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                    <text>ABSTRACT

In conjunction with the illuminating flare test and evaluation program on
Eglin AFB Reservation, a project was initiated to determine the effect of
the flare testing on the flora and fauna on the test areas, as well as selected
laboratory species. The results from these tests demonstrate that the
residue of illuminating flares has minimal environmental effects except at
high concentrations.

Approved for public release; Distribution Unlimited

iii
(The reverse of this page is blank)

�AFATL-TR-72-204

STUDIES TO DETERMINE
THE

ENVIRONMENTAL EFFECTS

OF
ILLUMINATING FLARE RESIDUE

PYROTECHNICS BRANCH
FLAME, INCENDIARY, AND EXPLOSIVES DIVISION

TECHNICAL REPORT AFATL-TR-72-204

NOVEMBER

1972

Approved for public release; Distribution Unlimited

AIR FORCE ARMAMENT LABORATORY
AIR FORCE SYSTEMS COMMAND * UNITED STATES AIR FORCI

EGLIN AIR FORCE BASE, FLORIDA

�Studies to Determine
the

Environmental Effects

of
Illuminating Flare Residue

Bobby M. Agerton
Don D. Harrison
John W. Sigler, 2Lt, USAF
Stephen W. Lander, Jr., 2Lt, USAF

Approved for public release; Distribution Unlimited

�FOREWORD

The USAF project directly related to the information in this report is
Project 5066, Armament Development Pollution Control, Task 01, Work Unit 01.
This report documents specific studies conducted during the period November
1971 to September 1972.
The authors would like to express their appreciation to Captain Jimmie
C. Cornette, Dr. John H. Hunter, 2Lt Vanessa Birdsey, Mrs. Sandra Lefstad,
Captain Allen B. Beach, ILt Ray Kruzek, and SSgt Terry Collatz for their
assistance in this project and in the preparation of this report.
Because of the nature of the experimentation performed, the results
were dependent on the exact materials and equipment used; therefore, a notation
of sources and manufacturers is provided for reference but is not intended
to constitute endorsement of these companies by the United States Air Force.
This technical report has been reviewed and is approved.

FRANKLIN C.' DA1/IES,'tolonel, USAF

Chief, Flame, Incendiary and Explosives Division

11

�ABSTRACT

In conjunction with the illuminating flare test and evaluation program on
Eg!in AFB Reservation, a project was initiated to determine the effect of
the flare testing on the flora and fauna on the test areas, as well as selected
laboratory species. The results from these tests demonstrate that the
residue of illuminating flares has minimal environmental effects except at
high concentrations.

Approved for public release; Distribution Unlimited

111
(The reverse of this page fs blank)

��TABLE OF CONTENTS

Section
I

Page

III

IV

1

GENERAL MATERIALS AND METHODS

2

MAMMALIAN TOXICITY STUDIES

3

1. Methods and Materials
2. Results and Discussions

II

INTRODUCTION

3
5

V

PLANT TOXICITY STUDIES

6

1.
2.
3.
4.

6
7
7
8

FISH BIOASSAY STUDY

1.
2.
3.
4.
VI

Experiment One
Experiment Two
Experiment Three
Discussion
Water Chemistry Investigation
Methods and Materials
Results
Discussion

9

9
10
11
15
16

1. Methods and Materials
2. Analytical Techniques for Soil pH
3. Analytical Techniques for Magnesium and Sodium
Determinations in Soil
4. Discussion
VII

SOIL LEACHING STUDY

16
17

CONCLUSION

20

V
(The reverse of this page is blank)

17
18

��SECTION I
INTRODUCTION

Testing of illuminating flares to determine various illumination
characteristics involves outside burning. Air Force Regulation 19-1 requires
that the environmental efforts of any action be assessed; however, no data
were available concerning the environmental consequences of outside testing
of flares. Since an ecological impact on the test sites and the surrounding
area was considered possible, investigations were conducted to determine the
effects of the residue from the combustion process.
Testing of pyrotechnic items is currently carried out at the Pyrotechnics
Research Area adjacent to Range 22 of Eg!in AFB Main Complex and at Test Area
C-52A. The Pyrotechnics Research Area outdoor test facility is adjacent to
Choctawhatchee Bay and is 50 to 75 meters from the bay high tide line.
The toxic properties of the illumination flare constituents are fairly
well documented with regard to humans. However, little is known concerning the
effect of the residue produced on plant and animal life, especially the
aquatic ecosystem. LDcQ data are available for some species of test organisms.
These data (Reference T;, however, deal with massive, one-time injections or
orally administered dosages and do not account for effects from exposure
associated with soil or aquatic systems. The illumination flare residue is
relatively insoluble in water, as is the major constituent, MgO (1.9 mg/l
from Reference 1), but it imparts alkalinity to water and also acts as an
abrasive.
A series of tests was designed and conducted to determine the actions
and effects of illumination flare residues in relation to mammals (white mice),
plants (various species), water chemistry (pH, Mg, and Na changes), fish
(mosquito-fish, Gambusiaaffinis Batrd and Girard.and bluegill sunfish,
Lepomis macrochirus Rafinesque), and leaching in a soil column.
The tests were intended as a survey to determine possible problems in
the environment and to indicate where further studies might profitably be
directed.

�SECTION II
GENERAL MATERIALS AND METHODS

Pyrotechnic residue was obtained from three sources. Samples One and Two
were obtained from a contractor's facility bag house and expansion chamber,
respectively. The major constituents of these flares before combustion were:
Magnesium (Mg)

58.0%

Sodium Nitrate (NaNOa)

37.5%

Laminae Binder

(Mark 24 or 45 Composition)

4.5%

Sample Three was collected on polyethylene sheeting at the Eglin Pyrotechnics Research Area outdoor test facility. During a test period when
twenty-five LUU-2/B flares were to be burned, a sheet of 6 mil polyethylene
3.04 by 6.1 meters (10 by 20 feet) with an area of 18.6 square meters (200
square feet) was placed on the test site downwind from the flare which was
suspended 40 feet above the ground. The wind during this test was generally
from the southwest (210 degrees from north) at 5 knots. The center of the
polyethylene was 25 meters from a point directly beneath the suspension
apparatus.
At the conclusion of the flare test, the material on the sheeting was
collected and placed in a drying oven at 49°C for 48 hours. Total weight
of the material was approximately 2500 grams after drying. 2 This results
in approximately 134.5 g/m2 or 5.38 g/m2/f!are (12.5 g/ft or 0.5 g/ft2/
flare) at a distance of 25 meters downwind from the burning flare. From
these data, the approximate amounts of residue to be used in the various
biological and chemical tests described in this report were established.
The composition of the flares burned at the Eglin Pyrotechnics Research
Area was:
Magnesium (Mg)
Sodium Nitrate (NaNOa)
Polymer Binder

61.0%
30.0%
9.0%

(LUU-2/B Composition)

The most probable products of combustion from these flares are:
5 Mg + 2 NaN03

-&gt; Na20 + 5 MgO + N

Since magnesium is in excess in the flare composition:

2 Mg -i- 02

-&gt;

2 MgO

This results in the production of a maximum of 6,771 grams of MgO per flare,
assuming 100% conversion or an average of 159,275 grams (352 pounds) per 25
flare test.
Concentrations of illumination flare residue used in the bioassays and chemi'
cal studies were selected to approximate the most extreme conditions which might
be encountered during normal testing to illustrate the extreme effects of the
residue on the environment. Further studies to determine actual concentrations
of residue resulting from testing will be conducted and reported in future
technical reports.

�SECTION III
MAMMALIAN TOXICITY STUDIES
1. METHODS AND MATERIALS
A study was conducted to determine the effects of illumination flare
residue (Sample 1) on white mice, The residue was administered by exposure and
in drinking water.
Thirty mice were randomly selected to test the effects of the residue.
The experiment consisted of three groups, each containing 10 male Swiss-Webster
albino mice. The mice were weighed and placed in three separate cages. The
cages were supplied with litter (San-i-cel© ), commercial food (Purina Lab
Chow ©) and water as follows:
CAGE ONE (Control)
1400 gm litter
400 ml H20
250 ml food
10 male mice
CAGE TWO (Residue in water)
1400 gm litter
400 ml H20 (2,500 mg illumination flare residue/^)
250 ml food
10 male mice
CAGE THREE (Residue in litter)
1400 gm litter (with 1 gram of illumination flare residue)
400 ml H20
250 ml food
10 male mice
The litter and water were replaced 7 days after the experiment was initiated,
and the experiment was terminated at the end of 15 days. It was felt that
gross effects would occur during this time period. Weights of the individual
mice were again determined at that time. Results of the test are shown in Table I.
The mice in Cage Two ingested the pyrotechnic residue while those in
Cage Three were allowed to come in contact with the material through their
skin and by inhalation. Autopsies were not performed, but the animals were
observed for a period of 30 days after the test termination.

�CAGE
NO.

INITIAL
WEIGHT,
gram

TABLE I. MOUSE TOXICITY STUDY
AVERAGE
AVERAGE
AVERAGE
INITIAL
FINAL
FINAL
WEIGHT
WEIGHT, WEIGHT,
WEIGHT,
CHANGE,
gram
gram
gram
gram

AVERAGE
WEIGHT
CHANGE,
%

ONE

35
37
37
39
39
40
43
43
45
46

40.4

38
39
40
41
48
43
44
45
45
48

43.1

2.7

6.68

TWO

24
26
26
29
34
36
37
37
38
38

32.5

33
33
33
39
40
40
40
41
41
41

38.1

5.6

17.23

THREE

29
30
31
36
36
37
37
40
43
45

36.4

37
37
41
41
42
42
42
42
45
46

41.6

5.2

14.28

�2. RESULTS AND DISCUSSIONS

Visual operations during this experiment indicated that illumination flare
residue, in the quantity used, had no detrimental effects on mice. There
was a normal increase in weight with the control group, but the mice in both
treatments (Cages Two and Three) gained more weight than the control group
(Table I). It is not clear whether the increased weight gain was due to the
treatment or other factors, and further tests would be required to determine
the reason for the variation in weight gain. If it was due to treatment,
other observations indicated that it was in no way detrimental.

�SECTION IV
PLANT TOXICITY STUDIES

Plant toxicity data were obtained from three experiments: (1) cucumber
seed germination and root development, (2) illumination flare residue applied
to foliage, and (3) plant growth in soil containing illumination flare
residue.
1. EXPERIMENT ONE

a. Methods and Materials
Several preliminary experiments were conducted to determine concentration ranges to consider in this experiment. This experiment was then set
up to determine the effects of illumination flare residue on the germination
and initial development of cucumber seeds. Thirty-gram samples of soil, each
containing 50, 100, 250, 500, or 1000 mg/kg of illumination flare residue
(Sample One) were placed in petri dishes. For comparison purposes, reagent
grade MgO was added to separate soils in various concentrations. Distilled
water (12 ml) was then added and a piece of Whatman #3 filter paper was placed
on the soil surface. Five cucumber (Cucumis sativus var. Long Green) seeds
were placed on the filter paper and allowed to germinate for 72 hours in the
dark at 26°C. The root lengths were measured to determine if any inhibition
had occurred. Experiments were conducted in triplicate.
b. Results
Treatment
(illumination flare
residue/soil)
Control
50 mg/kg
100 mg/kg
250 mg/kg
500 mg/kg
1000 mg/kg

Root Length (cm)after 3 days
Average of each Petri dish
5.4

5.1

6.4

4.1

4.3

4.1

4.5

3.9

3.9

1.7

1.9

1.9

1.4

1.3

1.3

0.9

0.8

0.6

Average
5.6
4.2
4.1
1.8
1.3
0.8

Slight inhibition of root development occurred at levels as low as
50 mg/kg and soil with 1000 mg/kg almost completely inhibited germination.
There was also a large increase in inhibition from 100 mg/kg to 250 mg/kg.
These results, however, were not different from the effects of the reagent
grade MgO used in this experiment. The pyrotechnic residue used in this
experiment had no effects on cucumber development greater than the reagent
grade MgO.

�2. EXPERIMENT TWO

a. Methods and Materials
Several species of plants received foliar application of illumination
flare residue (Sample One) to determine if dusts or fall-out from illumination
flare tests would injure vegetation. The foliage was wet with a small hand
sprayer to facilitate sticking and then approximately 1 gram of the illumination
flare residue was dusted onto a portion of the foliage. The following plant
species were used:
SCIENTIFIC NAME

COMMON NAME

Paspa1 urn no taturn

bahia grass

Pueraria thunbergiana

kudzu

Fortu1 aca o1eracea

portulaca

Mam' ho t u til 1 s s i ma

cassava

Melia azederach

chinaberry

Prunus caroli m'ana

cherry laurel

Musa sp.

banana

Oryza sativa

rice

Utricularia sp.

bladderwort

Cynodon dactyl on

bermuda grass

Pinus elliotii

slash pine

Observations were made periodically for 30 days after treatment to determine
if any damage had occurred.
b. Results
No visible damage had occurred to any plants 30 days after foliar
treatment.
3. EXPERIMENT THREE

a. Methods and Materials
An experiment was initiated to determine if residue from illumination
flare tests visibly affected the growth of several plant species. Since the

�flare residue does not leach readily (see Section IV) and would therefore
remain predominantly on the soil surface, the residue was applied in terms
of units per area rather than units per volume of soil. Seeds of the following
species were planted in a soil consisting of a 7:3:1 ratio of sandy loam, peat
moss, and perlite with 5 pounds of dolomite lime and 1 pound of super phosphate
added per cubic yard of soil mix.
SCIENTIFIC NAME

VARIETY

COMMON NAME

Oryza sativa

IR-8

rice

Latuca satiy a

Grand Rapid

lettuce

Zea mays

Coker 71

corn

Cucumis satiyus

Long Green

cucumbers

Lycopersicon esculentum

Homestead

tomatoes

Illumination flare residue (Sample I) was added to the soil samples
on the surface at rates of 500 Ib/acre and 1000 Ib/acre after seeds were
planted. Plants were grown in a glass greenhouse with 45% shade. Pots were
watered daily from the top to allow the residue to leach downward. Visual
observations only were made for 60 days.
b. Results
No visible difference was observed between the control plants and those
receiving either concentration of illumination flare residue. Lettuce plants
died after approximately 30 days as a result of disease, but there was no
effect from the treatment.
4. DISCUSSION

Even when illumination flare residue falls directly on vegetation, it does
not appear to be extremely harmful. The largest portion of the residue is
MgO, and this is probably used by the plant after it enters the soil system.
Magnesium is one of the required plant nutrients and is a component of the
dolomitic limestone commonly used in agricultural operations.
The only effect observed in these studies was inhibition of initial root
growth after the germination of cucumber seeds in soil that contained the
illumination flare residue. This residue could conceivably affect the seed
germination of native plant species around a pyrotechnic test area if
sufficient amounts accumulated. However, it is expected that any
effect would be limited to a small area close to a highly used test
site.

8

�SECTION V
FISH BIOASSAY STUDY

The limited reference material available concerning the effects of
illumination flare residue applies chiefly to terrestrial animals
("Environmental Statement" compiled in October 1971 by Captain Jimmy C,
Cornette from Navy OP 2793). Therefore, the effect of the residue on two
fish species was investigated.
The chemistry of the illumination flare residue and the reactions which
occur in combination with water are fairly straightforward. Upon combination
with water (humid air is sufficient), NaJ) and MgO convert as follows:
Na20 + H20 -»• 2NaOH
MgO + H20^ Mg(OH)2

Magnesium and sodium hydroxides impart alkalinity to water if present
in high concentrations. Sodium compounds, NaOH and particularly Na20, combine
readily with water (Reference 1). Due to the lack of pertinent information
concerning aquatic effects, a study utilizing fish as a bioassay organism
was designed and implemented. It should be stressed at this time that these
tests were a survey and did not provide detailed information concerning the
effects of the illumination flare residue on fish.
1. WATER CHEMISTRY INVESTIGATION

Because pH increase was known to be the main effect of the materials
incorporated in the illumination flare residue, varying concentrations of the
residue were added to four types of water, and the increase in pH was measured.
Quantities of the illumination flare residue were added to water from the
following sources:
1. Distilled water (from the laboratory Barnstead still)
2. Weekly Pond (fresh water)
3. Choctawhatchee Bay (salt water)
4. Tap water (aerated for 5 days)

�a. Methods and Materials
A beaker containing 1 liter of the water to be tested was placed on
a magnetic stirrer (speed six, Sargent Stir Plate©) and constantly stirred
with a Teflon©stir bar. Amounts of the illumination flare residue (Sample
One) were added to the water to obtain concentrations of from 1.0 mg/liter to
1000 mg/liter of the residue. After 5 minutes of stirring at each concentration,
pH determinations were made with a standard laboratory unit. The results are
shown in Table II.
b. Discussion
The pH of all four types of water tested was increased by the
addition of as little as 0.01 gram (10.0 mg/liter) of the illumination flare
residue.
A smaller initial increase in pH and a lower, or equal, increase in
pH at the higher concentrations were noted in the Choctawhatchee Bay samples
compared to the other types. This effect is probably due to the greater
buffering capacity of sea water compared with that of fresh water. Because
of the lower buffering capacity of the distilled water and tap water, it
follows that the pH of the Weekly Pond water would increase more than that of
sea water and less than or equal to that of tap water. These effects probably
account for a large percentage of the variability in the results of the Fish
Bioassay Section as discussed below.
2. METHODS AND MATERIALS

Fish were obtained from three sources. Mosquitofish (Gambusia affinis
Baird and Girard) were obtained from ponds on Eg!in AFB Reservation, chiefly
from Anderson Pond. Bluegill sunfish (Leppmis macochirus Rafinesque) were
obtained from the Holt Fish Hatchery, Holt, Florida, and the Jackson Guard
Station on Eg!in AFB Reservation.
All fish were transported from the field to the laboratory in 50 gallon
plastic containers and placed in 20 gallon Instant Oceans®, aquaria equipped
with a two air stone filter-flow aeration system. The tanks were filled with
either tap water (aerated for 5 to 10 days) or water from Weekly Pond.
Variations in water type used will be discussed later.
Fish were placed in glass battery jars which had previously been filled
with 10 liters of the test water to be used. An air stone system attached
to a series of Silent Giant®air pumps was placed in each jar.
With the exceptions noted on the tables, five male and five female
mosquitofish of approximately equal size were used for each treatment
involving Gambusia. Six bluegill of approximately equal size, without
regard to sex, were used for each treatment in the Lepomis tests. During
Test Two with the Lepomis, all fish were weighed and marked, but only limited
data were obtained due to the premature termination of the test (see Table III).
10

�TABLE II. WATER pH INCREASES EFFECTED BY ILLUMINATION FLARE RESIDUE
(SAMPLE THREE)
CONCENTRATION,
mg/l
00.00
1.00
10.00
25.00
50.00
100.00
200.00
300.00
500.00
1000.00

TAP WATER

DISTILLED

WEEKLY POND

CHOCTAWHATCHEE
BAY

8.4
8.4
8.4
8.5
8.5
8.6
8.8

5.4
5.6
5.6
5.8
6.0
6.4
8.7
9.4
9.7
10.0

7.4
7.5
7.5
7.7
8.0
8.8
9.3
9.6
9.9
10.0

8.0
8.0
8.1
8.1
8.2
8.3
8.5
8.7
8.9
9.6

—
9.1
9.6

|
1
i
;

Readings were taken after a 5 minute period on a magnetic stirring plate.

During the tests, the fish were fed 0.1 gram of commercial fish food
(Purina Fish Food©) in the morning. If the fish did not eat during the morning feeding, the evening feeding was omitted for all test fish. Seven tests
were conducted with Gambusia and two with Lepomis. Due to the wide variations
in test procedures, each test and its results will be described separately.
Because of the method of introducing the illumination flare residue and the
fact that the tests dealt with an aquatic system, TLX data are presented rather
than LDijQ or LD-JQQ data. All conditions and results of the tests are presented in Tables ill to V.
3. RESULTS

In concentrations of 100 mg/l and above, the illumination flare residue
appeared to be toxic to the Bluegill Sunfish. Lower concentrations seemed
to have little detrimental effect (Table III).
Gambusia were not affected detrimentally by the illumination flare residue
when tested in water from Weekly Pond, but seemed extremely susceptible in
tap water (Table IV).
As this study was intended to be a survey, replications of individual
tests were not to be performed. However, the results obtained in the Gambusi'a
bioassays in tap water were so difficult to interpret that they were repeated
(Table V). At the end of three replications, it appeared that the illumination
flare residue was not toxic to Gambusia in the concentrations used.
11

�TABLE III.
TEST
NUMBER
ONE

BLUEGILL SUNFISH BIOASSAY TESTS

HOLDING
TEST JAR
TEST
TANK WATER PARAMETERS/
MATERIAL
TYPE
ACCLIMATION TIME TYPE/CONC.
Tap
pH 8.1
SAMPLE ONE3
DO —
50 mg/£

% Sat.
1 hr.

100 mg/£
500 mg/£

TWO

ro

Weekly
Pond

pH 8.1
DO 6.4-8.0
% Sat. 16-20.5

8 days

TL

50

TL

x

COMMENTS

&gt;2 days TL11C 144 hr. All fish that died showed
D
gill damage. Filaments
41 hr. TL w \J 66 hr. were torn. Heavy mucous
was present and all deaths
18 hr. TL I VW 52 hr. observed were preceded by
flashing.

SAMPLE THREEb

100 mg/£
125 mg/£
150 mg/£
200 mg/£
300 mg/£

The fish were weighed and
placed in the tank.
Observations were made
during a 12 hour period
of the day. Additional
observations were made
after 24 hours. No
distress was evident in
any tank. After 48 hours
all the fish were found
dead with the exception
of the controls. The
fish had been dead for
12-18 hours and were
partially decayed. These
data yield an approximate
TLiQg of 36-42 hours.

.Sample I: Residue from bag house at contractor's facility.
Sample III: Residue from Eg!in Pyrotechnics Research Area.

�TABLE IV. GAMBUSIA BIOASSAY TESTS
1

TEST

9

TEMPERATURE MATERIAL^
TEST TEST JAR1
NUMBER WATER TYPE OF TEST, C TYPE/CONC.

ONE

Tap3

18°

TWO

Weekly
Pond

17°

Weekly
Pond

18°

ONE
mg/l
mg/l
mg/l

50

10 hr.
5 hr.
10 hr.

ADDITIONAL
TL
x
TL80 30 hr.
TL1Q 30 hr.
TL^g 30 hr.

COMMENTS

,

Moderate to severe
distress before all
deaths.

SEE TABLE V

THREE

SAMPLE
10
100
1000

TL

FOUR4

j SAMPLE ONE
0.1 mg/l
1 .0 mg/l
10.0 mg/l
50.0 ma/ 1
! SAMPLE THREE
!
50 mg/l
I 100 mg/l
i 125 mg/l

No mortality at any
concentration.
Experiment terminated
at end of 13 davs.
&gt; 24 days TL334 7 days
&gt; 24 days TLis 9 days
&gt; 24 days TL]g 4 days

No aeration for 2-1/2
hours before test
started. Additional
subsequent loss of power
at 24 days prompted
termination of experiment.

1 Tests One and Two had a jar acclimation time of 1 hr. 45 minutes, Test Three
had a jar acclimation time of 68 hours, and Test Four had a jar acclimation
2time of 16 days.
Sample One: Residue from contractor's facility, bag house, Sample Two:
Residue from contractor's facility, expansion chamber, and Sample Three:
^Material collected on polyethylene sheeting at Eg!in Pyrotechnic Research Area,
.Tap water had been aerated from 2 to 4 days.
Only six fish were used in each treatment of Test Four.

�TABLE V. RESULTS OF TEST TWO, GAMBUSIA

TEST TWO/ ,

REPLICATES'
A

TEST
TEST
JAR
WATER TEMPERATURE MATERIAL
TYPE OF TEST, C TYPE/CONC.
18°
SAMPLE TWO
Tap
10 mg/£

TL

50

ADDITIONAL
TL
x

COMMENTS

Sample Two material is
approximately twice as
dense as Sample One.

100 mg/£
1000 mg/£
B

Tap

18°

7 hr.

TL90 21 hr.
TL10Q 19 hr.
TL100 19 hr.

1000 mg/£

2

3 hr.
7 hr.

0
0
0

TL]0 76 hr.

SAMPLE TWO
10 mg/£

0

TL1Q 76 hr.

SAMPLE TWO
10 mg/£

100 mg/£
3

C

Tap

18°

100 mg/£
1000 mg/£
3,4D

Tap

18°

76 hr.

SAMPLE TWO
10 mg/£

No mortality at the end of

100 mg/£
1000 mq/£

96 hours.
_i

—

_

In the Initial test, A, 10 mg/£ appeared to be more toxic than 1000 mg/£ . The test was then
^replicated three times.
Replicate B was run with 10 fish in each test jar. Two jars of each 1 evel , 10, 100, and 1000 mg/£
oWere observed for 80 hours. These jars were 1 liter and were not aerated during the test.
Tests C and D were replicates of each other using 10 liters of water and aeration. Statistically
meaningful deaths occurred only in the 1000 mg/£ test (TLgn 76 hours) in Test C above. During the
course of the test, one of the pregnant Gambusia gave birth to 3 young at between 80 and 90 hours
Uinto the test. These young were observed dead at 96 hours.
Fish selected without regard to sex.

�4. DISCUSSION

During the fish bioassay study, results were obtained over a moderately
wide range of toxicity. It must be remembered that these tests were conducted under laboratory conditions as static bioassays involving only two
species of fish. However, the results seem to indicate that in concentrations
of 100 mg/£ or greater, the illumination flare residue would prove to have
detrimental effects during 1-2 day exposures. Concentrations up to 50 mg/£
would probably have little permament effect during longer exposures.
Mortality data (Tables III to V), indicate that within the controlled
conditions (as outlined in the tables) of these tests, the fish were affected
depending on the type of water used. This evidence is augmented by the
findings during the water chemistry investigation, which indicate that the
limited buffering capacity of tap water affects the pH increase upon addition
of even minute amounts of the illumination flare residue.
The effect of this residue on the aquatic ecosystem is then largely
dependent not only on the type of water that it is deposited in but also
on the chemistry of that water. The chemical effect is, of course, a direct
result of the amount of the material added.

15

�SECTION VI
SOIL LEACHING STUDY

To determine the effects of illumination flare residue in the soil, (and
the mechanism of these effects) a laboratory experiment was designed and
implemented to duplicate a portion of the soil column.
1. METHODS AND MATERIALS

Soil samples were obtained from an area south of the Eg!in Environmental
Research Facility from a soil type closely resembling that of the flare test
areas. Several samples were collected from the natural soil column with a
2 inch core borer to a depth of 48 inches in 6 inch increments. All of the samples
from each increment were thoroughly mixed in a dry soil blender, and the soil
was added to an aluminum tube 4 inches in diameter and 56 inches high (Figure 1).
The soil was added to the tube in small increments and packed to approximate
natural conditions. Each level of the natural soil column was thereby represented
within the study apparatus.

Figure 1. Soil Leaching Tube Test
16

�Distilled water was then poured through the column to approximate packing
due to rainfall and allowed to dry. Sufficient illumination flare residue
(Sample Three) was then applied to equal 4,000 pounds per acre on the surface.
This rate is equal to high applications of agricultural lime, which would
Probably result in similar reactions.
A uniform amount of distilled water (205 ml) was then sprinkled evenly on
the top of the column daily for 54 days to simulate 1 inch of rainfall per
day.
Subsamples of the initial mixes and the soil in the column were taken at
0, 20, and 54 days and analyzed for magnesium and sodium content by atomic
absorption spectroscopy. Determinations of pH were made at 0 days and 54
days only. A replicate of the samples analyzed for Mg and Na were sent to the
University of Florida Soils Department for independent analysis.
2. ANALYTICAL TECHNIQUES FOR SOIL pH

Before pH determinations were made, all soil samples were dried at 50°C.
for 24 hours. Two separate methods were used to determine pH. Literature
reviews (Reference 2) indicate that use of distilled water introduces
variability.
METHOD ONE consisted of the dilution of 20 grams of premixed soil
with 80 ml of distilled water.
METHOD TWO consisted of the dilution of 50 grams of premixed soil with
100 ml of 0.01 M CaClr,. This method was employed following the recommendations
of Smiley and Cook (Reference 2).
All pH measurements were taken on a standard laboratory pH unit. Samples
were stirred for 2 minutes and allowed to equilibrate before the final reading
was recorded. Results of the pH determinations of the original control soil
and the subsamples from the soil leaching column are shown in Table VI.
3. ANALYTICAL TECHNIQUES FOR MAGNESIUM AND SODIUM DETERMINATIONS IN SOIL

To determine the actual concentrations of magnesium and sodium present in
the soil samples collected from the laboratory soil leaching study, soil
extractions were made, and analyses were performed to determine magnesium
and sodium as mg/kg of soil. Five grams of soil were extracted (Reference 3)
with 100 milliliters of one normal ammonium chloride (IN NH^l) for 6 hours
in 250 ml Nalgene bottles with mechanical shaking. The solutions were
filtered through Whatman #1 filter paper to remove suspended soil particles
from the extract. Before analysis, each sample was diluted as necessary to
be within the working range of the instrument (0.1 to 3 ppm).

17

�TABLE VI.

SOIL pH VALUES OF LEACHING EXPERIMENT

•

SOIL pH VALUE
!

1
:

SOIL COLUMN
DEPTH, inches

Surface
6
12
18
24
30
36
42

BEFORE ADDITION OF
PYROTECHNIC RESIDUE
5.7
5.7
4.9
5.1
5.3
5.8
5.8
6.1

54 DAYS AFTER ADDITION
OF PYROTECHNIC RESIDUE
8.6
6.5
5.1
5.5
5.4
5.4
5.5
5.8

!
,

Analysis for magnesium was performed by aspirating samples into a Jarre!Ash Model 82-500 Atomic Absorption Spectrophotometer on the absorbance mode
with a tri-flame burner. Operating conditions were: wavelength, 2851
Angstroms; lamp current, 10 milliamperes; fuel, hydrogen at 10 SCFH flow;
oxidant, compressed air at 15 SCFH flow, chart recorder range, 0 to 10
millivolts; average sample aspiration time, 5 seconds.
Analysis for sodium was performed by aspirating samples into the spectrophotometer while operating on the flame emission mode using the HETCO burner.
Operating conditions were: wavelength, 5890 Angstroms; fuel, hydrogen at 10
SCFH flow; oxidant, compressed air at 15 SCFH flow; chart recorder range
0 to 10 millivolts; average sample aspiration time, 5 seconds.
A standard curve was established for both elements from which the concentrations of the unknown samples were read. Standards were prepared by the
dilution of stock solutions of 1000 mg/l of Mg or Na atomic absorption
standards (HARLECO). The data were plotted as peak height (percent absorption)
versus concentration. The observed values of Mg and Na concentrations in the
soil samples are given in Table VII.
4. DISCUSSION

The results of the analyses for magnesium and sodium in the soil column
leaching study (Table VII) show that the illumination flare residue leaches
through the soil to a depth of only 12 inches. The analysis for magnesium
showed extremely high concentration levels (500 and 450 mg/kg) in the first
18

�TABLE VII. OBSERVED VALUES OF Mg AND Na CONCENTRATIONS IN SOIL LEACHING
STUDY
BEFORE ADDITION OF 20 DAYS AFTER ADDITION 54 DAYS AFTER ADDITION
SOIL COLUMN
DEPTH, inches PYROTECHNIC RESIDUE OF PYROTECHNIC RESIDUE 'OF PYROTECHNIC RESIDUE
Mg,mg/kg Na,mg/kg Mg,mg/kg
Na, rug/kg Mg,mg/kg
Na,mg/kg
P
Surface
5
25
500
26
450
20
23
6
2
28
2
26
I
30
12
1
1
24
28
23
2
18
1
1
1
25
27
30
1
1
24
23
30
|
1
25
1
1
1
28
30
27
28

j

36
42

1
1

1
1

23
21

24
28

1
1

21
23

«

level, which was to be expected since grains of the white illumination flare
residue were visible in the soil sample before extraction. A significant amount
leached into the second level (6 inches) after 54 days. Below 12 inches, there
was no increase in the magnesium concentration over that of the control soil.
The sodium concentration in the soil, however, after the illumination flare
residue had been added, remained approximately the same as the control soil.
Data obtained from the University of Florida Soils Department indicated the same
trends. Unpublished results from an experiment conducted by Harrison, Lander,
and Sigler ("Residual Levels of Sodium and Magnesium in Soil from Two Pyrotechnic
Tests Areas on Eglin AFB, Florida") indicate that the flare residue collected at
Eglin AFB had no sodium present, while that collected at the contractor's facility
did. The difference is apparently due to the method of collecting the residue.
At Eglin AFB, the flares were burned in an open area, and the residue was collected
on polyethylene sheeting. The wind dispersed the light material which could have
contained the sodium. At the contractor's facility all the residue was collected
within the test chamber.
The analytical technique was limited to approximately 90% accuracy due to
mixing, weighing, and extracting procedures. The atomic absorption instrumentation data itself were reproducible to 0.01 ppm.

19

�SECTION VII
CONCLUSION

Illumination flare residue appears to have a very low toxicity to mice,
plants, and fish. Concentrations above 100 mg/l of illumination flare
residue would likely have detrimental effects on indigenous fish populations
during a short term (1 to 2 day) exposure. Lower concentrations (10 to 50
mg/l ) appear to be relatively innocuous over longer periods (10 to 20 days)
of exposure. Mice were not affected by ingestion or skin contact and inhalation of the residue at relatively high concentrations. Plants were not
affected detrimentally at concentrations of 1000 Ib/acre in the soil or by
having the residue applied directly to the foliage. Germination of the
cucumber seeds were slightly affected at concentrations above 50 mg/kg in a
petri dish bioassay method. The concentrations required to cause any of the
above effects, however, are not likely to occur as a result of pyrotechnic
testing even after several years of testing over the same site.
Calculations from the data in this study indicate that the pH in a 4
hectare (10 acres) pond with an average depth of 3 meters (10 feet) would
be increased less than 0.1 unit if all the residue from 100 flares (15 pounds
is the approximate composition weight/flare or residue weight/100 flares)
fell into the pond and was evenly distributed. The concentration of pyrotechnic residue for this hypothetical case would be 2.27 mg/£.
The results from these studies indicate that the effects of illumination
flare residue are very minimal and are not particularly dangerous to the
environment in the concentrations used in these studies, which were selected
to represent the high range that would be found on a pyrotechnic test area.

20

�BIBLIOGRAPHY

1. The Merck Index of Chemicals and Drugs 7th Edition, Merck and Co., Inc.
Rahway, N. J., 1960.
2. R. W. Smiley and R. J. Cook. "Use and Abuse of the Soil pH Measurement."
Phytopathology. January 1972, Vol. 62, pp 193-194.
3. Analytical Methods for Atomic Absorption Spectrophotometry. Perkin
Elmer

21
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��INITIAL DISTRIBUTION
AFSC(DLW)
AFSC (SDWM)
AFSC (VN/Col F. Smith)
AFSC (LO/Code 143 Maj Brown)
USAF(RDPA)
USAF (PREU/Col Bell)
ASD (ENYS/Mr Hartley)
AMRL/HEF Maj Hilgendot
AMD (Maj David Beatty)
SAMTEC (Col Borgstrom)
SAMSO (SG/Maj W. D. Tuttle)
AUL LSE-70-239
USAF Env Health Lab (CC)
Naval Ammo Depot (Code 501)
Edgewood Arsnl (SMUEA-SA)
USNWC (Code 753 Tech Lib)
USNWC (Code 4541)
Picatinny Arsnl (SMUPA-AD-D-R-4)
Picatinny Arsnl (SMUPA-FR/L. Eriksen)
USNWL (Code FCV)
Ft Detrick Veg Control Div (Dr Darrow)
NASC(AIR 5323)
DDC
PACAF (IGY)
ADTC(DEN)
ADTC (DEEE/Dr Pierce)
ADTC (SGPA/Maj Conrad)
AFATL(DL)
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AFATL(DLI)
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TRADOC/ADTC DO

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23
(The reverse of this page is blank)

��UNCLASSIFIED
Security Classification

DOCUMENT CONTROL DATA - R &amp; D
{Security &lt; ?as sificatiort of title, body of absTretciand indexing annotation m u s t be entered when the overall report is
O R I G I N A T I N G A C T I V I T Y (Corporate author)

Unclassified

Flame, Incendiary, and Explosives Division
Air Force Armament Laboratory
Eglin Air Force Base. Florida 32542
_
-j

classified)

*2a. R E P O R T S E C U R I T Y C L A S S I F I C A T I O N

26. GROUP

REPORT TITLE

STUDIES TO DETERMINE THE ENVIRONMENTAL EFFECTS OF ILLUMINATING FLARE
RESIDUE
A

D E S C R I P T I V E N O T E S (Type ol repott and inclusive dates)

Final Report (November 1971 - September 1972)
Bobby M. Agerton
Don D. Harrison
John W. Sigler, 2Lt, USAF , Stephen W. Lander, Jr, 2Lt, USAF
A U T H O R i S i (First name, middle initial, last name)

REPORT DATE

7a. T O T A L M O

November 1972
8S. C O N T R A C T O R

G R A N T NO,

6- P R O J E C T NO

5066 01 01

OF P A G E S

176, NO OF R E F S

3

28
*9. O R I G I N A T O R ' S R E P O R T NUMBER(S)

AFATL-TR-72-204
9fc. O T H E R R E P O R T NO(St (Any other numbers that may 6e&gt; assigned
this report)

t O . D t S T R i 8UT1ON S T A T EMENT

Approved for public release; distribution unlimited.

M - S U P P L E M E N T A R Y NOTES

Available in DDC

1 2 - SPONSORING M I L I T A R Y A C T I V I T Y

Air Force Armament Laboratory
Air Force Systems Command
Eglin Air Force Base, Florida 32542

3. A SS TR AC T

In conjunction with the illuminating flare test and evaluation program on Eglin
AFB Reservation, a project was initiated to determine the effect of the flare
testing on the flora and fauna on the test areas. The results from normal testing
demonstrate that the residue of illuminating flares is not toxic to representative
species.

DD ,

UNCLASSIFIED
Security Classification

�UNCLASSIFIED
Security Classification
1 4.

LINK A
KEY

LINKS

ROLE

WT

ROL E

W T

Illuminating Flare
Test and Evaluation
Residue
Effects
:

LINK' C

WORDS

lora and Fauna

Environmental
Ecology

UNCI Security Classification
ASSTFIED

ROL E

WT

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