ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
EPA-330/2-75-007
South Dakota Toxaphene Use Study
June - September 1975
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
AND
x.
REGION VIM JX
DENVER, COLORADO r '-
OCTOBER 1975
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ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
South Dakota Toxaphene Use Study
June-September 1975
October 1975
National Enforcement Investigations Center
and
Region VIII
Denver, Colorado
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CONTENTS
I INTRODUCTION 1
II SUMMARY AND CONCLUSIONS 2
III STUDY AREA 3
South Dakota Sunflower Belt ... 3
Brown-Spink County Study Area . . 4
Sampling Stations, Schedules
and Methods 4
IV STUDY FINDINGS ..... 7
June 1975 Study 7
July 1975 Study 10
September 1975 Study 10
REFERENCES . . . . 12
APPENDICES
A Region VIII Request to NEIC . . 13
B Field Sampling Methods .... 16
C Analytical Methods 18
TABLES
1 Analytical Results of Toxaphene
Use Study, June 1975 9
2 Toxaphene Analysis from Fish
Collected in the Area of a
Fish Kill, July 1975 11
3 Analytical Results of Toxaphene
Use Study 11
FIGURES
1 Sampling Station Locations 5
2 Acreage Cultivated in Sunflowers
and Treated with Toxaphene .... 8
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I. INTRODUCTION
During the spring of 1975, the State of South Dakota reported an
infestation of cutworms which threatened the sunflower production in
twenty-three counties. To suppress the cutworm population and prevent
the projected damage to 20,000 ha (50,000 acres) of crop, the State
requested a special exemption from the Environmental Protection Agency
(EPA) to use toxaphene.* Pursuant to Section 18 of the Federal In-
secticide, Fungicide and Rodenticide Act, the EPA granted an exemption,
allowing South Dakota to use toxaphene from 4 June to 15 July to control
the cutworms.
On 11 June 1975, the National Enforcement Investigations Center
(NEIC) was requested by the Enforcement Division, EPA Region VIII,
Denver, Colorado, to investigate the environmental impact of toxaphene
spraying in South Dakota. The request [Appendix A] lists the exemption
restrictions set forth by the EPA Pesticide Registration Division,
Washington, D. C.
Following the request from EPA Region VIII, NEIC conducted a field
investigation in Brown and Spink Counties, South Dakota. The principal
objectives of the study were to:
1. Assess the short-term effects of toxaphene on the ecosystem
adjacent to fields being sprayed to control cutworms.
2. Determine the efficacy of using toxaphene to control
cutworms in young sunflower plants.
* The name Toxaphene is registered for common usage.—Merck Index, 8th Ed.
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II. SUMMARY AND CONCLUSIONS
On 4 June 1975, EPA issued a 42-day permit to South Dakota, allowing
the State to use toxaphene on the commercial sunflower crop to control a
cutworm infestation. The NEIC was asked by EPA Region VIII to help its
Pesticides Branch monitor the application of toxaphene, assess the
environmental impact of it, and determine how effectively toxaphene
controlled cutworms.
A field investigation began in June 1975 at two areas adjoining the
James River in Brown County, South Dakota. A reference area, where use
of toxaphene was prohibited, was selected near the Sand Lake National
Wildlife Refuge. Another area 30. km (18 mi) south, which included
toxaphene-treated fields and adjacent wetlands, was used to monitor the
environmental effects of toxaphene.
The June study showed that toxaphene provided adequate control of
cutworms on young sunflower plants. Also, measurable amounts of toxaphene
(0.1 to 0.51 yg/g) were found in minnows collected from nearby streams.
Surveillance of the area by EPA and U. S. Fish and Wildlife Service
revealed no other environmental impact.
The second phase of the toxaphene use study was conducted in July
1975, following a fish kill near the Sand Lake Refuge reference area.
NEIC reported the .probable cause of the kill to be a lack of oxygen in a
reach of the James River. Chemical analyses of vital organs removed
from the fish confirmed the fact that toxaphene did not kill the fish.
The final phase of the study was completed in September 1975.
Neither harm nor detectable residues from toxaphene were apparent in
fish or crayfish from the treated area.
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III. STUDY AREA
SOUTH DAKOTA SUNFLOWER BELT
The sunflower belt begins near the northeastern border of South
Dakota and extends south and west through the James River Valley. Its
gently undulating terrain is elevated 274 to 427 m (900 to 1,400 ft)
above sea level.1 Much of the area is dotted with ponds or lakes, lying
adjacent to extensive marshlands -- 280,000 ha (700,000 acres) of wetlands.
A portion of the sunflower production area is drained by the James
River.
Commercial sunflower production in South Dakota began about 1966.
The crop is grown principally for vegetable oil but has other uses,
including confectioneries and bird seed. Young sunflower plants are
annually subjected to a barrage of insect pests. One of the most trouble-
some is the larvae of a moth known as cutworm (Chorizagrotis sp). This
insect larvae feeds on the sunflower stems and leaves, often cutting the
plant off near the soil. Many of these larvae have infested fields and
have been responsible for complete crop failure.
In 1975, about 26,000 ha (65,000 acres) in South Dakota were culti-
vated with sunflowers. In May a cutworm outbreak threatened the com-
mercial sunflower crop. The State requested and received permission
from the EPA to apply toxaphene (an organochlorine insecticide) to
control the cutworm infestation in 23 counties of northeastern South
Dakota. The EPA restricted the applicators to minimize environmental
damage to wetlands adjacent to the sunflower fields. NEIC conducted the
toxaphene monitoring program described in this report to specifically
measure the environmental impact.
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BROWN AND SPINK COUNTY STUDY AREA
Brown and Spink Counties lie in the James River Valley. The river
flows southward, dividing each county into approximately equal halves.
More than 10,000 ha (25,000 acres) of sunflowers are grown in the two
counties; the majority of crop is produced adjacent to the James River.
A reference area at the northern boundary of Sand Lake National
Wildlife Refuge in Brown County was selected for the field evaluation.
The Refuge is comprised of wetlands used by migratory waterfowl as a
major breeding area. Contributing to the selection of the reference
area was the fact that it was not subjected to aerial spraying of toxaphene.
Also, since the area lay north of the sunflower belt, runoff water from
toxaphene-treated fields did not flow into the reference area wetlands.
The study area selected to monitor environmental effects of toxa-
phene application included treated fields and a portion of the James
River and its principal tributaries south of Sand Lake Refuge in Brown
and Spink Counties. This portion of the study area was directly sub-
jected to aerial spraying of toxaphene. Furthermore, water runoff from
the fields drained into the streams being monitored for pesticide
contamination.
SAMPLING STATIONS, SCHEDULES AND METHODS
Ten sampling stations were established to monitor toxaphene. One
station was in the reference area at the northern boundary of Sand Lake
Refuge (Station 01). The remaining 9 stations were in the toxaphene-
treated fields in Brown and Spink Counties and in the James River and
its tributaries. From these sampling stations, fish, invertebrates,
water, sediment, aquatic vegetation and soil were collected [Fig. 1].
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5
BROWN
COUNTY ROAD 5
ABERDEEN |—I
= FISH
= WATER
= SED/MENT
= INVERTEBRATES
= 5011
f=VEGETAT/ON
KILOMETERS
L if
10 STATE ROAO 20
figure I. Sampling Station localioni, Brown and Spink Counties, South Ookolo
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From 25-27 June 1975, toxaphene applications were monitored, and
the efficacy of toxaphene for control of cutworms on young sunflower
plants was evaluated. When a fish kill occurred near the reference area
on 5 July, fish were collected on 9 July for examination at NEIC. On 2-
3 September, the possibility of short-term translocation of toxaphene
from treated sunflower fields into the surrounding environment was
investigated.
Grab sampling techniques (one sample per station per sampling
period) were used to collect water, soil, sediments and biota for
pesticide analyses. Times and types of samples were varied to correlate
with toxaphene-spray applications and rain-runoff periods. Detailed
methods for field sampling and analyses are presented in Appendices B
and C.
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IV. STUDY FINDINGS
An infestation of cutworms (chorizagrotis sp) was discovered in the
commercial sunflower crop of Brown County, South Dakota on 1 June 1975.2
Three days later (4 June 1975) the EPA granted a special permit to the
State to use a toxaphene formulation to suppress the cutworm population
and to reduce the threat of severe sunflower crop destruction. Immediately,
an intensive pesticide spraying program began on cutworm-infested sun-
flower fields throughout Brown County as well as the northeast corner of
South Dakota. As shown in Figure 2, farmers and commercial applicators
applied toxaphene in 12 counties with air and ground equipment at the
EPA specified rate of 2.3 kg/ha (2 Ib/acre).
JUNE 1975 STUDY
NEIC began a field monitoring program in Brown County, South Dakota
on 25 June 1975. Approximately 99% of the planned toxaphene applications
on sunflower fields in the county were completed by that time.3'4
Following aerial pesticide application, samples of water, sediment,
soil and biota were collected from and adjacent to treated fields and
from the reference area in Sand Lake Refuge. Analysis of these samples
[Table 1] showed measurable amounts of toxaphene in field soils (Station
5: 0.32 yg/g) and minnows from nearby streams (Stations 2, 8 and 9:
0.12, 0.51 and 0.10 yg/g). Environmental Protection Agency and U. S.
Fish and Wildlife Service personnel* inspected these areas. They
Robert R. Johnson, Manager, Waubay National Wildlife Refuge, South
Dakota; William Bair, Manager, Sand Lake National Wildlife Refuge,
South Dakota
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Figure 2. Acreage Culrivafed in Sunflowers in South Dakota and Treated with Toxaphene ( ) at Authorized by the f P A,(June 4 — July 15, 1975)
00
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Table 1
ANALYTICAL RESULTS OF TOXAPHENE USE STUDY
IN BROW! AND SPINK COUNTIES, SOUTH DAKOTA
June 1975
Station
No.
01
02
03
04
05
06
07
08
08
08
09
10
Location
Reference Area
James R. , Brown Co. Hwy 5
. Toxaphene Sprayed Area
Elm R. Brown Co. Hwy 14
Pond, W. side S. 28
Putney Twp
Drain, SW of SE Sec 30
Putney Twp
Sunflower field SW of
SW Sec 28 Henry Twp
Sunflower field NE 1/4
Sec. 10, E. Gem Twp.
Ditch west of field NE 1/4
Sec 10, E. Gem Twp
Sunflower field 1/4 mile west
of Mud Cr. Brown Co. Hwy 21
Ditch from field west of Mud
Cr. Brown Co. Hwy 21
Mud Ck. , W. Hanson Twp.
Brown Co. Hwy 21
Mud Ck, Spink Co. Hwy 11
James R. , S. Dakota Hwy 20
Type off
Sample
Sediment
Water
Fathead minnow
N. pike (kidney)
Aquatic vegetation
Sediment
Water
Fathead Minnow
W. Crappie (liver)
Sediment
Water
Sediment
Water
Soil
Soil
Soil
Soil
Soil
Sediment
Water
Fathead Minnows
Crayfish
Aquatic Vegetation
Sediment
Water
Fathead Minnows
Crayfish
Sediment
Water
Bullhead (kidney)
Carp tf
Crayfish
Toxaphene
Concentration
<0.2
<0.8 vg/1
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10
found that toxaphene provided control of cutworms on sunflowers. And
they found no fish and wildlife mortalities or substantial decline in
species or wildlife numbers.
JULY 1975 STUDY .
On 5 July 1975, a fish kill occurred in the James River near the
Sand Lake National Wildlife Refuge. The kill, in the reference area
used by NEIC for the toxaphene study, was investigated by an NEIC senior
fishery biologist. The NEIC biologist joined a team of scientists from
the State of South Dakota and the U. S. Fish and Wildlife Service. The
team surveyed the affected reach of the James River and estimated 600
fish were killed, principally northern pike. Because water samples
collected and analyzed at various points along the James River revealed
a low dissolved oxygen level (2.0.mg/l), oxygen deficiency was suspected
to be the cause of the kill.
Live fish (perch and northern pike) were collected on 9 July,
preserved by freezing and returned to NEIC for further examination.
External and internal examination of fish showed no gross abnormalities.
Whole-body, young-of-the-year yellow perch were analyzed for toxaphene
residue, and kidneys were removed from the larger fish, northern pike,
and also analyzed for toxaphene; however, no toxaphene was detected
[Table 2].
SEPTEMBER 1975 STUDY
On 2-3 September, fish samples were collected at four sites [Table 3],
In June, fathead minnows collected at Station 08 in Mud Creek contained
0.51 yg/g toxaphene. However, in September Mud Creek was dry at Station
08 and no fish were collected there. Downstream at Mud Creek Station 09
and at all other locations no toxaphene was detected in any of the fish.
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11
Table 2
TOXAPHENE ANALYSIS FROM FISH COLLECTED
IN THE AREA OF A FISH KILL
North and South Dakota - July 1975
Location Type of Toxaphene
Sample Concentration
(yg/g)
James R., Dickey Co. Hwy 5
N. Dak. Northern pike (kidney) <0.50
James R., Brown Co. Hwy 5
S. Dak. Northern pike (kidney) <1.7
Yellow perch1" <0.2
Yellow perch1" <0.2
t Young-of-the-year
Table 3
ANALYTICAL RESULTS OF TOXAPHENE USE STUDY
IN BROWN AND SPINK-COUNTIES, SOUTH DAKOTA
September 1975
Station
No. -
Location
Type
of Sample
Toxaphene
Concentration
(vg/g)
Reference Area
01 James R., Brown Co.
Hwy 5 Carp (viscera) <0.5
Toxaphene Sprayed Area
02 Elm R., Brown Co.
Hwy 14 W. Crappie (viscera) <0.4
09 Mud Ck., Spink Co.
Hwy 11 Carp (viscera) <0.3
Fathead Minnows <0.3
Crayfish <0.3
10 James R., S. Dakota
Hwy 20 Carp (viscera) <0.2
Bullhead <0.2
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12
REFERENCES
1. Westin, F. C., L. F. Ruhr and G. J. Buntley, 1967. Soils of South
Dakota. Soil Survey Series No. 1; Agronomy Dept. S. Dakota State
Univ., Brookings, S.Dak., 32 p.
2. Berndt, Wayne, S. Dakota State Univ., Brookings, S.Dak. Personal
Communication (verbal) to John Hale, Environmental Protection
Agency, Denver, Colo. [June 17, 1975].
3. Caven, James, Aberdeen Flying Service, Aberdeen, S.Dak. Personal
Communication (verbal) to John Hale, Environmental Protection
Agency, Denver, Colo. [June 25, 1975].
4. De Hoog, Marvin, Brown County Agricultural Extension Agent.
Personal Communication (verbal) to John Hale, Environmental Protection
Agency, Denver, Colo. [June 26, 1975].
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Appendix A
EPA Region VIII Request to NEIC
11 June 1975
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
SUBJECT: Section 18 Exemption
DATE: June 11 • 1975
FROM: David A. Wagoner, Director
8AH
TO: Thomas P. Gallagher, Director
Pursuant to Section 18 of the FIFRA, EPA has granted an exemption
to the State of South Dakota on June 4, 1975 to use a toxaphene form-
ulation to suppress populations of cutworms destroying young plants
on 50,000 acres of the commercial sunflower crop in South Dakota. The
exemption is subject to the following restrictions:
1. The dosage rate shall not exceed 2.0 pounds per acre actual
toxaphene.
2. Treated acreage shall not exceed 50,000 acres.
3. The counties to be treated are limited as follows: Beadle,
Brookings, Brown, Campbell, Clark, Codington, Day, Deuel , Edmunds,
Faulk, Grant, Hamlin, Hand, Hughes, Hyde, Kingsbury, Marshall, McPherson,
Potter, Roberts, Spink, Sully, and Wai worth.
4. Leaves and stalks are not to be used for livestock feed.
5. • The South Dakota Cooperative Extension Service must supervise
any aerial application to avoid or minimize drift to non-target areas.
6. No toxaphene applications are permitted on or near reservoirs,
rivers, streams or wetlands. This will reduce probability of con-
tamination of domestic water supplies as well as minimize impact of
toxaphene on waterfowl .
7. This exemption will expire July 15, 1975.
8. The South Dakota Cooperative Extension Service will collect
data on efficacy, residues, and environmental impact of toxaphene spray
program. Pesticide personnel of EPA Region VIII shall be informed of
the times and places of toxaphene applications so that monitoring
activities of EPA can be coordinated with those of the Cooperative
Extension Service.
9. A residue level not to exceed 7.0 ppm in or on sunflower seeds
has been determined to be adequate to protect public health. The Food
and Drug Administration, DHEW, has been advised of this action. Sunflower
seeds not to exceed this level may be offered in interstate commerce.
EPA Form 1320-6 (Rev. 6-72)
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However, it should be emphasized that sunflower seeds harvested from
acreages treated with toxaphene must be used for oil and are excluded
from use for confectioneries, bird seed or any non-oil use.
Due to the magnitude of the exemption, the potential for misuse
and environmental effects and the need for data in order to evaluate
expected future use of toxaphene in this manner, I feel that it is
important to thoroughly investigate a few large toxaphene applications
to sunflowers. Hhatever support that you can provide to assist in this
effort would be appreciated.
If you are able to participate in this investigation, program
coordination should be through:
Ivan W. Dodson, Chief
Pesticides Branch
Robert W. Harding, Chief
Field Operations Section
Pesticides Branch
I hope that such a short notice does not present undue problems
for your program.
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Appendix B
Field Sampling Methods
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17
FIELD SAMPLING METHODS
SEDIMENT
Samples were collected with an Eckman dredge. Each sample was
placed in a glass wide-mouth quart bottle and sealed with a teflon
lined lid. The glass bottles were properly labelled and refrig-
erated on crushed ice for shipment to the analytical laboratory at
NEIC in Denver, Colorado.
WATER
Samples were collected in glass wide-mouth quart jars, sealed with
a teflon-lined lid, labelled and preserved on crushed ice for
shipment.
VEGETATION
Aquatic vegetation was collected by hand and wrapped in acetone-
washed aluminum foil, labelled and preserved on crushed ice for
shipment.
SOIL
Samples were collected with a metallic coring device capable of
collecting a core sample 5 cm (2 in) in diameter by 7.5 cm (3 in)
deep. Each sample was wrapped in acetone-washed aluminum foil,
labelled and refrigerated on crushed ice for shipment.
FISH AND CRAYFISH
Specimens were collected with a 10.5 m (35 ft) seine with 6.3 mm
(1/4 in) bar mesh. At each collection site, species were wrapped
separately in acetone-washed aluminum foil, and properly labelled.
Samples of fish and crayfish were preserved on crushed ice until
the end of the day and then placed in a freezer. The frozen samples
were returned to the NEIC laboratories in Denver for pesticide
.residue analyses.
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Appendix C
Analytical Methods
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19
ANALYTICAL METHODS
WATER
Approximately 1 liter of water was extracted in series with 150,
100, and 100 ml of hexane. The container of solvent was then
placed on a hot plate under a gentle stream of air and evaporated
to 10 ml. A 1 yl aliquot of the extract was analyzed on a gas
chromatograph (GC) with an electron capture detector (EC) for
toxaphene.
SOIL AND SEDIMENT
These were analyzed using a method developed by D. F. Goerlitz for
the ASTM.* A 50 g portion of the sample is dried overnight in an
oven to determine moisture content. All results are reported on
the basis of dry weight. Another 50 g portion is extracted with a
40 ml acetone/80 ml hexane mixture, then re-extracted twice with a
20 ml acetone/80 ml hexane mixture. The sample is back-extracted
three times with water and dried using sodium sulfate (NapSO*).
The extract is then evaporated to 10 ml in a Kuderna-Danish evaporative
concentrator. After an alumina column cleanup, a 1 yl aliquot of
the sample was analyzed on an EC/GC for toxaphene.
VEGETATION
Twenty grams of aquatic vegetation was put into a blender and
extracted in series using 17o ml and 175 ml of hexane. The hexane
extracts were combined and filtered through Whatman No. 1 filter
paper. The sample was then evaporated to 10 ml on a hot plate
under a gentle stream of air. A 1 yl aliquot of the extract was
analyzed for toxaphene using an EC/GC.
American Society fop Testing and Materials
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20
FISH AND CRAYFISH
A 20 g sample of whole organism or a smaller amount of organs, was
extracted in a blender using 175 ml and 175 ml of hexane. The
hexane extracts were combined and filtered through a Whatman No. 3
filter paper. The hexane extract was evaporated to 15 ml on a hot
plate under a gentle stream of air and then partitioned with four
25 ml portions of hexane-saturated acetonitrile. The acetonitrile
was evaporated to dryness on the hot plate and 10 ml of hexane
added. After an alumina column cleanup, a 1 ul aliquot of the
extract was injected in an EC/GC and analyzed for toxaphene.
ALUMINA COLUMN CLEAN-UP
The 10 ml extracts were added to 2 x 15 cm columns of activated
alumina deactivated with 3% water and pre-wetted with hexane. The
columns were eluted with 10% ethyl ether in hexane and four 50 ml
fractions were collected. Toxaphene elutes in fractions 1 through
3, with the majority eluting in fraction 2..
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