ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
TRANSLOCATION OF HEPTACHLOR AND CHLORDANE
FROM
INDIANA CORNFIELDS
September 1975
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
DENVER, COLORADO
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CONTENTS
I. INTRODUCTION 1
II. SUMMARY AND CONCLUSIONS 3
III. DESCRIPTION OF THE STUDY AREA 7
Throckmorton Farm 7
Sampling Stations 9
Sampling Schedule 11
IV. STUDY FINDINGS 13
Chlordane 13
Heptachlor 18
APPENDICES:
A Correspondence
B Sampling Equipment and Methods
C Analytical Methods
D Analytical Results
E Chain of Custody Procedures
TABLE
1 Sampling Schedule 12
FIGURES
1 Map, Throckmorton Agricultural Research Center ... 8
2 Sampling Locations 10
3 Chlordane in Air Samples 15
4 Wind Direction and Velocity 16
5 Heptachlor in Air Samples 20
iii
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I. INTRODUCTION
In recent years, concern has been expressed by environmentalists
and governmental agencies about the safety of the continued widespread
use of the pesticides chlordane and heptachlor. After reviewing issues
raised about environmental and health effects of these pesticides and
their metabolites, the EPA Administrator issued a Nat-ice of Intent to
Cancel Registration of heptachlor and chlordane [Appendix A]. The
notice was protested by manufacturers and formulators of these chlo-
rinated hydrocarbon pesticides. As a result, the Office of General
Counsel asked the National Enforcement Investigations Center (NEIC) to
assist them in preparing evidential material in support of the hearing.
A literature review by NEIC scientists on air quality aspects of
these two pesticides indicated, among other things, that the current
applications of these pesticides allow their vapors and dusts to occur
in ambient air masses. The Office of General Counsel then asked the
National Enforcement Investigations Center to further document these
literature survey findings with a verification study in an agricultural
area, particularly one in which chlordane and heptachlor normally are
used.
A field investigation was conducted from 24 April to 5 June 1975
during the corn planting season when the pesticides under study are
normally disked into soil of cornfields as a preplanting farming practice.
The area selected for study was the Throckmorton Agricultural
Research Center owned by Purdue University, West Lafayette, Ind. This
farm was selected because 1) it is an applied agricultural research
area; 2) the farm manager was willing to follow the NEIC study plan; and
3) the physical layout of the farm was appropriate for this study.
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II. SUMMARY AND CONCLUSIONS
A field investigation was conducted from 24 April to 5 June 1975 to
determine the fate of chlordane* and heptachlor which are disked into
field soils before corn is planted. Two fields at the Purdue University
Throckmorton Agricultural Research Center were selected for study. The
smaller field, 12 ha (29 acres), was treated with a formulation of 72 ECF
chlordane (72% technical chlordane) at a rate of 4.5 kg/ha (4 Ib/acre).
The larger field, 13 ha (32 acres), was treated with 3 ECF heptachlor
(30.2% heptachlor) at the rate of 2.2 kg/ha (2 Ib/acre). Immediately
following soil treatment, corn was planted in each field.
Air samples were collected from 32 stations, 16 in each cornfield.
Water samples from a tile drain underlying the heptachlor treated field,
and surface runoff from both fields were collected and analyzed for
pesticide contamination.
General Findings:
1. Two sampling techniques were used to determine translocation
of heptachlor and chlordane into ambient air. One method used
a nylon chiffon screen which was treated with ethylene glycol
and suspended in a metal frame above the fields for approxi-
mately three days; the second method used an impinger-type
sampler in which ambient air was drawn through a liquid
reservoir of ethylene glycol for 24 hours. The aerial screen
sampler was better for collecting the less volatile chlordane,
and the impinger sampler was more efficient for collecting
heptachlor.
* As used in this report, chlordane refers to "technical chlordane"
which encompasses all its major isomers and related compounds.
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2. The study demonstrated that heptachlor and chlordane were
translocated from soils upon which they were applied and
contaminated the surrounding air and water environment.
3. Prevailing winds transported airborne heptachlor and chlordane
compounds northeasterly across and away from the cornfields.
Specific Findings:
1. A preapplication sampling of the air above the two fields
conducted two and one-half weeks before the pesticide ap-
plication showed the presence of small amounts of chlordane,
3
averaging 2.36 yg on the aerial screens and 5.5 ng/m in the
impinger sample. Heptachlor was not detected in any samples.
A second sampling done just before application showed average
chlordane levels of 0.37 yg on the aerial screens and
1.6 ng/m in the impinger sample. Heptachlor was also found
at low levels; aerial screens contained an average of 0.08 yg,
3
with 0.94 ng/m found in the impinger samples.
2. Ambient air sampling immediately after application of chlor-
dane to the cornfield showed average chlordane levels of
3
22.1 yg on aerial screens and 30.5 ng/m in impinger samples.
Ambient air samples collected over the heptachlor treated
field immediately after the pesticide application showed
average levels of heptachlor were 0.51 yg on aerial screens
3
and 244 ng/m in impinger samples.
3. A second sampling of the air above the two pesticide treated
cornfields approximately one week after application showed
chlordane averaged 23.8 yg on the aerial screens and 13.9 ng/m
in the impinger samples. Heptachlor measured an average of
3
0.57 yg on aerial screens and 55.1 ng/m in impinger samples.
-------
A final sampling of the air about three weeks after pesticides
were applied to the cornfields showed an average chlordane
3
level of 7.19 yg on aerial screens and 16.9 ng/m in the
impinger samples. Heptachlor levels decreased to an average
of 0.22 ]
samples.
of 0.22 yg on aerial screens and 15.4 ng/m in the impinger
5. Rainfall and water from tile drains were collected prior to
the application of pesticides to the cornfields. No hepta-
chlor or chlordane were detected in these preapplication water
samples. Following rainfalls, postapplication sampling of
runoff water was done also. Surface runoff was collected from
the heptachlor and chlordane treated cornfields. Analysis of
a water sample collected on 22 May 1975 showed that runoff
from the heptachlor treated field contained 152 yg/1 of hepta-
chlor. Runoff collected 30 May 1975 from the chlordane
treated field contained 25 yg/1 chlordane. Also, on 30 May
1975 a water sample from a tile drain underlying the hepta-
chlor treated field was contaminated with 2.3 yg/1 heptachlor.
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III. DESCRIPTION OF THE STUDY AREA
THRQCKMQRTON FARM
Field studies on the translocation of heptachlor and chlordane were
conducted at the Throckmorton Agricultural Research Center in Tippecanoe
County, Indiana. The farm was given to Purdue University in 1935 and
has since been used as an agricultural research center and experimental
station. It is located on State Highway 43 and county road 800 South,
approximately 9 km (5-1/2 mi) southwest of Lafayette, Ind. [Fig. 1]. Of
the 120 ha (297 acres) comprising the farm, 54 ha (134 acres) are in
Section 5 (T 21 NR4W) and 66 ha (163 acres) in Section 6 (T 21 NR4W).
The study area consisted of 13 ha (32 acres) in Section 5 where hep-
tachlor was applied and 12 ha (29 acres) in Section 6 where chlor-
dane was applied. The study site and surrounding acreage are character-
ized by gently rolling terrain with several drainage areas. Five water-
sheds are located on the chlordane field and four on the heptachlor
field. The heptachlor field has a subsurface tile drain system which
empties into a creek 75 m (246 ft) southeast of the heptachlor field
[Fig. 2].
The chlordane field is bounded on the north and south by corn-
fields of 11 ha (27 acres) and 26 ha (65 acres), respectively. On the
west is a 6.5 ha (16 acre) field of soybeans; Highway 43 and the hepta-
chlor field are adjacent on the east.
Pasture land lies on the east and south boundaries of the hep-
tachlor field. County road 800S borders on the north side of the field.
Several residences are directly across the road, and numerous other
residential areas are in the vicinity of the farm [Fig. 1], In 1969 the
present heptachlor field was sprayed with heptachlor; both fields were
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l-t. 1
THROCKMORTON FARM
SCALE - MILES
Figure 1. Location of Throckmorton Agricuffural ftecearch Center
Tippecanoe County, Indiana
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treated with aldrin in 1971. No pesticides have been applied to either
field in the past four years.
SAMPLING STATIONS
Thirty-two sampling stations were established for this pesticide
study, sixteen in each cornfield [Fig. 2].
Air samples were collected from each of these sampling locations by
an aerial screen or an impinger-type air sampling apparatus. Descrip-
tions of the sampling equipment are presented in Appendix B.
2 2
Square nylon chiffon screens (0.25 m ; 2.25 ft ) were suspended
vertically from eleven wood-aluminum frames in the chlordane field. Two
frames held a lower and upper screen approximately 1 and 2 m (3 and 6 ft)
above the ground, while the remaining eight frames held single screens
about 2 m above the ground.
Historical records indicated the prevailing winds were from the
southwest; therefore, 1 double screen and 3 single screens were placed
diagonally in the northeast corner of the field. A double screen was
also placed in the center of the field facing southwest into the pre-
vailing winds. Single screens were placed in the northwest, southeast
and center of the field in the event that wind direction changed.
The placement of the frames in the heptachlor field was similar to
that of the chlordane field. These frame locations were used during
each phase of the study.
Air sampling units (ethylene glycol impinger apparatus) were pe-
riodically operated at three locations in each cornfield. The samplers
were placed near the center and in the northeast and southwest corners
of the heptachlor- and chlordane-treated fields [Fig 2 ].
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n
SAMPLING SCHEDULE
Air sampling began in April 1975 to correspond with the corn plant-
ing season and the normal time for application of heptachlor and chlor-
dane. The study consisted of five sampling sequences, four days each.
Sequences I and II occurred before application of the pesticides to
obtain background data. Sequence III began immediately after appli-
cation, sequence IV was 6 to 7 days after application, and sequence V
was 20 to 21 days after application [Table 1]. Analytical methods and
results, as well as chain of custody procedures followed during the
survey are described in Appendices C, D and E, respectively.
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Table 1
SAMPLING SCHEDULE
THROCKMORTON AGRICULTURAL RESEARCH CENTER
TTPPECANOE COUNTY, INDIANA
24 April-5 June 1975
Sequence
I-Preapplication
II-Preapplication
III-Postapplication
IV-Postappli cation
Date
(1975)
4/24-27
5/8-12
5/12-16
5/19-22
Sample
Air
Air
Air
Air
Rainfall
Tile Drain
Air
Air
Air
Air
Exposure Time
Sampling Method (hours)
Aerial Screens
Impinger
Aerial Screen
Impinger
Composite
Grab
Aerial Screens
Impinger
Aerial Screens
Impinger
48
24
85
24
2
68
24
70
24
5/24
5/30
V-Postapplication 6/2-5
Surface Runoff Grab
Tile Drain Grab
Tile Drain Grab
Tile Drain Grab
Surface Runoff Grab
Air
Air
Tile Drain
Aerial Screens
Impinger
Grab
70
24
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IV. STUDY FINDINGS
CHLORDANE
Field investigations began approximately two and one-half weeks
before chlordane was applied to the cornfield in the study area.
Samples of ambient air contaminants were collected at 14 locations
[Appendix D, Table D-6]. Analyses of these air samples revealed the
2 2
presence of technical chlordane. Square aerial screens (0.25 m ; 2.25 ft )
exposed to the ambient air for 48 hours collected an average of 2.36 yg
chlordane. An impinger-type sampler operating 24 hours in the southwest
corner of the field collected 10.9 ng/m of technical chlordane [Table
D-6]. Impinger-type samplers operating the same period in the center
and northeast corner of the field measured no technical chlordane. Air
contaminants were sampled a second time, just before chlordane was
applied to the cornfield. Aerial screens set up in the cornfield for 85
hours collected an average level of 0.37 yg technical chlordane. Once
again the impinger-type sampler operated 24 hours in the southwest
3
corner of the field, collecting 3.2 ng/m technical chlordane, while the
other units measured no chlordane in the ambient air near the center and
northeast corner of the field.
The only other sample collected from this cornfield during the
preapplication survey was a 2-hour composite rainwater sample. Anal-
yses revealed that the water sample was not contaminated with chlordane.
Chlordane detected during the preapplication survey was presumed to
have come from surrounding areas where it is used in both household and
agricultural pesticide applications. Specific sources of this back-
ground contamination were not determined.
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14
On 13 May 1975 a formulation of 72 ECF Chlordane (72% technical
chlordane) was applied at a rate of 4.5 kg/ha (4 Ib/acre) by a tractor
mounted sprayer and disked into the cornfield soil. Immediately after
the pesticide application, aerial screens and impinger air samplers were
set up at the predetermined sampling stations in the cornfield.
Analyses of samples collected by these devices revealed that chlor-
dane translocated from the cultivated soils into ambient air immediately
after application. Aerial screens exposed to the ambient air over the
cornfield immediately after application for a duration of 68 hours
collected an average level of 22.1 yg technical chlordane. This repre-
sents an increase in technical chlordane on the aerial screens when com-
pared with preapplication levels [Fig. 3].
Air samples collected by all three impinger samples contained
technical chlordane also. Sampling units operating in the northeast
and southwest corners of the field for 24 hours, immediately following
3
chlordane application, collected 37.9 and 23.1 ng/m of technical chlor-
dane. The impinger sampler operating in the center of the field col-
lected 0.20 yg of technical chlordane; however, operating time of this
unit was not recorded because of a malfunction in the timer.
Figure 3 shows a general pattern of chlordane translocation across
the cornfield from southwest to northeast. During the first 24 hours of
the sampling period (13-14 May 1975) prevailing winds of 6 to 10 knots
(7 to 12 mph) blew across the field in this same direction, southwest
to northeast [Fig. 4]. Although many other factors including wind ve-
locity, soil binding properties, humidity, vapor pressures and cultiva-
tion practices may have influenced translocation, these observed wind
conditions correlated with the progressive increase in chlordane con-
tamination across the cornfield.
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Six days after application of chlordane on the cornfield, another
series of air samples was collected. Aerial screens were exposed to
the ambient air for 70 hours. Analyses showed amounts of technical
chlordane in the air ranging from 6.4 yg in the southwest corner of the
field to 43.0 yg in the northeast corner. The pattern of chlordane
distribution was again from the southwest to the northeast, correspond-
ing with prevailing winds [Figs. 3, 4].
Impinger collected air samples showed the persistence of technical
chlordane in the air also. Sampling units, operated for 24 hours in
the northeast and southwest corners of the cornfield, collected air
3
containing 13.7 and 14.1 ng/m of technical chlordane. The impinger in
the center of the field (with a faulty timer) collected 0.12 yg of
technical chlordane.
A series of water samples was collected from drainageways in
watersheds 5, 7 and 8 in the chlordane treated cornfield during this
segment of the survey [Fig. 2]. These surface water samples contained
chlordane levels ranging from 0.3 to 1.6 yg/1, indicating that the pesti-
cide was being washed from field soils following local rain showers.
Twenty days after application of chlordane on the cornfield, a
final series of air contaminant samples was collected. After 70 hours
of exposure to ambient air of the cornfield, aerial screens were analyzed
for chlordane contamination. Analyses of the screen contaminants showed
a decline in technical chlordane to an average of 7.19 yg.
Air contaminants collected by the three impinger samplers during a
24 hour period showed the center of the field and the northeast corner
3
contained 0.92 yg and 33.8 ng/m of technical chlordane, respectively.
Ambient air drawn through the impinger unit in the southwest corner of
the field contained no chlordane. Distribution patterns of chlordane
across the cornfield were again generally in the direction of the
prevailing wind, southwest to northeast [Figs. 3, 4].
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18
Following rainfalls, another postapplication sampling of water was
done. Surface runoff was collected from drainageways in watersheds 5, 7
and 8 in the chlordane treated cornfield. The three samples contained
1.6, 0.3, and 0.8 yg/1 of technical chlordane, respectively.
This study has demonstrated that chlordane was translocated from
soils upon which it has been applied into water supplies and into
ambient air masses.
HEPTACHLOR
A second field investigation was conducted on the same farm in
an adjacent cornfield to the northeast of the chlordane treated field
[Fig. 2]. The purpose of this study was to determine the fate of hepta-
chlor disked into field soil prior to planting corn. The study samp-
ling periods and pesticide application generally corresponded with
those described for the chlordane study.
Samples of ambient air contaminants were collected on 26 April and
12 May 1975 to determine levels of heptachlor prior to treating the
soils of the study area cornfield with the pesticide. No heptachlor
was detected in the ambient air in April, while low levels of 0.07 and
3
0.12 yg heptachlor on screens and 0.94 ng/m in impinger samples were
recorded in May.
Rainfall and water from tile drains underlying the cornfield were
collected prior to the application of heptachlor to field soils. No
contamination by heptachlor was detected in these water samples.
Heptachlor detected in air samples during the preapplication sur-
vey was presumed to have come from surrounding areas, but specific
sources were not determined.
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19
On 12 May 1975, a formulation of 3 EOF heptachlor (30.2% heptachlor)
was applied at the rate of 2.2 kg/ha (2 Ib/acre) by a tractor mounted
sprayer and disked into the cornfield soil. Immediately after appli-
cation, as well as 7 and 21 days later, ambient air was sampled at
various locations in the heptachlor treated cornfield. Samples of
contaminants, collected by aerial screens exposed to the air masses
flowing over the cornfield, generally showed a peak increase in heptachlor
contamination 7 days after the pesticide was applied to the cornfield
soil [Table D-4 and Fig. 5], Typically, during all postapplication
sampling periods, the highest values for heptachlor were recorded from
screens set up in the northeastern section of this L-shaped cornfield
which corresponded with the direction of the prevailing winds.
Airborne heptachlor collected by impinger samplers during the
postapplication studies progressively decreased with time [Tables D 3-5].
Nevertheless, the highest values were recorded from the sampling units
in the northeastern part of the cornfield. Distribution patterns of
air-carried heptachlor were southwest to northeast, again corresponding
with prevailing wind direction.
Analyses of samples collected on 22 and 30 May 1975 showed that
rainwater runoff from the cornfield contained as much as 152 yg/1 of
heptachlor. Additionally, a water sample from the tile drain collected
on 30 May 1975 showed the subsurface water system contained 2.3 pg/1 of
heptachlor.
This study has demonstrated that, after rainfalls, heptachlor was
washed from and percolated through soils into surface and ground water
systems. Furthermore, the study demonstrated that measurable quanti-
ties of heptachlor were translocated from cornfield soils into ambient
air masses flowing over the fields.
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APPENDIX A
CORRESPONDENCE
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UNITED STATES OF AMERICA
ENVIRONMENTAL PROTECTION AGENCY
NOTICE OF INTENT TO CANCEL REGISTRATIONS
HEPTACHLOR OR CHLORDANE
On March 18, 1971, the Administrator of this Agency announced that
active internal review was being initiated on a number of pesticide
products, including those containing chlordane and heptachlor. As the
result of such review and for the reasons set forth in the attached
Statement of Reasons, I find that the continued registration and use
of these pesticides appear to pose substantial questions of safety
amounting to an unreasonable risk to man and the environment. I there-
fore serve and file this Notice of Intent, together with the attached
Statement of Reasons, to cancel all registered uses of heptachlor and
chlordane within thirty (30) days, pursuant to Section 6 of the Federal
Insecticide, Fungicide, and Rodenticide Act, as amended, (86 Stat. 973, 7
U.S. § 136d), with the exception of the use of heptachlor or chlordane
through subsurface ground insertion for termite control and the dipping
of roots or tops of nonfood plants. Any affected party may contest this
action by requesting a hearing on specific registered uses within thirty
(30) days of the date of this notice. Requests for hearings should be
submitted to the Agency's hearing clerk at the following address:
Mrs. Betty J. Billings
Hearing Clerk
U.S. Environmental Protection Agency
Room 1019, Waterside Mall - East Tower
401 M Street, S.W.
Washington, D.C. 20460
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The proposed cancellation shall become final and effective thirty
(30) days from the date of this notice as to those registered uses for
which a hearing is not requested by any affected party. The proposed
cancellation shall not take effect regarding any registered use for
which a hearing is requested until the hearing has been completed,
unless there is a concurrence from all parties to the proceeding. The
Agency reserves the opportunity to present evidence on any registered
use affected by this order regardless of whether or not a hearing has
been requested on that use, or whether or not such use is to be actively
defended in the hearings.
Administrator
\
Dated: Nov 18, 1974
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STATEMENT OF REASONS: Heptachlor and Chlordane
I. Legal Authority
Section 6 (b) of the Federal Insecticide, Fungicide, and Rodenti-
cide Act (7 U.S.C. § 135 et seq) as amended (7 U.S.C. § 136a(c)(5)(D))
authorizes the Administrator of the Environmental Protection Agency
(or his designee) to issue a notice of intent to cancel the registration
of a pesticide or to hold a hearing "[i]f it appears to the Administrator
that a pesticide or its labeling . . . does not comply with the pro-
visions of this act or, when used in accordance with widespread and com-
monly recognized practice, generally causes unreasonable adverse effects
on the environment. . . ." The phrase "unreasonable adverse effects on
the environment" is defined in Section 3 of the Act (7 U.S.C. § 136(bb))
as "any unreasonable risk to man or the environment taking into account
the economic, social, and environmental costs and benefits of any pesti-
cide."
The Act also prohibits the sale of pesticides which are misbranded.
A product is considered misbranded if the label does not contain direc-
tions for use and a warning or caution statement which are necessary and
if complied with are adequate to protect health and the environment.
(7 U.S.C. § 136(a)(l)(F) and (G)).
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APPENDIX B
SAMPLING EQUIPMENT
AND METHODS
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SAMPLING EQUIPMENT AND METHODS
AIR SAMPLER
The air-sampling unit is shown schematically in Fig. B-l. It
contains a pump that draws air through a sampling series or train
and auxiliary equipment to control and measure air flow, switching
the flow from one sampling train to another after a pre-set interval
(a) Sampling train- Each sampling train contains an im-
pinger containing 100 ml of ethylene glycol to trap
particulates and gasses and an adsorption tube packed
with a plug of glass wool to remove any splashover or
water condensation.
(b) Flow control and pump - After the air has been pulled
through the sampling train, it passes through a solenoid
valve controlled by a timer, through a control valve by
which the air flow in the sampling train may be set at
the desired rate as shown on a flowmeter, through the
flowmeter, and finally through the vacuum pump. A momen-
tary contact switch may be closed to switch the air flow
to a particular sampling train so that its flow may be
adjusted or read any time.
Three air sampling units were used in each field. Each unit was
given a station number and was used only at that station. The impingers
were filled with approximately 100 ml of ethylene glycol. Flow rates
were set for 0.9 standard ft /min. The timers were adjusted to permit
collection of two samples in 24 hours (the dial calibrated in percent
of a 24-hour day). Pesticide-free aluminum foil was used to cover the
air intake tubes while transporting the units to their sampling lo-
cations in the fields.
A gas generator provided the power supply at station B-l7. The
generator was set approximately 23 m (75 ft) away to avoid exhaust
contamination.
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AIR INLET
ADSORBENT TUBE
(Glass Wool)
•V..WJ'
RUBBER STOPPER
SOLENOID VALVE
IMPINGER
(Ethylene Glycol)
FLOWMETER
VACUUM PUMP
CONTROL VALVE
Figure B —I. Schematic Drawing of /mpinger-Type Air Samp/ing Unit
-------
The sampling units shutoff automatically after 24 hours. The
units were then transported to the servicing area and disassembled.
The ethylene glycol was removed from the sampling trains and trans-
ferred to 250 ml screw-cap glass bottles. Impingers were rinsed with
approximately 25 ml ethlene glycol which was added to the samples.
The bottles were appropriately labeled and stored in an ice chest
for transportation to the laboratory under chain of custody pro-
cedures [Appendix E].
The ethylene glycol was replaced in the impingers, fresh glass
wool plugs were inserted, the timers were reset, and pesticide free
aluminum foil was placed on the ends of the air intake tubes. The
samplers were then stored until the next sampling sequence.
AERIAL SCREEN APPARATUS
Each aerial screen apparatus consisted of a wood and aluminum
framework. Two 10-ft poles were attached to a 76 x 101 cm (30 x 40 in)
aluminum channel frame, and each apparatus was placed at a sampling
site in the cornfield study area. The top of each frame was above
ground level.
o
Pretreated nylon chiffon cloths (aerial screens) 0.5 m were sus-
pended vertically within the aluminum frame. These aerial screens were
securely suspended in the framework to ensure that they would withstand
sudden gusts of wind and not be blown from the frames. Screens used in
this study were prepared by the method of Tessari and Spencer.* This
method employs treating the screens with a 10% ethylene glycol and
acetone solution. All screens were prepared at NEIC-Oenver and trans-
ported to the study site in chemically clean glass jars.
* Tessavi, J. D. and D. L. Spencer, 1971, Air- sampling in the Human
Environment. Jour. AOAC3 54 (6): 1S76-2382.
-------
Rubber gloves, pre-rinsed in ethylene glycol, were worn while the
screens were suspended within the frame. A different pair of gloves was
worn in each field. At the end of each exposure, the screens were
removed (again using pre-rinsed rubber gloves), placed in chemically
clean glass jars, packed in a shipping container, and transported to the
laboratory under chain of custody procedures [Appendix E].
-------
APPENDIX C
ANALYTICAL METHODS
-------
-------
ANALYTICAL METHODS
EXTRACTION
Aerial Screen Samples: The nylon chiffon screens were
extracted in small soxhlet extractors for 4 hr with
150 ml of 1:1 hexane and acetone. The solvent extract
was then back extracted with 250 ml water in a 500 ml
separatory funnel. The solvent layer was removed and
the water extracted again with two 75 ml portions of
hexane. The combined solvent was concentrated to 10 ml
on a hot water bath under a gentle stream of filtered air.
Impinger Samples: Ethylene glycol samples (ca 250 ml)
were extracted in a 500 ml separatory funnel with two
75 ml portions of hexane. The combined hexane extract
was then back extracted with 250 ml water in the separa-
tory funnel, the solvent layer removed and the water again
extracted with two 75 ml portions of hexane. The combined
solvents were then concentrated to 10 ml on the hot water bath,
Water samples (ca 1 liter) were serially extracted in a
2,000 ml separatory funnel with two 150 ml portions of
hexane. When difficult emulsions were encountered, the
samples were extracted again with a third 150 ml portion
of hexane. The combined hexane extracts were then concen-
trated to 10 ml on a hot water bath under a gentle stream
of filtered air.
ALUMINA CLEANUP
Both the cloth and the ethylene glycol extracts still contained
gross amounts of interfering compounds after back extraction with water
and required additional cleanup. The extracts were added to 2 x 15 cm
columns of activated alumina deactivated with 3% water and prewetted
with hexane.* The columns were eluted with 10% ethyl ether in hexane
* Boyle, H. W.3 R. E. Burttsohell and A. A. Rosen. Infrared Fish.
Advances in Chemistry Series, No. 60: '^rganio Environment.
-------
and four 50 ml fractions were collected. Heptachlor elutes almost
entirely in fraction 1, trans-nonachlor in fraction 2, and gamma and
alpha chlordane in fractions 3 and 4. Fractions 3 and 4 are combined
for subsequent electron-capture gas chromatography. The fractions were
again concentrated to 10 ml on the hot water bath.
ELECTRON-CAPTURE GAS CHROMATOGRAPHY
A 1 yl aliquot of the alumina column fractions of each extract was
analyzed by electron-capture gas chromatography. Minimum detectable
limits for heptachlor and chlordane were 0.01 to 0.1 ug, respectively.
Quantitative estimates were made by computer calculation after cali-
bration runs on standard insecticides run at the same concentration
levels as the samples. The following gas chromatographic conditions
were used:
Gas Chromatograph Hewlett/Packard Model 5713
with Automatic Sampler
Detector Electron-Capture Ni-63
Column 2 mm ID x 6' - Glass 6% 0V-
101 on 60/80 GC-Q
Carrier Gas P-10 (90% Argon/10% Methane)
Flow 20 ml/min
Temperatures:
Injector 200°C
Column 200°C
Detector 250°C
-------
APPENDIX D
ANALYTICAL RESULTS
-------
Tables D 1-11
ANALYSES OF AMBIENT AIR AND WATER CONTAMINANTS
FROM AN INDIANA CORNFIELD
Sample
Location
Date
(1975)
Type
Results
1. Air analyses. Field to be treated with heptachlor.
Sequence 1, preapplication.
H-7
H-ll
H-18
H-2
H-3
H-4
H-5
H-6
H-9
H-10
H-13
H-14
H-15
H-16
H-17
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
NW corner
SW corner
SW corner
SW corner
SW corner
4/28
4/26
4/25
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
NDf
ND
ND
ND
ND
ND
ND
ND
- ND
ND
ND
ND
ND
ND
ND
2. Air analyses. Field to be treated with heptachlor.
Sequence 2, preapplication.
H-7
H-ll
H-18
H-2
H-3
H-5
H-6
H-9
H-10-B
H-10-C
H-13
H-14
H-15
H-16
H-17
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
Center
NW corner
SW corner
SW corner
SW corner
SW corner
5/11
5/11
5/11
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
ND 7
0.908 ng/m^
0.962 ng/nr
0.06 total yg
0.06 "
0.08 "
0.09 "
0.04 "
0.05 "
0.09 "
0.12 "
0.10 "
0.08 "
0.13 "
0.11 "
t Not detected
-------
Tables D 1-11 (Cont.)
ANALYSES OF AMBIENT AIR AND WATER CONTAMINANTS
FROM AN INDIANA CORNFIELD
Sample
Location
Date
(1975)
Type
Results
3. Air analyses. Field treated with heptachlor.
Sequence 3, postapplication
H-7
H-n
H-18
H-2
H-3
H-4
H-5
H-6
H-9
H-10-B
H-10-C
H-13
! .- 1 4
H-15
H-16
K-17
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
Center
NW corner
SW corner
SW corner
SW corner
SW corner
5/13
5/13
5/13
5/15
5/15
5/15 .
5/15
5/15
5/15
5/15
5/15
5/15
5/15
5/15
5/15
5/15
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
145 ng/m3
474 "
112 "
0.51 total
0.61 "
0.44 "
0.52 "
•0.47 "
0.42 "
0.64 "
0.75 "
0.10 "
0.59 "
0.46 "
0.46
0.71
yg
II
4. Air analyses. Field treated with heptachlor.
Sequence 4, postapplication
H-7
H-n
H-18
H-2
H-3
H-4
H-5
H-6
H-9
H-10-B
A-10-C
H-13
H-14
H-15
H-16
H-17
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
Center
NW corner
SW corner
SW corner
SW corner
SW corner
5/21
5/21
5/21
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
47.8 ng/m3
80.2 "
37.2 "
0.45 total
0.86 "
0.33 "
0.63 "
0.24 "
0.75 "
0.94 "
1.08 "
0.28 "
0.29 "
0.57 "
0.66 "
0.30 "
yg
1)
II
II
II
II
II
II
II
II
II
II
II
-------
Tables D 1-11 (Cant.)
ANALYSES OF AMBIENT AIR AND WATER CONTAMINANTS
FROM AN INDIANA CORNFIELD
Sample
Location
Date
(1975)
Type
Results
5. Air analyses. Field treated with heptachlor.
Sequence 5, postapplication
H-7
H-ll
H-18
H-2
H-3
H-4
H-5
H-6
H-9
H-10-B
H-10-C
H-13
H-14
H-15
H-16
H-17
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
Center
NW corner
SW corner
SW corner
SW corner
SW corner
6/4
6/4
6/4
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
20.6 ng/m3
20.0 "
5.77 "
0.29 total
tt
0.26 "
0.39 "
0.33 "
0.07 "
0.45 "
0.41 "
0.19 "
0.07 "
0.13 "
0.03 "
0.05 "
6. Air analyses. Field to be treated with chlordane.
Sequence 1, preapplication
B-7
B-ll
B-17
3-2
B-3
B-4
B-5
B-6
B-9
B-10
B-12
B-14
B-15
B-16
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
NW corner
SW corner
SW corner
SW corner
4/26
4/26
4/25
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
4/26
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
ND
ND -
10.9 ng/m
3.48 total
3.62 "
2.91
3.48 "
2.40 "
2.08 "
1 . 70 "
1.55 "
1.38 "
1.02 "
2.40 "
tt Sample spilled and lost
-------
Tables D 1-11 (Cont.)
ANALYSES OF AMBIENT AIR AND WATER CONTAMINANTS
FROM AN INDIANA CORNFIELD
Sample
Location
Date
(1975)
Type
Results
7. Air analyses. Field to be treated with chlordane.
Sequence 2, preapplication
B-7
B-ll
B-17
B-l
B-2
B-3
B-4
B-6
B-9
B-10-B
B-10-C
B-12
B-14
B-15
B-16
B-7
B-ll
B-17
B-2
B-3
B-4
B-5
B-6
B-9
B-10-A
B-10-B
B-10-C
B-12
B-14
B-15
B-16
NE corner
Center
SW corner
NW corner
NW corner
NW corner
NW corner
NW corner
SE corner
Center
Center
NW Corner
SW Corner
SW Corner
SW Corner
8. Air analyses
Sequence 3,
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
Center
Center
NW corner
SW corner
SW corner
SW corner
5/11
5/11
5/11
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
5/12
. Field
postappl
5/13
5/13
5/13
5/16
5/16
5/16
5/16
5/16
5/16
5/16
5/16
5/16
5/16
5/16
5/16
5/16
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
treated with chlordane.
i cation
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
ND
ND 3
3.20 ng/m
0.38 total
0.45 "
0.48 "
0.58 "
0.36 "
0.29 "
0.32 "
0.35 "
0.39 "
0.26 "
0.26 "
0.27 "
37.9 ng/m3
0.20 total
23.1 ng/m
41.2 total
36.0 "
23.6 "
29.5 "
28.7 "
20.8 "
11.0 "
12.8 "
19.3 "
14.4 "
17.0 "
14.8 "
18.0 "
yg
it
ii
it
n
ii
n
n
n
n
n
n
yg
yg
n
n
n
n
n
n
n
n
n
it
M
n
-------
Tables D 1-11 (Cont.)
ANALYSES OF AMBIENT AIR AND WATER CONTAMINANTS
FROM AN INDIANA CORNFIELD
Sample
Location
Date
(1975)
Type
Results
Air analyses. Field treated with chlordane.
Sequence 4, postapplication
B-7
B-ll
B-17
B-2
B-3
B-4
B-5
B-6
B-9
B-10-A
B-10-B
B-10-C
B-12
B-14
B-15
B-16
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
Center
Center
NW corner
SW corner
SW corner
SW corner
5/21
5/21
5/21
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
5/22
Impinger
Impinger
Impinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
13.7 ng/m3
0.12 total yg
14.1 ng/mj
38.8 total yg
25.6 "
7.00 "
36.2 "
43.0 "
22.1 "
23.3 "
33.5 "
29.9 "
28.0 "
6.40 "
7.41 "
8.04 "
10. Air analyses. Field treated with chlordane.
Sequence 5, postapplication
B-7
B-11
B-17
B-2
B-3
B-4
B-6
B-9
B-10-A
B-10-B
B-10-C
B-12
B-14
B-15
B-16
NE corner
Center
SW corner
NE corner
NE corner
NE corner
NE corner
SE corner
Center
Center
Center
NW corner
SW corner
SW corner
SW corner
"~ *~ " -T ~" ~~" -"--"•• - -J"-'-- ~-~ '-'-'-
6/4
6/4
6/4
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
6/5
Impinger
Impinger
Irroinger
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
Screen
33.8 ng/m
0.92 total yg
ND
6.10 "
5.50 "
9.20 "
13.2 "
1.80 "
7.52 "
8.20 "
9.10 "
4.10 "
NMttt
NM
NM
-------
Tables D 1-11 (Cont.)
ANALYSES OF AMBIENT AIR AND WATER CONTAMINANTS
FROM AN INDIANA CORNFIELD
Sample
Location
Date
(1975)
Insecticide - yg/1
Heptachlor
Chlordane
11. Water Analyses.
and chlordane
Fields treated with heptachlor
Rainfall
Tile Drain
Tile Drain - A
Tile Drain - B
Tile Drain - B
Tile Drain
Watershed 15
Watershed 18
Watershed 19
Watershed 15
Watershed 18
Watershed 19
Watershed 5
Watershed 7
Watershed 8
Watershed 20
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Hept. Field
Chlor. Field
Chlor. Field
Chlor. Field
Chlor. Field
5/11
5/11
5/24
5/24
5/30
6/5
5/22
5/22
5/22
5/30
5/30
5/30
5/22
5/22
5/22
5/30
ND
ND
ND
ND
2.3
ND
152
2.2
2.6
7.0
4.8
3.8
ND
1.6
0.3
0.8
25
-------
MASS SPECTROMETRY CONFIRMATION OF HEPTACHLOR AND CHLORDANE
IN SAMPLES FROM THE INDIANA CORNFIELD SURVEY
Initially a water runoff sample was chosen for gas chromatog-
raphy/mass spectrometry (GC/MS) identification because it contained
relatively high concentrations of heptachlor and gamma chlordane. The
sample was labeled Watershed 15 and represented runoff from the hepta-
chlor field on 22 May 1975. The alumina column fraction number 1 from
this sample was concentrated to 0.5 ml on a hot water bath under a
gentle stream of filtered air. A 1 yl sample of the concentrated
sample was injected into a Finnigan Model 1015 gas chromatograph/mass
spectrometer system. The resulting mass spectrum [Fig. D-l] was a
perfect match to a heptachlor standard run concurrently using the same
instrumental conditions [Fig. D-2],
The impinger air samples H-7, H-ll, and H-18 collected immediately
after application in the heptachlor field were analyzed next. The first
alumina column fraction from each of these samples was combined, con-
centrated, and analyzed on the GC/MS. Again the mass spectrum was a
perfect match [Fig. D-3] to the standard heptachlor. These results
unequivocally confirm the identity of heptachlor in the runoff water
and ambient air samples taken from the heptachlor field.
A standard gamma chlordane sample was run on the GC/MS [Fig. D-4],
along with the gamma chlordane in the combined alumina column fractions
3 and 4 of a technical chlordane standard [Fig. D-5]. These two spectra
were identical. The alumina column fractions 3 and 4 from the H-15
runoff water sample were combined, concentrated and analyzed on the
GC/MS [Fig. D-6]. The resulting spectrum was a match with the gamma
chlordane standard and the gamma chlordane separated from technical
chlordane by column chromatography [Figs. D-4 and D-5]. This confirmed
the identity of chlordane in the water samples.
-------
The alumina column fractions 3 and 4 from the cloth air samples
H-16, H-17, B-3, B-4 and B-5 were combined and concentrated; these
samples were taken from both fields immediately after application.
The combined sample was analyzed on the GC/MS and the presence of
gamma chlordane was quite clear [Fig. D-7]. Another set of samples
from the heptachlor field (cloth samples H-2, H-3, H-4, H-5, H-9, and
H-10) taken during sequence III were combined, concentrated and an-
alyzed on the GC/MS [Fig. D-8]. This combined sample also showed
clear evidence of the presence of gamma chlordane.
-------
FIGURE D-l
SPECTRUM NJMBEB 25 - ZO
1 JN 0-S M-
iln i|.
4JlJ|la^
20
30 1
M/ e
50
60 70 80 90 100 no J20 ,: •'^"••^•-^"^JJ-r^--r
100
FIGURE D-2
SPECTRUM NUMBER 17 -
HePTflCHLflR STD 2S0N6 16SC
3« 3SO 360 370 399 390
-------
1 1 ll I ..I.I ... . ..1
T I"T-''>1"V"-'""
tin!
ill,, «J,I,, m,.,ljlHll
"1 ' "'•' '1 '" '1 ""1"" "
}
t itui i t ultNiij i t It I 1 II 1
1 I ' 1 ' 1 ' I ' 1 ' 1 ' 1 ' ' T ' ' (' ' ' T ' '!" •i"--|----i---'|----i-"'
200 Z10 ZZ0 230 2-K3 Z93 260
280 Z30 300 310 320 330 3-KJ 3S0 36C3 S70 380 390
. «. -
200 213
-------
8
^-
5L
§-
j£O
tijiD
Wi-
tt
1?
Gw_
R-
SJ
FIGURE D-5
SPECTRUM NUM3ER 51 - 47
STD TECH OCQR PL FP 3.1 2S3NS 16SC
t'-| |'"
3SO 360 370 380 330 100 110
n ii
30 H3 SO 60 73 80 30 130 U0 120 130
§
8_
S_
^o
pcc^* —,
(jjO
Qu>_
fcS_
a*.
6S_
o
FIGURE D-6
SPECTRUM NUTfiER 17 - 13
H-IS-WHTER fTR 3-1 16SC 7-30-7S
a » « so b Vo bo ^ oo no U IT
M/ E
I
i|
r^
;10 353 360 370 380 330 100 110
-------
200 210 220 330 2
-------
APPENDIX E
CHAIN OF CUSTODY
PROCEDURES
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL FIELD INVESTIGATIONS CENTER-DENVER
BUILDING 53, BOX 25227. DENVER FEDERAL CENTER
DENVER, COLORADO 80225
July 24, 1974
CHAIN OF CUSTODY PROCEDURES
General:
The evidence gathering portion of a survey should be characterized by the
minimum number of samples required to give a fair representation of the
effluent or water body from which taken. To the extent possible, the quan-
tity of samples and sample locations will be determined prior to the survey.
Chain of Custody procedures must be followed to maintain the documentation
necessary to trace sample possession from the time taken until the evidence
is introduced into court. A sample is in your "custody" if:
1. It is in your actual physical possession, or
2. It is in your view, after being in your physical possession, or
3. It was in your physical possession and then you locked it up in
a manner so that no one could tamper with it.
All survey participants will receive a copy of the survey study plan and will
be knowledgeable of its contents prior to the survey. A pre-survey briefing
will be held to re-appraise all participants of the survey objectives, sample
locations and Chain of Custody procedures. After all Chain of Custody samples
are collected, a de-briefing will be held in the field to determine adherence
to Chain of Custody procedures and whether additional evidence type samples
are required.
Sample Collection:
1. To the maximum extent achievable, as few people as possible should
handle the sample.
2. Stream and effluent samples shall be obtained, using standard field
sampling techniques.
3. Sample tags (Exhibit I) shall be securely attached to the sample
container at the time the complete sample is collected and shall
contain, at a minimum, the following information: station number,
station location, date taken, time taken, type of sample, sequence
number (first sample of the day - sequence No. 1, second sample -
sequence No. 2, etc.), analyses required and samplers. The tags
must be legibly filled out in ballpoint (waterproof ink).
-------
Chain of Custody Procedures (Continued)
Sample Collection (Continued)
4. Blank samples shall also be taken with preservatives which will
be analyzed by the laboratory to exclude the possibility of
container or preservative contamination.
5. A pre-printed, bound Field Data Record logbook shall be main-
tained to record field measurements and other pertinent infor-
mation necessary to refresh the sampler's memory in the event
he later takes the stand to testify regarding his action's
during the evidence gathering activity. A separate set of field
notebooks shall be maintained for each survey and stored in a
safe place where they could bo protected and accounted ror at
all times. Standard formats (Exhibits II and III) have been
established to minimize field entries and include the date, time,
survey, type of samples taken, volume of each sample, type of
analysis, sample numbers, preservatives, sample location and
field measurements such as temperature, conductivity, DO, pH,
flow and any other pertinent information or observations. The
entries shall be signed by the field sampler. The preparation
and conservation of the field logbooks during the survey will
be the responsibility of the survey coordinator. Once the
survey is complete, field logs will be retained by the survey
coordinator, or his designated representative, as a part of the
permanent record.
6. The field sampler is responsible for the care and custody of the
samples collected until properly dispatched to the receiving lab-
oratory or turned over to an assigned custodian. He must assure
that each container is in his physical possession or in his view
at all times, or locked in such a place and manner that no one can
tamper with it.
7. Colored slides or photographs should be taken which would visually
show the outfall sample location and any water pollution to sub-
stantiate any conclusions of the investigation. Written documenta-
tion on the back of the photo should include the signature of the
photographer, time, date and site location. Photographs of this
nature, which may be used as evidence, shall also be handled
recognizing Chain of Custody procedures to prevent alteration.
Transfer of Custody and Shipment:
1. Samples will be accompanied by a Chain of Custody Record which
includes the name of the survey, samplers signatures, station
number, station location, date, time, type of sample, sequence
number, number of containers and analyses required (Fig. IV).
When turning over the possession of samples, the transferor and
transferee will sign, date and time the sheet. This record sheet
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Cnain of Custody Procedures (Continued)
allows transfer of custody of a group of samples in the field,
to the mobile laboratory or when samples are dispatched to the
NFIC - Denver laboratory. When transferring a portion of the
samples identified on the sheet to the field mobile laboratory,
the individual samples must be noted in the column with the
signature of the person relinquishing the samples. The field
laboratory person receiving the samples will acknowledge receipt
by signing in the appropriate column.
2. The field custodian or field sampler, if a custodian has not
been assigned, will have the responsibility of properly pack-
aging and dispatching samples to the proper laboratory for
analysis. The "Dispatch" portion of the Chain of Custody Record
shall be properly filled out, dated, and signed.
3. Samples will be properly packed in shipment containers such as
ice chests, to avoid breakage. The shipping containers will be
padlocked for shipment to the receiving laboratory.
4. All packages will be accompanied by the Chain of Custody Record
showing identification of the contents. The original will accom-
pany the shipment, and a copy will be retained by the survey
coordinator.
5. If sent by mail, register the package with return receipt request-
ed. If sent by common carrier, a Government Bill of Lading should
be obtained. Receipts from post offices and bills of lading will
be retained as part of the permanent Chain of Custody documentation.
6. If samples are delivered to the laboratory when appropriate person-
nel are not there to receive them, the samples must be locked in
a designated area within the laboratory in a manner so that no
one can tamper with them. The same person must then return to the
laboratory and unlock the samples and deliver custody to the
appropriate custodian.
Laboratory Custody Procedures:
1. The laboratory shall designate a "sample custodian." An alternate
will be designated in his absence. In addition, the laboratory
shall set aside a "sample storage security area." This should be
a clean, dry, isolated room which can be securely locked from the
outside.
2. All samples should be handled by the minimum possible number of
persons.
3. All incoming samples shall be received only by the custodian, who
will indicate receipt by signing the Chain of Custody Record Sheet
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Chain of Custody Procedures (Continued)
accompanying the samples and retaining the sheet as permanent
records. Couriers picking up samples at the airport, post
office, etc. shall sign jointly with the laboratory custodian.
4. Immediately upon receipt, the custodian will place the sample
in the sample room, which will be locked at all times except
when samples are removed or replaced by the custodian. To the
maximum extent possible, only the custodian should be permitted
in the sample room.
5. The custodian shall ensure that heat-sensitive or light-sensitive
samples, or other sample materials having unusual physical
characteristics, or requiring special handling, are properly
stored and maintained.
6. Only the custodian will distribute samples to personnel who are
to perform tests.
7. The analyst will record in his laboratory notebook or analytical
worksheet, identifying information describing the sample, the
procedures performed and the results of the testing. The notes
shall be dated and indicate who performed the tests. The notes
shall be retained as a permanent record in the laboratory and
should note any abnormalities which occurred during the testing
procedure. In the event that the person who performed the tests
is not available as a witness at time of trial, the government
may be able to introduce the notes in evidence under the Federal
Business Records Act.
8. Standard methods of laboratory analyses shall be used as described
in the "Guidelines Establishing Test Procedures for Analysis of
Pollutants," 38 F.R. 28758, October 16, 1973. If laboratory
personnel deviate from standard procedures, they should be prepared
to justify their decision during cross-examination.
9. Laboratory personnel are responsible for the care and custody of
the sample once it is handed over to them and should be prepared
to testify that the sample was in their possession and view or
secured in the laboratory at all times from the moment it was
received from the custodian until the tests were run.
10. Once the sample testing is completed, the unused portion of the
sample together with all identifying tags and laboratory records,
should be returned to the custodian. The returned tagged sample
will be retained in the sample room until it is required for trial.
Strip charts and other documentation of work will also be turned
over to the custodian.
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Chain of Custody Procedures (Continued)
11. Samples, tags and laboratory records of tests may be destroyed
only upon the order of the laboratory director, who will first
confer with the Chief, Enforcement Specialist Office, to make
certain that the information is no longer required or the samples
have deteriorated.
EXHIBIT I
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EPA, NATIONAL FIELD INVESTIGATIONS CENTER - DENVER
Station No. I Station
I I ocation
Date
BOD
Time Grab Sequence Number
Comp .
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ents Other
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EXHIBIT IV
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL FIELD INVESTIGATIONS CENTER - DENVER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
Station
Number
Station Location
Date Time
Relinquished by:
Relinquished by:
Relinquished by:
SAMPLERS: (Signature)
Sample
Type
Coinp_.
Grab
Seq.
#
No. of
Containers
Analysis
Required
Received by: Date Time
Received by: Date Time
Received by Mobile Laboratory for Date Time
Field Analysis:
Dispatched by: (Signature) Date Time Received for Laboratory by: Date Time
Method ot Shipment:
Distribution: Original - Accompany shipment
1 copy - Survey Coordinator Field Files
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