duplicates
One duplicate field sample was collected per sampling event for each grab sample analyte
(ammonia, chloride, formaldehyde). One duplicate sample for laboratory analysis of
formaldehyde was also collected from a sample taken from the automated discrete sampler
during each sampling event.
Field Blanks
One field (rinsate) blank was collected per facility and analyzed for formaldehyde at the
laboratory. This was performed by running de-ionized water through the ISCO sampler,
collecting the water in the 10-L glass jug, then pouring the water into a formaldehyde sample jar.
Laboratory Matrix Spike
Following discrete sample collection at the effluent site, three formaldehyde sample jars were
filled from the first ISCO bottle (representing a sample prior to treatment start). The samples
were used by the EPA laboratory to conduct a laboratory matrix spike and matrix spike
duplicate.
10.2 Corrective action processes
All data were submitted to the EPA. Corrective action procedures are described in EPA (2016),
and will be determined by the EPA Principal Investigator for this project.
91
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Appendix 6
11.0 Management Procedures
11.1 Data recording and reporting requirements
See EPA (2016). All data will be submitted to EPA for data reduction and reporting.
11.2 Laboratory < ckage requirements
See EPA (2016). All data will be submitted to EPA.
lO Electronic tictnsfep recjusferneeits
Not Applicable.
1 L4 Elll/STORET data upload procedures
Not Applicable. All data will be submitted to EPA. The EPA Principal Investigator of this
project will provide data upon request.
11.5 Model information management
Not Applicable.
12.0 Audits and Reports
12.1 Field, laboratory, and other audits
To ensure Ecology's sampling and field analysis followed EPA's procedures, Ecology staff
accompanied and observed EPA field staff on one of their sampling dates for this project. In
addition, EPA staff assisted Ecology at the first WDFW hatchery sampled.
12.2 Responsible personnel
Not Applicable.
12.3 Frequency. and disfsibution of report
Not Applicable.
12.4 Responsibility* fot leports
The EPA is responsible for all data reduction and reporting for this project (EPA, 2016).
92
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Appendix 6
13.0 Data Verification
13.1 Field data verification, and
responsibilities
See EPA (2016).
data verification
See EPA (2016).
13 J Validation requirements, if necessary
See EPA (2016).
13.4 Model quality assessmenf
Not Applicable.
14.0 Data Quality (Usability) Assessment
14.1 Process for deft1! milling piojeot objectives wr*-- met
EPA is responsible for all data quality determinations (EPA, 2016).
14.2 Treatment of e ion-detects
See EPA (2016).
14 J Data analysis and presentation methods
All data will be submitted to the EPA for data analysis. Presentation methods will be determined
by the principal investigator.
14.4 Sampling design evaluation
Not Applicable.
14.5 Dociifiienteitian of assessment
See EPA (2016).
93
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Appendix 6
15.0 References
Anderson, P., 2016. Standard Operating Procedures for Hydrolab DataSonde® and MiniSonde®
Multiprobes. Version 2.1. Washington State Department of Ecology, Olympia, WA. SOP
Number EAP033.
http://www.ecv.wa.gov/programs/eap/qa/docs/ECY EAP SOP Hydrolab v2 lEAP033.pdf
EPA, 2015. Biological Evaluation- Federal Aquaculture Facilities and Aquaculture Facilities
Located in Indian Country within the Boundaries of Washington State. U.S. Environmental
Protection Agency.
https://www3.epa.gov/regionlO/pdf/permits/npdes/wa/WA Hatchery GP WAG 130000 BE.pdf
EPA, 2016. Quality Assurance Project Plan for Water Sampling and Testing for Formaldehyde at
Northwest Aquaculture Facilities. U.S. Environmental Review and Assessment, U.S.
Environmental Protection Agency, Region 10.
Friese, M., 2014. Standard Operating Procedures for Decontaminating Field Equipment for
Sampling Toxics in the Environment. Version 1.0. Washington State Department of Ecology,
Olympia, WA. SOP Number EAP090.
http://www.ecv.wa.gov/programs/eap/qa/docs/ECY EAP SOP EciuipmentDeconToxicsSamplin
g vl 0EAP090.pdf
94
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Appendix 6
16.0 Appendix. Glossaries, Acronyms, and
Abbreviations
Glossary of General Tmns
Conductivity: A measure of water's ability to conduct an electrical current. Conductivity is
related to the concentration and charge of dissolved ions in water.
Dissolved oxygen: A measure of the amount of oxygen dissolved in water.
Effluent: An outflowing of water from a natural body of water or from a human-made structure.
For example, the treated outflow from a wastewater treatment plant.
National Pollutant Discharge Elimination System (NPDES): National program for issuing,
modifying, revoking and reissuing, terminating, monitoring, and enforcing permits, and
imposing and enforcing pretreatment requirements under the Clean Water Act. The NPDES
program regulates discharges from wastewater treatment plants, large factories, and other
facilities that use, process, and discharge water back into lakes, streams, rivers, bays, and oceans.
pH: A measure of the acidity or alkalinity of water. A low pH value (0 to 7) indicates that an
acidic condition is present, while a high pH (7 to 14) indicates a basic or alkaline condition. A
pH of 7 is considered to be neutral. Since the pH scale is logarithmic, a water sample with a pH
of 8 is ten times more basic than one with a pH of 7.
Acronyms and Abbreviations
Ecology Washington State Department of Ecology
EIM Environmental Information Management database
EPA U.S. Environmental Protection Agency
GPS Global Positioning System
MQO Measurement quality objective
NPDES (See Glossary above)
QA Quality assurance
QC Quality control
SOP Standard operating procedure
WDFW Washington Department of Fish and Wildlife
Units of Measurement
mg/L
mL
uS/cm
milligrams per liter (parts per million)
milliliter
microsiemens per centimeter, a unit of conductivity
95
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Appendix 6
Quality Assurance Glossary
Accuracy: The degree to which a measured value agrees with the true value of the measured
property. USEPA recommends that this term not be used, and that the terms precision and bias
be used to convey the information associated with the term accuracy. (USGS, 1998)
Analyte: An element, ion, compound, or chemical moiety (pH, alkalinity) which is to be
determined. The definition can be expanded to include organisms, e.g., fecal coliform,
Klebsiella. (Kammin, 2010)
Bias: The difference between the population mean and the true value. Bias usually describes a
systematic difference reproducible over time, and is characteristic of both the measurement
system, and the analyte(s) being measured. Bias is a commonly used data quality indicator
(DQI). (Kammin, 2010; Ecology, 2004)
Blank: A synthetic sample, free of the analyte(s) of interest. For example, in water analysis,
pure water is used for the blank. In chemical analysis, a blank is used to estimate the analytical
response to all factors other than the analyte in the sample. In general, blanks are used to assess
possible contamination or inadvertent introduction of analyte during various stages of the
sampling and analytical process. (USGS, 1998)
Calibration: The process of establishing the relationship between the response of a
measurement system and the concentration of the parameter being measured. (Ecology, 2004)
Comparability: The degree to which different methods, data sets and/or decisions agree or can
be represented as similar; a data quality indicator. (USEPA, 1997)
Completeness: The amount of valid data obtained from a project compared to the planned
amount. Usually expressed as a percentage. A data quality indicator. (USEPA, 1997)
Data Quality Objectives (DQO): Qualitative and quantitative statements derived from
systematic planning processes that clarify study objectives, define the appropriate type of data,
and specify tolerable levels of potential decision errors that will be used as the basis for
establishing the quality and quantity of data needed to support decisions.
(USEPA, 2006)
Data verification: Examination of a data set for errors or omissions, and assessment of the Data
Quality Indicators related to that data set for compliance with acceptance criteria (MQOs).
Verification is a detailed quality review of a data set. (Ecology, 2004)
Duplicate samples: Two samples taken from and representative of the same population, and
carried through and steps of the sampling and analytical procedures in an identical manner.
Duplicate samples are used to assess variability of all method activities including sampling and
analysis. (USEPA, 1997)
96
-------
Appendix 6
Field blank: A blank used to obtain information on contamination introduced during sample
collection, storage, and transport. (Ecology, 2004)
Matrix spike: A QC sample prepared by adding a known amount of the target analyte(s) to an
aliquot of a sample to check for bias due to interference or matrix effects. (Ecology, 2004)
Measurement Quality Objectives (MQOs): Performance or acceptance criteria for individual
data quality indicators, usually including precision, bias, sensitivity, completeness,
comparability, and representativeness. (USEPA, 2006)
Method: A formalized group of procedures and techniques for performing an activity (e.g.,
sampling, chemical analysis, data analysis), systematically presented in the order in which they
are to be executed. (EPA, 1997)
Parameter: A specified characteristic of a population or sample. Also, an analyte or grouping
of analytes. Benzene and nitrate + nitrite are all "parameters." (Kammin, 2010; Ecology, 2004)
Precision: The extent of random variability among replicate measurements of the same
property; a data quality indicator. (USGS, 1998)
Quality assurance (QA): A set of activities designed to establish and document the reliability
and usability of measurement data. (Kammin, 2010)
Quality Assurance Project Plan (QAPP): A document that describes the objectives of a
project, and the processes and activities necessary to develop data that will support those
objectives. (Kammin, 2010; Ecology, 2004)
Quality control (QC): The routine application of measurement and statistical procedures to
assess the accuracy of measurement data. (Ecology, 2004)
Relative Percent Difference (RPD): RPD is commonly used to evaluate precision. The
following formula is used:
[Abs(a-b)/((a + b)/2)] * 100
where "Abs()" is absolute value and a and b are results for the two replicate samples. RPD can
be used only with 2 values. Percent Relative Standard Deviation is (%RSD) is used if there are
results for more than 2 replicate samples (Ecology, 2004).
Replicate samples: Two or more samples taken from the environment at the same time and
place, using the same protocols. Replicates are used to estimate the random variability of the
material sampled. (USGS, 1998)
Representativeness: The degree to which a sample reflects the population from which it is
taken; a data quality indicator. (USGS, 1998)
Sample (field): A portion of a population (environmental entity) that is measured and assumed
to represent the entire population. (USGS, 1998)
97
-------
Appendix 6
Sensitivity: In general, denotes the rate at which the analytical response (e.g., absorbance,
volume, meter reading) varies with the concentration of the parameter being determined. In a
specialized sense, it has the same meaning as the detection limit. (Ecology, 2004)
Spiked sample: A sample prepared by adding a known mass of target analyte(s) to a specified
amount of matrix sample for which an independent estimate of target analyte(s) concentration is
available. Spiked samples can be used to determine the effect of the matrix on a method's
recovery efficiency. (USEPA, 1997)
Split sample: A discrete sample subdivided into portions, usually duplicates (Kammin, 2010)
Standard Operating Procedure (SOP): A document which describes in detail a reproducible
and repeatable organized activity. (Kammin, 2010)
References for QA Glossary
Ecology, 2004. Guidance for the Preparation of Quality Assurance Project Plans for
Environmental Studies. https://fortress.wa.gov/ecv/publications/SummarvPages/040303Q.html
USEPA, 1997. Glossary of Quality Assurance Terms and Related Acronyms. U.S.
Environmental Protection Agency, http://www.ecv.wa.gov/programs/eap/qualitv.html
USEPA, 2006. Guidance on Systematic Planning Using the Data Quality Objectives Process
EPA QA/G-4. U.S. Environmental Protection Agency.
http ://www. epa. gov/qualitv/q s-docs/ g4-final.pdf
USGS, 1998. Principles and Practices for Quality Assurance and Quality Control. Open-File
Report 98-636. U.S. Geological Survey, http://ma.water.usgs.gov/fhwa/products/ofr98-636.pdf
98
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1 0(2
SPA R10 Lab {MEL) COC (REGION COPY)
DateShipped: 8/18/2018
CarrierName: Hand Delivered
Appendix 7
CHAIN OF CUSTODY RECORD
Formaldehyde NW Aquacuitur«/WA
Project Code: WTR 184A
1 of 1
No; 10-081116-165338-0005
20182017B10P202BD4X24
Contact Name, Jed Januch
Contact Phone. (360) 871 8731
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99
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Page 2 of 2
EPA R10 Lab (MEL) COG {REGION COPY)
DateShipped: 8/18/2016
CarrierName: Hand Delivered
Appendix 7
CHAIN OF CUSTODY RECORD
Formaldehyde NW Aquaculture/WA
Project Code. WTR 184A
1 of t
No: 10-081118-165338-0005
20182017B1OP202BD4X24
Contact Name: Jed Januch
Contact Phorw: (360) 871 8731
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100
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Appendix 7
Page 1 of 2
EPA Hid Lab {MEL) COC (REGION COPY) CHAIN OF CUSTODY RECORD No: 10-070618-150810-0002
07/14/16 Formaldehyde NW Aquaculfure/WA 20162017B10P202BO4X24
Hand Carry WTR-184B Jed Januch
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Page 2 of 2
EPA RIO Lab PEL) COC (REGION COPV)
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Hand Cany
Appendix 7
CHAIN OF CUSTODY RECORD
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1 of 1
No: 10-070618-150810-0002
20162017B10P202BD4X24
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Appendix 7
Page 1 of 2
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§7/12/2016
Formaldehyde NW Aquaculture/WA
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103
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Appendix 7
Page 2 of 2
EPA R10 Lab (MEL) COC (REGION COPY)
CHAIN OF CUSTODY RECORD
No; 10-070616-144407-0001
07/12/2016
Formaldehyde NW Aquacultyre/WA
20162017B10P202BD4X24
UPS
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1 Items/Reason j Relinquished by (Signature and Organization)
I
Dale/Time
Received by (Signature and Organization)
104
-------
Appendix 7
Paget of2
EPA R10 Lab (MEL) COC {REGION COPY)
CHAIN Of CUSTODY RECORD
No: 10-071216-151359-0003
07/19/16
Formaldehyde NW Aquacu*ure/WA
20162017B10P202BO4X24
UPS
WTR-1840
Jed Januch
1ZA4202V1S363S1919
1 of 1
(360) 871-8731
Sample Identifier : CLP Sample '
: ; No.
Matrix/Sampler
Coll.
Method
j Analysis/Turnaround (Pays)
Tag/Preservatlve/Boltles
Location
Coilectton
Date/Time
Sample Type
16294100 ^
Surface Water
Total/ J Jartucb
Composite
; Porm(8 Weeks}
!
N1 (None) (1)
0NFH1 influent
07/18/2016 14:04
Field Sample
16294101 ;
*
Surface Water
Total/ J Januch
Discrete
Interval
, Forntp Weeks)
N1 (None) (1)
0NFH2effluent
§
JO
1
Field Sample
16294102
Surface Water
Total/ J Januch
Discrete
Interval
form(8 Weeks)
N1 (None) (1)
DNFHZefflusnt
07/18/201811:13
Field Sample
16294103 .
Surface Water
Total/ J Januch
Discrete
Interval
Form(a Weeks)
N1 (None) 0)
DNPHZaffloent
07/18/2016 11:23
Field Sample
16294104
Surface Water
ToiaV J Januch
Discrete
Interval
Form(8 Weeks)
N1 {None) (1)
DNFH2effluent
07/18/201611:33
Field Sample
16294105 :
Surface Water
Total/ J Januch
Discrete
Interval
Form(8 Weeks)
N1 {Now) (1)
DNFH2eHtuent
07/18/2018 11:43
Field Sample
18294106
Surface Water
ToiaV J Januch
Discrete
Interval
; Form (8 Weeks}
Wl HI N3(Nona)CT
DNFHZeffluent
07/18/201811:53
Field Sample
16294107
•
Surface Water
Total/ J Januch
Discrete
Interval
; Form(8 Weeks)
:
N1 (None) (1)
DNFHZBffloent
07/18/2016 12:03
Field Sample
16294108
:
Surface Water
Total/ J Januch
Discrete
Interval
; Form(8 Weeks)
Nt (None) (1)
DNFH2efftuem
07/18/2016 12:13
Field Sample
16294109
Surface Water
Total/J Januch
Discrete
Interval
Form(S Weeks)
:
N1 (None) (1)
DNFH2efftuerrt
07/18/2018 12:23
Field Sample
16294110
Surface Water
Total/ J Januch
Discrete
Interval
= Form(8 Weeks)
t
N1 (None) (t)
DNFH2effluent
07/18/2016 12:33
Field Sample
' : Shipment for Ca#« Complete? M
; Sample{s> to be used for Lab OC: 18294108 Tag N3 Samples Transferred From Chain of Custody?
! Analysis Key: Fonn^ornialdehyde
Items/Reason Relinquished by (Signature and Organization)
Received by (Signature and Organization)
Sample Condition Upon Receipt
105
-------
Appendix 7
Page 3 of 2
EPA mo Lab (MEL) COC (REGION COPY)
CHAP OF CUSTODY RECORD
No; 10-071216-151959-0003
07/19/16
Form aldehyde NW Aquacufture/WA
20162017B10P202BD4X24
UPS
WTR-184D
Jed Januch
1ZA4202V1596381919
1 of 1
(360) 871-8731
: Sample Identifier
:
CLP Sample
No.
Matrix/Sampler
Coil.
Method
I Anatysis/Tumarou nd {Days) .
Ta§/PreservatIvelBotltes
I Location
Collection
Date/Time
Sample Type
18294111
Surface Water
Tola!/ J Jartucb
Discrete
Interval
, Form(B Weeks)
N1 (None) (1)
. DNFH2e«luent
i
07/18/2016 12:43
field Sample
i 16294112
Surface Water
Total/ J Januch
Discrete
Interval
Form(8 Weeks)
:
N1 (None) (1)
: DNFH2effloent
>
07/18/2018 12:53
Field Sample
, 16294113
Surface Water
Total/ J Januch
Discrete
Interval
Form(8 Weeks) :•
•
N1 (None) (1)
: DNFH2effluent
07/18/2018 13:03
Field Sample
; 16294114
Surface Water
Total/ J Januch
Composite
: Form(8 Weeks) ;
i
Ni (None) (1)
; DNFH3rw
07/18/2018 14:30
Field Sample
' 18294115
;
Surface Water
Total/ J Januch
Grab
j Form{8 Weeks)
N1 (None) (1)
DNFH2silusnt
07/18/2016 13:30
Field Sample
! 16294116
Water/ J Januch
Grab
; Form(8 Weeks)
N1 (None) (1)
Blank
07/18/2016 11:17
OC Blank -
Hinsate/Ecjuipm
ent
Special Instructions:
Shipment lor Case Complete? i
Samples Transferred From Chain of Custody #
Analysis Kef,' Form-Formaldehyde
i Items/Reason : Ttetinquished by {Signature and Organization)
Date/Time
Received toy {Signature and Organization)
Date/Time : Sample Condition Upon Receipt
in a Ml
ICCD
106
-------
Appendix 7
EPA RIO Lab (MEL} COC (REGION COPY)
01/21/16
. .red
CHAIN OF CUSTODY RECORD
Formaldehyde NW Aquaculturo/WA
WTR-WE
c-t »
No: 10-071516-164155-0004
.¦*011201 ?B ICP202BD4X24
J ad JanucEs
(360) 3~1-P7j1
S: ilifier
CLP Sample i Matrix/Sampler
i No- i
Coll.
Method
Analysis/Turnaround (Days)
TagfPre*ervativC.'Botttos
; Location
;
Collection .
Date/Time ;
Sample Type
16294120
! ; Surface Water
; Total/J Januch
Composite
FormfS Weeks)
N1 {None} (1J
• QWFHt influent
07/20/2016 1t ;35
Field Sample
16234121
j Surface Water
: Total/J Januch
Discrete
Ip.jefvat
FormfB Weeks)
Ml {None) {1}
« CSWFH2efflucsnt
87/20/2016 03:20
Field Sampfo
162941??
. : Surface Water
' I Total/ J Januch
Discrete
Interval
Form(8 Weeks)
Ni (Nonel (i)
: CIWFHSolflucnt
07/20/2016 09.30
Field Sample
16294123
: Surface Water
! Total/ J Januch
Discrete
Interval
Form{8 Weeks)
Nt (None) (1)
; CIWPH2off!uonf
07/20/2018 09 40
Field Sample
16234124
' Surface Water
; Total/ ,1 Januch
Discrete
Interval
Porm(8 Weeks)
Ml {None} (1)
CIWFHZetlluont
¦
07/20/2016 03:50
Field Sample
16294125
: Surface Water
i Total' J Januch
Discrete
Interval
FermfS Weeks}
NI (Mono) (t)
: CiWFH2ei«iient
07/20/2016 10:08
Field Sample
16234126
! Surface Water
: Total/ J Januch
Discrete
Interval
Form(8 Wools}
: Nl(Nono)(i)
; CiWFHZoffiueni
07/20/2016 10 10
Field Sample
16294127
: = Surface Water
¦ Total/ J Januch
Discrete
Interval
Petnn(8 Weeks!
I Ni (None) (1)
: CIWFH2effluent
07/20/2016 10 20
Field Sample
16294128
: ' Surface Water
Total/ J Januch
Discrote
Interval
Fertn(8 Weeks)
; Ni (Nono) (1)
: CiWFHZeffluertt
:
. 07/20/2016 10:30
Field Sample
16294129
Surface Water
Total/ J Januch
Discrete
Interval
FormfB Weeks)
Nl |None) (1)
; CiWFHSoffluont
j 07/20/2016 10 40
Field Sample
16234130
: : Surface Water
: • Total' J Januch
Discrete
interval
f c»m{8 Weeks}
: Ni (Nor>o) (t)
: CiWfHMfiuent
:
; 07/20/2016 10:50
Field Sample
; Special Instructions.
: Shipment for Case Complete? N
; Samples Transferred From Chain of Custody#
i Analysis Key. Farm-Formatdohyde
Items/Reason Relinquished by (Signature and Organization) f Date/time
\jcmA..
Received by (Signature and Organization)
Date/T?me ; Sample ConcJition Upon Receipt
•f-frrd
107
-------
Appendix 7
EPA RiU Lab {MEL) COC (REGION COPY)
c: :i.
Hand Dc'i.verect
Sample Identifier
CLP Sample ¦ Matrix/Sampler
No. :
Coll.
Method
16294131
16294132
18294133
Surface Water : Discrete
Total/ J Jsnvch Interval
Surface Water ; Discrete
Totsl/J Janoch ; interval
Grab
16294134
16294135
18294138
TDial/J Jani/ch
^ Water/J Januch
Grab
Surface Water
Iota;' J Januch
Discrete
Interval
! Sampte(s) lo be used for lab QC 16294134 Tag N3
' Analysis Key Form * Formaldehyde
CHAIN OF CUSTODY H6CORD
- rm -Idi- ^yd- NW Aquacutswo/WA
W-H-1S4E
* of t
No; 10-07151S-164155-0004
2016201?B10P202BD4X:'4
Jed Januch
{360} 871-8731
• Anaty»i*.Turnarour*cl (Days) _ T»gfPrcicrvative/Botttes
Surtace Water
Total/ J Januch
Surface Water ; Compotie
Form(8 Weeks}
Form(8 Weeks)
Fom*(« Weeks}
N" {Mono) (1)
"Nf(Noncj"(t}"
' N1 fNonil'|i")"
Fcrta(8 Weeks)
Fcrm(8 Weeks)
Form(B Weeks)
N3 (None) (3)
-Nja ,w.l
NT fNonoJ (1|
N1 (Mono) (1)
Location
Collection
Date/Time
Sample Type
C!WfB2eff«nt i 07/20/2018 11-00 > Field Sample
! CIWFB&fBuom j 07/20/2018 11:10 ; Field Sample
! CIWFHSiluirft*'' f 07/20/20l'il 0:36 T Field Sample
J : . I
» ClWffiiw i 6»20K0l6'l2:4? j" field Sample'
! Blank
, 07/20/2016 07.4? ; GC Blank -
¦ , Rinsate/Equipm
era
"oWFi^Hiucnt' ] ~0^0/26T6 Tolio r 'Ftold'Du^TMlo "
: Shipment for Case Complete? N
; Samples Transferred From Chain of Custody #
;• items/Reason I Relinquished by (Signature and Organization) ! "Dae/time
Received by (Signature and Organization)
Sample Condition Upon Receipt
A— J 5.
108
-------
Appendix 8
Page 1 of 2
EPA R10 Lab PEL) COC {REGION COPY}
CHAIN OF CUSTODY RECORD
No: 10-090816-164101-0006
DafeShipped 9/12/2016
Formaldehyde NW Aquaculture/WA
20162017B10P202BD4X24
CarrierName Hand Delivered
Project Code: WTR-184F
Contact Name: Stana Wong
1 ef1
Contact Phone- (360) 407-6432
Sample Identifier
CLP Sample
No.
Matrix/Samplor
Coll.
Mot hod
; Analysis/Turnaround (Days)'
1
Ta§IPresorvativeBottles
: Location
!
i Collection
i Date/Time
Sample Type ;
18375100
<
;
Surface Water
Total? S Wong
Composite
: Fofm(fl Weeks) >
¦
¦
N1 (None) (1)
; KFH_influent
! 09/12/2016 14 38
l
Field Sample :
18375101
,
.
Surface Water
Total/S Wong
Grab
¦ Form(B Weeks) ;
N1 (Norse), N2 pone), N3
{None) {3}
: KFH_E (fluent
:
: 09/12/2016 11 06
Field Sample
16375102
'
:
Surface Water
Total/ S Wong
Grab
1 Form(8 Weeks)
; ;
N1 (None) (i)
: KFH Effluent
:
. 09/12/2018 11 26
i
Field Sample ;
16375103
'
¦
Surface Water
Total/ S.Wong
Grab
: Form(B Weeks) :
: :
N1 (None) (1)
1 KFH_Effluent
j 09/12/2018 11:46
Field Sample :
;
16375104
Surface Water
Total/ S Wong
Grab
i Pormf'B Weeks) ¦
; :.
N1 (None) (1)
: KFH Effluent
:
! 09/12/201612-06
Field Sample !
:
16375105
;
Surface Water
Total/ S.Wong
Grab
: Form(8 Weeks} ,
N1 (None) (1J
; KFH Effluent
.: 09/12/201612-28
:
Field Sample •
18375106
.
>
Surface Water
Total/ S.Wong
Grab
Form{8 Weeks) :
>
N1 (None) (1)
, KFH,, Effluent
- 09/12/201812-48
!
Field Sample ;
16375107
;
Surface Water
Total/S.Wong
Grab
: Form {8 Weeks) :
•
N1 (None) (1)
: KFH Effluent
;
i 09/12/2016 13 06
!
Field Sample :
16373108
i
;
Surface Water
Totall S Wong
Grab
• Forrnffl Weeks) ;
:
N1 (None) (1)
; KFHJHIuent
: 09/12/2016 13:26
Field Samp% •
16375109
:
; ;
Surface Water
Totall S Wong
Grab
: Form(8 Weeks) ;
= ;
N1 (None) (1)
s KFH Effluent
; 03/12/2016 13:48
Field Sample j
:
16375110
i
:
Surface Water
Total/ S.Wong
Grab
: F ormfS Weeks) !
*
:
N1 (None) (1)
: KFH_B«!ueot
. 09/12/2016 14:08
field Sample !
: . Shipment for Caso Complete? Y
Samplefs) to be used for lab QC: 16375101 Tag N1,16375101 Tag HZ, 16375101 Tag N3 ¦ Special Instructions. Samples collected by •«;- _- r—r; —— -
' Ecology and delivered by EPA/Januch, Questions regarding Scribe lie - contact Jed Januch ' jampos Transforred from Chain of Custody #
: Analysis Key; Form«Formaldehyde
hems/Reason < Relinquished by (Signature and Organization) ; Date/Timo
Received by (Signature and Organization)
Dale/Time ' Sample Condition Upon Receipt
109
-------
Appendix 8
Page 2 of Z
EPA R10 Lab {MEL) COC {REGION COPY) CHAIN OF CUSTODY RECORD No: 10-090816-164101-0006
nat»nf>rt Q?i?/?niR Formaldehyde WW AquacuttureWVA 20162017B10F202BD4X24
ZTL„ ^ Code WTR 164F
1 0f i Contact Phone: (380) 407-8432
! Sample identifier j
CLP Sample
No,
Matrix/Sampler
Coll.
Method
Annlysis/Tunwound {Days)j
TaglPrasBrvalivelBolllcs
Location
Collection
Data/Time
Sampto Typo
: 18375111 !
i
Surface Wafer
Total! S.Wong
Grab
Form{8 Weeks) >
!
N1 (None) (1)
KFH . Effluent
09/12/2016 14 26
Field Sample
. 18375112 .
Surface Water
Total# S.Wong
Grab
Form(8 Weeks) :
N1 (None) (1)
KFH,Effluent
09/12/2016 14.46
Field Sample
: 16375113 i
!
Surface Water
Total/ S.Wong
Grab
Forrn(8 Weeks) j
N1 (None) (1)
KFH_Effluent
09/12/2016 13 07
Field Sample
: 16375114
Surface Water
Total! S.Wong
Composite
Form(8 Weeks) i
N1 (None) (1)
KFH rw
-
09/12/2018 14 57
Field Sample
: 16375115
:
Wafer/ S.Wong
Grab
formfS Weeks)
N1 pone) (1)
Blank
09112/2016 09'52
QC Blank -
Rtnsale/Equtprn
ent
I 16375118
i Surface Water
' Total? S.Wong
; Grab
; Form(8 Weeks) ;
N1 (None) (1)
KFH,Effluent
01/12/201812:46
Field Duplicate
:
:
:.
—— — — - — ¦— - «—-« — ——- — — — ¦ ^ Shipment for Case Complete? Y
Special Instructions: SampSes collected by Ecology and delivered by EPA/Januch. Queshoras regarding Scribe lie - contact Jwf Januch. ! Samples Transferred From Chain of Custody I
; Analysis Key. Form=Formaldehyde
"itenriS^eason - 'Relinquished by (Signature and Organization)
Date/T«me
Received by {Signature and Organization}
J&o- u ood
Date/Time ! Sample Condition Upon Receipt S
i
110
-------
Page 1 of 2
EPA R10 Lab (MEL) COC (REGION COPY)
DateShipped 9119/2016
CarriwName FedEx
AlfblllNo,
Appendix 8
CHAIN OF CUSTODY RECORD
Formaldehyde NW Aquaculture/WA
Project Code WTR-184G
1 of 1
No; 10-091516-140459-0007
20162017810P202BD4X24
Contact Name. Siara Wong
Contact Phone (350) 407-6432
Sample identifier ' CLPSampta
l No.
16385200
~16385201"
-E
18385203
1638520-4
18385205
¦TOanzmr
16385207
18385208
18315209
18385210"" *
NtatrlxISampler j Coll, I An»lyil*rrurn* round (Days)
| Method [
Surface Water f Composite
Total! S Wong !
Form(8 Weeks)
Surface Water
Total/ S.Wong
Grab
Surface Water
Total! S Wong
Surface Water
Total/ S.Wong
Grab
Grab
Surface Water > Grab
Total/ S Wong :
Surface Water
Total/S,Won§
-Snrfacrwawr*
TolaH S.Wong
« Surface Water
i Total/ S.Wong
Surface Water
Total/ S.Wong
, Surface Water
Total/ S.Wong
Grab
Surface Water
Total! S Wong
-Gritr
Grab
Grab
Grab
Grab
Pefffl(8 Weeks)
Form(8 Weeks)
Form (8 Weeks)
Form(8 Weeks)
Form{8 Weeks)
-ftjrmffl-wwtsr
Porm{8 Weeks'#
Form(6 Weeks)
Form(8 Weeks)
Form(B Weeks!
T»g/P r» *e rvetl ve/B ottte t
Location
N1 (None) (1)
N1 (Norte), N2 (None), N3
(None) (3)
N1 (None) (1)
N1 (None) (1)
Nt {None) (1)
N1 (None) (1)
¦ _ .-ffwpr
N1 (None) (1}
N1 (None) (II
N1 (None) (1)
N1 (Nona) {11
WRFH influent
WRFH Effluent
Collection
DatofTIma
WRFH_Eflfuenl
WRFH_Effluent
WRFH_Effluent
WRFH_E fluent
¦WWCBHtamr
WRFM,_E«uerit
WRFH Effluent
WRFH_Efftuent
09/19/2016
:fe;M
09/19/2016
oJiMili
09/19/2016
MJS
Q9rt9ao«^,
mnWsr
-wwrarw-
M1
09/19/2016 .
" 09/19/2016 ~~
S3h.
09/18/2016
mx
Sample Type 1
FteW Sample j
i
' Field Sample )
Field Sample
Field Sample
Field Sample
Field Sample
_ Field Sample
Field Sample
Reld Sample
field Sample
I ' " I Shipment for Ca>« Complete? Y
' Sample(s) to be used for Lab QC: 163B5201 Tag N1,18385201 Tag Nt, 16385201 Tag N3 - Special Instructions: Samples collected [" 5"_ir'¥ra,i.farr«rf From Chain el Citttodv #
; and shipped by Ecology. RSCC needs ecology sample limes and associated collection into emailed on day of shipment. |
Analysis Key. Form*Farmaid6hyde
Sample Condition Upart Receipt
07: IS J X
k _ lAiktl. 1
Dale/Time
(Signature and Organization)
Date/Time
Items/Reason
Relinquished by {Signature and Organization)
i . A
111
-------
Appendix 8
Page 2 of 2
EPA R10 Lab (MEL) COC (REGION COPY}
Date Shipped 9/19/2016
CarrierName; FedEx
AirbHtNo: :
CHAIN Of CUSTODY RECORD
Formaldehyde NW Aquaculture/WA
Project Code WTR-184G
1 of 1
No; 10-091518-140459-000?
20182017B10P202BD4X24
Contact Name: Slana Wong
Contact Phone: (360) 407-8432
Simple Identifier CLP Sample I Matrix/Sampler 1 Coil, TAnaiysislTumaround (Days) | fag/Preserva'tiWBQtties
; No. > ! Method
Surface Water :
1638521
1638521
1638521
16385214
Tola!/ S.Wong
Grab
FormCS Weeks)
N1 (None) (1)
Surface Water
Total/ S.Wong
Grab
Surface Water
Total/ S.Wong
: Surface Water
• Total/ S.Wong
16385215
18385216
16335217
Waler/ S.Wong
Surface Water
Total/ S.Wong
Surface Water
Total/ S.Wong
16385218
18385213
I"
Surface Water
Total! S.Wong
Grab
FormfB Weeks)
N1 pone) (1)
Location
WRFH Effluent
WRFH Effluent
Composite
Grab
Form{8 Weeks}
Form{8 Weeks)
Form (I WeeFsl
N1 (None) (1)
WRFH Effluent
N1 (None) (1)
WRFH rw
N1 (None) (1)
Blank
Grab
Grab
Grab
Forra(S Weeks)
Formp Weeks}"
FormlS Weeks]
N1 (None) (1)
Collection
Date/Time
OS ¦' 19/2016
lt*ST
09/19/2016
J
oirtKOie
09/13/2016 _
|^b
09/19 ^l 6
W'ir
WRFH Effluent
Sample Type !
Field Samp*e
Field Sample •
rield Sample ;
Field Sample 1
QC Blank -
Rinsate/Equipm ,
ant I
Field Duplicate
N1 (None) (1)
WRFH_EggTreat
mentEflluent
0S/19/2016
iV-'S-s
09/19/2015 F«W Duplicate
N1 (None) (1)
Surface Water
Tola!/ S Wong
Grab
Form(8 Weeks)
N1 (None) (1)
WRFH_EggTreat
mentEflluent
WRPH_EgsTreat
mentEflluent
uw/19/2016
1^13- i
09/19/2018 !
J
Field Duplicate
Field Duplicate
Special Instructions1. Samples collected and shipped by Ecology, RSCC needs ecology sample limes and associated collection info
emailed on day of shipment
' Shipment for Cat* Complete? Y
, Samples Transferred From Chain of Custody #
Analysis Key form=Formaidshyde
Items/Reason Relinquished by {Signature and Organization)
Date/Time
Received Dy (Signature and Organization)
Date/Time
cn-15
Sample Condition Upon Receipt '
~oT CwwwVWrs;"*
%oW _
112
-------
Appendix 8
Page 1 of 2
EPA RIO Lab (MEL) COC (REGION COPY)
DaieShipped 9/30/2016
Carrier Nam® FedEx
AirbiliMo: .
CHAW OF CUSTODY RECORD
Formaldehyde NW Aquaojlture/WA
Project Code WTR-184H
1 of 1
No; 10-032818-174017-0008
201S2017B10P2Q2BD4X24
Contact Name Siana Wong
Contact Phone (380) 407-6432
Sample Identifier j CLP Sample
I No,
15395271
163952J
16395251
16395253
16395254
Matrix/Sampler
Surface Water
Total/ S.Wong
Surface Water
Total/ S Wong
Coil
Method
G*ab
Analysis/Turnaround (Days) Tag/Preservative/Bottles
Location
Composite
Surface Water
Total/S Woog
Surface Wafer
Total/ S.Wong
Surface Water
Total/ S.Wong
Discrete
Interval
Form{8 Weeks)
Ml {None) (1J
C5FH_Effloent
Collection
Date/Time
Sample Type
field Samp'e 1
N1 (None) (1}
Discrete
Interval
16396255
18395256
16395257
Surface Water
Total/ 5 Wong
Discrete
Interval
Discrete
Interval
N11None), H2 (None), N3
(None) (3)
N1 fNonsl (1)
N1 (None) (1)
N1 (None) (1)
03/30/2016 14.48
CSFH^.nfioent ' 09/30/2016 15 &? Field Samp'e
CSf Effluent 03/30/201610.00 . Field Sample
CPFH "Effluent 09/30/2016 10 3C ( " Field Sample
'mmmmnm j FSfisam^e"
09/30/2016 11:30 Field Sample
16395258
18395259
Surface Water
Total/ S Wong
Surface Water
Total/ S Wong
Discrete
Interval
Discrete
interval
Form(8 Weeks}
N1 (None) (1)
' N1 (None) (1)
Surface Water
Total/ S Wong
Surface Water
Total/S.Wong
Discrete
Interval
FormfS Week*)
Discrete
Interval
Form(8 Weeks)
N1 (None) (11
Nl"{None)(ir
09/30/2016 12 00 Field Sample
CSFH_ Effluent 1 09/30/201512:30 j Field Sample
C8FH_E!uen» ! 09/30/2016 13 00 I Field Sample
CSFH_Etfloent 08/30/2018 13:30 Field Sample
16385260
Surface Water Discrete
Total/S.Wong : Interval
Form(8 Weeks)
Ni (None) (1)
CSFHJffluertt 08/30/2016 14 00 I Field Sample.
r
: Sample!s) to be used for Lab QC 16395271 Tag N1.16395261 Tag N1,16395251 Tag N2,16395251 Tag N3 - Special instructions.
! Samples collected and shipped by Ecology RSCC need* ecology sample times and associated collection info emailed on day of
i shipment.
Shipment for Case Complete? Y
i Samples Transferred From Chain of Custody *
' Analysis Key Form*Fomialdehyde
Items/Reason
Relinquished by (Signature and Organization)
Date/Time
Received by (Signature and Organization)
Dale/Time Sample Condition Upon Rece-pt
?'2D , !»/$./]b
113
-------
Appendix 8
Page 2 of 2
EPA R10 Lab (MEL) COC (REGION COPY}
DateShipped: 9/3012016
CarrierMame- FedEx
AirMINo:
CHAIN Of CUSTODY RECORD
Formaldehyde NW AquacuiturelWA
Project Code. WTR-184H
1 of 1
No; 10-092816-174017-0008
20162017810P202BD4X24
Contact Name SiartaWong
Contact Phone: (360) 407-6432
Sample Identifier
18395261
16395262
11315263""
CLP Sample Matrix/Sampler
No.
Surface Water
Total/ S Wong
Coil.
Method
Surface Water
Total/ S Wong
Surface Water
Total/ S.Wong
16335264
Surface Water
Total/ S Wong
Discrete
Interval
Discrete
Interval
Discrete
Interval
Artafysis/Turnaround (Days) |
Form(8 Weeks)
TagfPreservative/Bottles
Location : Collection
Dale/Time
CSFH Effluent : OSOWOTsli 30
Form(i Weeks)
N1 {None) (1)
Form(8 Weeks;
N1 (None) (1)
Discrete
Interval
Forro(8 Weeks)
Ml (None) (1)
CSFH Effluent
CSFH Effluent
C5FH_Effluent
09/30/2016 15 00
Sample Type
field Sample .
Field Sample
09/30/2016 15 30 ' Field Sample
09/30/2016 18 00 : Field Sample
16335265
16395266~
Surface Water
Total/ S.Wong
Composite
Form(8 Weeks)
j Water/ S.Wong
Grab
16395267
Surface Water Discrete
Total# S.Wong r Interval
Fofm{8 Weeks)
FormfB Weeks)
N1 (None) (1)
N1 (None) (1)
CSFH_rw 09/30/2016 16'40 i Field Sample
N1 {None) |1}
S Blank
'T'cSFH^EffltSenT
! QC Blank -
S RifisatBlEquipm
* mi
09/30/2016 14 00 | Field Duplicate
Special Instructions Samples ca lected and sh poed by Eco'ogy RSCC needs ecology sample times and associated collection info
emailed on day of shipment
Shipment for Case Complete? Y
i Samples Transferred From Chain of Custody #
! Analysis Key Fcxm-Formaidehyde
Items/Reason j Relinquished by (Signature and Organization) " Date/Time
Received by (Signature and Organization)
Dale/7 me 1 Sample Condition Upon Receipt
H" ... ... .. . ... ...¦ .... -
ll ">1X271
oc,
N
1
_ y
\
1 !
j
1
114
-------
Appendix 8
Pafle 1 of 2
SPA R1Q Ub (MEL) COC {REGION COPY}
DateShippeti: 11/7/2018
CtrterNams: Hand Dslivered
AlrbHIMo
CHAIN Of CUSTODY RECORD
Formaldehyde NW Aquactilture/WA
Project Coda- WTR-1841
1 of 1
No: 10-110216-135814-0009
20182017B10P202BD4X24
Contact Name' Slana Wong
Contact Phone: (360j 407-8432
Sample Identifier
CLP Sampl* j MatrixfSampler
No, !
Coll,
Method
Analystcff umareund pays) j"™-fagfPreservaUve/Bottles
Location | Collection
Date/Time
Sample Type
16444000
Surface Wafer
Total/ S.Wong
Surface Water
Total/ S Wong
Composite
Form(8 Weeks) | N1 (None) (1)
PRFHJnfluent f 11/04/2018
1 IHoo
PieW Sample
J 16444001 |
Discrete
Interval
Form(6 Weeks) i NT(None), N2 (None), N3 •
J (None) (3)
PRFH Effluent t i 1/04/201 i
1 O'W 0
..pie
18444002
Surface Water
Total/ S Wong
Discrete
Interval
Form(B Weeks) "1 N1(None)(1)
PRFHJEffktent 11/04/2018
I |OOo
field Sample
16444003
Surface Water
Total/ S.Wong
Discrete
interval
Form(8 Weeks) 1 N1 (None) (1)
I
PRFH_Efjjuent j 11/04/2016
• \oU>
Field Sample
16444004 i Surface Water
j [ j Total/ S.Wong
Discrete
Interval
Form(8 Weeks} T N1 (None) (1)
_ _ _
PSr-i Effluent j 1 t<04/2C''6
I -ofo
Field Sample
18444005
I Surface Water
| Total/ S.Wong
Discrete
Interval
Fott){8 Weeks)
N1 {None) (1)
PRFH_Effluent
11/04/2016
Moo
Field Simple
16444008
Surface Water
Total/S.Wong
Discrete
Interval
Form(B Weeks)
N1 (None) (1)
PRFH_Ef8uent
11/04/2018 1 Field Sample
••10
1644400?
Surface Water
Total/ S.Wong
Discrete
Interval
f orm(8 Weeks)
N1 (None) (1)
PRFHJEffluerH
11/04/2018
sHo
Field Sample
18444008
Surface Water
Total/ S.Wong
Dlscrett | Form(B Weeks)
Interval (
N1 (None) (1)
PRFH_Efftuent
11/04/2015
UbO
Field Sample
18444009
Surface Water Discrete i FormfB Weeks)
Total# S.Wong J Interval j
N1 {None} (1) ,
FRFH_Efltient
11/04/21 pie
12:
| 18444010
I
Surtece Water ' Discrete ' Form(8 Weeks)
Total/ S.Wong [ Interval
N1 (None) (1)
PRFH_Effluerfl
11/04/2016 I Field Sample
f;^d
Samplefs) to be used for Lab QC: 16444001 Tag N1,16444001 Tag N2,16444001 Tag N3 - Special Instructions: Samples collected
and shipped by Ecology. RSCC needs ecology sample times anrt associated collection Info emaited on day of shipment
Shipment for Cast Complete? Y
Samples Transferred From Chatn of Custody *
Analysis Key: Form*Formatotby
V
-------
Appendix 8
Page 2 of 2
eJ»A R10 Ub (MEL) COC (REGION COPY)
DaleShlpped 11/7/2016
CarrterName Hand Delivered
AMINO
CHAIN Of CUSTODY RECORD
Formaldehyde NW Aquaeulture/WA.
Project Code: WTR-184!
1 of 1
No: 10-110216-135814-0009
201S2017B1QP202BD4X24
Contact Name; Sfana Wong
Contact Phone <360) 407-6432
Sample Identifier
CLP Sample
No,
Matrix/Sampler
Coll.
Mtthorf
Analysis/Turnaround {Day#)
Tag/Preaervatlvw/Bottl
Location
Collection
Date/Time
Sample Type
16444011
Surface Water
Total/ S.Wong
Discrete
IntervsH
Form{8 Weeks}
N1 (None) (1)
PRFH_Effluent 11/04/2016
I ilao
Field Sample
18444012
Surface Water
Total/ S.Wcmg
Discrete
Interval
FormfB Weeks)
N1 (None) (1) j PRFH_EHIuent
11/04/2018
Field Sample
18444013
Surface Water
Total/ S.Wong
Discrete j Fofm(8 Weeks)
Interval ]
N1 (None) (1) . PP-H_l^yent
11/04*2018
13M0
field Sample
j 16444014
Surface Water
Total/ S.Wong
~~Compoilejj Forrn(8 Weeks)
' N1 (None) {1) J PRFH_rw
11104/2016
Hod
Field Sample
18444015
| Water! S.Wong
i
Grab
Form(B Weeks)
N1 (None) (1)
Blank
11104/2016
t) fh *
Rift! m
16444016
. Surface Water
I lotal/SWong
Discrete
Interval
Fotm(8 Weeks)
N1 (None) (1)
PRFH_Etttoml
11/04/2016
Fie !e
18444017
I Surface Water
! Total/ S Wong
Grab | Form(8 Weeks)
N1 (None) (1)
PRFH_Effluent
5
Field Sample
i mhwr
.>«,N,UAk/
„ ACL r-U—
—1^13 -j rorvf f Ste/
1 K/v y*
i
———f-
1
J
i
j
I
1
i
"" ~ 1
i i
Special Instructions" Samples collected and shipped by Ecology. RSCC needs ecology sample times and associated collision into
emailed on day of shipment.
"sSpmeht for Case Compete? Y ]
Samples Transferred From Chain of Custody # 1
Analysts Key; Form*Fomi»W»hytJ« 1
Items/Reason
ReSnq wished by (Signature and Organization)
Date/Time
Received by (Signature and Organization)
Date/Time
Sample Condition Upon Receipt-]
(f/v/)<- ft ^ c4^i/rv\ i-1
lu;ir2
- - - - - /—
lihLi if
i t |
( _m
1
116
-------
WW \d{l uc,qn~ i m*«>&<> io is/ rt
Page 1 of 2
EPA R10 Lab PEL) COC (REGION COPY)
DateShipped: 12/1/2016
CamerName: Hand Delivered
AirbllINo: NA
CHAIN Of CUSTODY RECORD
Formaldehyde NVtfAquacuiture/WA
Project Code: WTR-1841
1 of 1
No: 10-112916-133120-0010
2017201 SB 10P2O2BD4X24
Contact Name: Stana Wong
Contact Phone: (380) 407-6432
Sample Identifier
CLP Simple
No.
Matrix/Sampler
Coll.
Method
Anatysis/Tunwound (Days)
Tao/P reaenrative/Bottlea
Location
Collection I
Data/Time
Sample Type
16484000 '
Surface Water
Total/S.Wong •
Composite
Fonn(8 Weeks)
N1 (None) (t)
PRFHJnluent
11/3012018
'f/r
Field Sample
16484001
Surface Water
Total/ S.Wong >
Discrete
Interval
Form{8 Weeks)
N1 (None), N2 (None), N3
(None) {3)
PRFH Effluent
11/30/2016
,! JO
Field Sample
15484002
Surface Water
Total/ S.W
Discrete
Interval
FormfB Weeks)
N1 (None) (1)
PRFH_Effluent
11130/2018
H'fO
Field Sample
16484003
Surface Water
Total/ S.Wong
Discrete
Interval
Form(8 Weeks)
N1 (None) (1)
PRFH.EBuent
11/30/2016
II./t?
field Sample
16484004
Sorts
Total/ S.Wong
Discrete
Interval
FormfB Weeks)
N1 (None) (1)
PRFH_E(fluent
11/30/2016
(i o
Field Sample
16484005
Surface W
Total/ S.Wong
Discrete
Interval
Form(8 Weeks)
N1 (None) O)
. PRFH_Effluent
i.
11/30/2016
lx: So
Field Sample
| 16484006
I
Surface Water
Total/ S.Wong
Discrete
Interval
Formffl Weeks)
N1 {None) (1)
PRFH_Effl«ent
11130/2018
V)°
Field Sample
t 16484007
i
!
I
Surface Water
Total/ S.Wong
Discrete
Interval
FormfB Weeks)
N1 (None) (1)
PRFH.Effloent
11/30/2018
O •'}°
Field Sample
P~ll4M008
1
Surface Water
Total/ S.Wong
Discrete
Interval
Fonm{8 Weeks)
N1 (None) (1)
PRFH_EtHuent
11/3012016
Field Sample
! 16484008
|
Surface Water
Total! S.Woog
Discrete
Interval
Form(8 Weeks)
Nt (None) (1)
1 PRFH Effluent
11/30/2016
ii-io
Field Sample
| 16484010
1
Surface Water
Total/ S.Wong
Discrete
Interval
Form<8 Weeks)
I - , _ _ _ •
N1 (None) (1)
PRFH_Effluent
11/30/2016
t . W
SeW Sample
i
D
: Samp»e{5) Id be used for Lab QC 18484001 Tag N1,16484001 Tag N2,1S484001 Tag N3 - Special Instructions: Samples collected
; and sapped by Ecology EGGS ONLY. RSCC needs ecology sample times and associated collection Info emailed on day of shipment
Shipment for Case Complete? Y
Samptes Transferred From Chain of Custody #
I
Analysis Key Form=Forfnaldehyde
Items/Reason
Relinquished by (Signature and Organization)
o.. /(0
sd by (Signature and Organization)
II 50 I t !2d:o Q ivulvj' &|V 0£
W"'J _ f^v-r
Date/Time
\\-roii:ic;io
Sample Condition Upon Receipt
I2- Qt/%
Or. ¦*>' s
* C^fdv: "tV<~ i»t#c f
9
\l. m
Of.#
/* I (
'-:*D
117
-------
Appendix 8
»it ivfi, coc cap«)
Date5hlppcd: 12/1/2016
CafrierNwne: Hand OsKvered
AlrttINo: NA
ci-a n or ey.sic.vv mcc^m
fit trai h-typc >M niU.nWA
Project Code: WTR-1U4I
s OJ i
ipl# IdentifierCLP SampHt j Matrix/Sampler
Ceil,
Method
U'lRlOl* J c, rfar8lV,r)"
Location
f«5.ent
fiViS
PRFH rw
No: l0-11£Si5-!J31Sp.0fti»1
A't IPWWC4
Contact Name Slana Wong
Corrtvt ^farc E») 40? 8 ij£
Bate/Tin*
flUQCOW
ii y&
11/30/2016 I Field Sample
I :: . :
11d »»f W j r rlc! Fanm#
h' - j Q [ :
1113012818 I^HSdSaBipe-
I
11/30/2016 QC Blank- j
_ Rhsals/E^ulpin'
'n'00 ! cru ;
tela samon
F oim(8 Weeks)
f an»P Weeks)
Field Oupfleate
/V if.
1141
v/Ki£ffl|i4Weef
~
11/30/2016
1 fi3oSli~—T—H55s5Sp^
i w.
P of
cial instructions: Saroptes cofleeiro sk vtj
•ctton Info emaited on day ef shipment
Shipment for Cmm Complete? Y
> oon*Fonnaklehyde
ReftiquJ.v1 by (Signature and Orgar atton) 1 P*l>Vfnn* > Ganc'i- C t> uSuon i >fxn »s
II I' . « rit
(vtU'ce
, c-V_£,
\\-3e- "
/
•to i In
y-Aa*.
f
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„>,m _'
n)r0C. ip >
, .|S , i- * I £
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V ' sv )'i 111
«."• ... ¦* :)
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4 - "" f.
y;-4 3
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*"*• %
4T ,
<• \ *
lift
-------
P»fle 1 Of 2
EPA R10 Lab (MEL) COG (REGION COPY)
DateSWpped: 12/8/2018
CarrterNsme: Hand Delivered
AlrbillNo: NA
K'i
Appendix 8
CHAIN OF CUSTODY RECORD
Formaldehyde NW Aquacuttore/WA
Project Code, WTR-184K
1 of 1
No: 10-112916-204545-0011
20172018B10P2:,2B.,4X24
Contact Name' S'ana Wong
Contact Phon- ,360) 407-5432
Sampta Identifier
CLP Sample
No,
MitrljrfSamplar
Coil,
Method
Analysis/Turnaround (Dayi)
Tag/Pre»ervative/Bottl««
Location
Collection
Date/Time
Sample Type ;
. . i
18494100
i Surface Water
Total/ S.Wong
Composite
Forms 8 Week*'
N1 (None) {1)
HFHJn fluent
12/07/2018
* .eld • am {
; .,,e J
16494101
Surface Water
Total/ S Wong
Discrete
Interval
FermfB Weeks)
ni
4Mbaste-
HFH_E(iuent
12/07/2018
PL£> ^
t-iad Sample >
_ 4~—-
18494102
Surface Water
Total/ S.Wong
Discrete
Interval
Pomp Weeks)
rn {None) (1)
HFH_Eflluent
12/07/2018
I v. go
Field Sample
18484103
I Surface Water
1 Total/ S.Wong
Discrete
Intswal
Form(8 Weeks)
N1 (None) (1)
HFH_EfBuent
12/07/2018 .
Field Sampl®
16494104
Surface Water
; Total/ S Wong
Discrete
Interval
Form(8 Weeks)
N1 {None) (1)
HFH_Effluent
12/07/2015
Ji:0
Field Sample
16494105
Surface Water
Total/ S.Wong
Discrete
Interval
! Form(8 Weeks)
N1 (None) <1}
HFH_Ef9uent
12/07/2018
iJPt
Field Sample j
18494
Surface Water
Total/ S.Wong
Discrete
Interval
FormfB Weeks)
NI (None) (1)
HFH_Efflyent
12/07/2018
lb ID
Field Sample
18494'
Surface Water
Total/ S.Wong
Discrete
Interval
! FormfS Weeks)
NI (Nope) (1)
HFH_EfBuent
12/07/2016r>
IS""1-
pie
18494108
Surface Water
Total/ S.Wong
Discrete
Interval
1 Fotm(8 Weeks)
N1 (None) (1)
HFHJEffluent
12/07/2016
Field Sample
| 10494 i" 09
Surface Water
Total/ S.Wong
Discrete
Interval
FormtB Weeks)
N1 {None) {1J
HFH_E«uent
12/07/2016
Field Sample
1
Surface Water
Total/ S.Wong
Discrete
Interval
J Form{8 Weeks)
N1 (None) (1)
HFHJEffluent
12/07/2018
Raid Sample
'tlkSeJ
POP
Sampled) to be used for Lab QC. 16494101 Tag NI, 18494101 Tag N2, 18494101 T*g N3 • Special Instructions. Samples collected
and shipped by Ecology. RSCC needs ecology sample times and associated collection Wo emaled on day of shipment
Shipment for Ca«e Complete? Y
Sample* Transferred From Chain of Custody #
Analysis Key: Form»FormaWeby
Items/Reason
Relinquished by (S gnature and Organization)
Date/tir Signature and Organization)
rte | Sample Conditio!
t__ —
^ f >.
il'? • L. 'S, ;|<7 Cc- Ccrk/
M.'7-iL \H >';
!
> ' w. u
tXi-U!
A ' , CL
i -nD
I
i
1 i *
119
-------
Appendix 8
Page 2 of 2
EPA R10 Lab (MEL) COC (REGION COPY)
DateShipped 12/8/2018
CarrierName Hand Delivered
AirbiNNo: NA
CHAIN Of CUSTODY RECORD
Formaldehyde NW Aquaculture/WA
Project Code WTR-184 K
1 of 1
No: 10-1 Kir
20172018610P202BD4X24
uOiiUCi (»c re i-at *
Contact Pton 37-6432
Sample Identifier
CLP Sample
No,
MatrixfSampler
Coil.
Method
Analysis/Turnaround {Days)
Taj/Preservative/Bottles
Location
Collection
Date/Time
Sample Type
16454111
Surface Water
Total/ S.Wong
Discrete
Interval
Form(8 Weeks)
N1 (None) (1)
1
j
Field Sample
16494112
Surface Water
Total/S.Wong
Discrete
Interval
Form(8 Weeks)
N1 (None) (1)
HFH_Effluent
12/07/2016
Field Sam
18494113
Surface Wafer
Total/ S.Wong
Discrete
Interval
ForraCI Weeks)
N1 (None) (1)
Jifil
Field Sample
[ 16494114
Surface Water
TataV S.Wortj
Composite
FormfB Weeks)
Ml (None! (1)
HFH_rw
Field Sample
16494115
Water/ S.Wong
Grab
Form(8 Weeks}
N1 {None) (1}
Blank
QC Blank-
Rlnsate/Equlpm
ami
18494116
Surface Water
Total/ S.Wong
4Qm5ai
tejJormjB Week*)
N1 (None} (1)
jsnl
1B494VI7—•j
Surfade Water
Total/S.Wong
Sast»
„ ,r; c-1
. . n'8 Weeks)
H l/iWAM
N1 {Nona) (1)
"V Z^mni
te,JalB5E:
%
r
i
I
i i
|
i
i
1
i ; .!
[ ]
i r 1
f I
I
i€
Special Instructions: Samples collected and shipped by Ecology, RSCC needs ecotegf sample limes and associated collection info
¦mailed on day of shipment.
Shipment for Casa Complete? Y
Samplas Tra Deferred From Chain of Custody #
Analysis Key: Form=FomaIdehyde
Items/Reason
Relinquished by (Signature and Organization}
i by {Signature and Organlzatie
Date/Time
Sample Condition Upon Receipt
**"» tjiJ
\2-'lip, jf ^ U- t*>*%J"'
J
|
120
-------
&EPA
United States Environmental Protection Agency, Region 10
1200 Sixth Avenue, Suite 900
Seattle, WA 98101-1128
A
EPA-910-R-17-005
August 2017
------- |