YELLOW RAIN-ANALYSIS EVALUATION OF METAL FRAGMENTS AND GLOVES

• Document Type: FOIA
• Collection: FOIA Collection
• Document Number (FOIA) /ESDN (CREST): 00037511
• Release Decision: RIFPUB
• Original Classification: U
• Document Page Count: 6
• Document Creation Date: December 28, 2022
• Document Release Date: September 26, 2017
• Case Number: F-2012-01432
• Publication Date: April 5, 1985

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Analytical Division
Research Directorate .
Analysis/Evaluation of Metal Fragments and Cloves
A shipment designated 10027C(6), received by the Analytical Division
5 Apr 85 from FSTC, contained twenty-two subsamples. A group of samples
identified by the SEA team as of prime interest and all related to
suspect chemical munitions were evaluated concurrently. These consist of
a threaded metal piece identified with CB 850215-004U, figure 1, several
solid chunks which appear metallic identified with CE65D215-002/2KA,
figure 1, a second group of similar solid chunks identified with
CBE50215-002/3KA, figure 1, a third group of similar solid chunks
identified with CB850215-002/1KA, figure 1, dark brown granules
identified with CE650215-002XA, figure 2 and a pair of surgeons gloves
reportedly used in taking and separating these samples identified with
CB650215-003SW, figure 3. Subshipment designations for these samples
are: 10027C(6)-5, 10027C(6)-6, 10027C(6)-7, 10027C(6)-E, 10027C(6)-9, act
10027C(6 -11 respectivel- . Each sam le was contained in a glass jar.
sealed, Vapor samples withdrawn from
within eac sam e jar enclosure we su jected to analysis by gas
chromatography/mass spectrometry (GC/MS). Portions of each sample were
either swabbed or leached with chloroform. Additional portions of each
sample were treated similarly with 1:1 methanol:water. The solvent
soluble materiala were analyzed by GC/MS, ion chromatography (IC), thin
layer chromatography (TIC) and infrared spectrometry (IR).
Sample 10027C(6)-5 (Metal. Piece) (CB850215-004XA)
This sample was subjected to swabbing with solvents. The GC/MS
spectra of the vapor associated with the sample identified the presence
of acetone, rylene, naphthalene, methyl naphthalene, biphenyl and a
terpene similar to cadinene. GC/MS analysis of the chloroform solubles
identified only an alcohol, possibly a glycol. No detectable ions were
separated by IC. No separation of any detectable compounds was evident
by TLC. IR identified the presence of water, aliphatic hydrocarbons, a
carbonyl band at 1736 cm-I, nitrite NO2, and inorganic silica, SiO2.
Derivatization with negative ion chemical ionization MS detection was
negative for trichothecenes.
10027C(6)-6 (Large Solid Chunks) (CB850215-002/2XA)
A chunk having white, yellow and black surface colorations was
leached in chloroform. Another chunk having rust and black surface
colorations was leilached in 1:1 methanol:water. Upon covering the solid
with methanol/water, a degassing was observed, suggesting that the
material contained either pores of a size which permitted the solvent to
displace air in them or an acid salt which liberated a gas on solution,
eg. a carbonate giving CO2. The GC/MS spectra of the vapors associateo
with the sample identified the presence of acetone,
'7
Classified by: CIA
OADR
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trichlorofluorocethane, chloroform, triethylamine,-toluene,
chlorubenzene, two isomers of natrotoluene, a sesquiterpeoe, naphthalene,
diphenylamape, E-hydroutoluene and au unidentified aliphatic
hydrocarbon. Analysis of the chloroform eolubles by CC/MB identified the
major component as TNT. IC separated no detectable ions. TLC separated
two UV absorbers at Ef 0.75-0.80 and 0.81-0.85, supportive of aromatic
nitrocompounds. IR analysis identified TNT as the major component with
smaller quantities of an aliphatic hydrocarbon, possibly a paraffin wax.
Derivatizatlon with negative ion chemical iocizatioo SS detection for
trichothecenes was negative.
100277(6)-7 (Large Solid Chunks) (CB850215-002/3XA)
Chunks similar to those described in 10027C(6)-6 were -subjected to
the same solvent leaches. A degassing phenomenon similar to that in
10027C(6)-6 was observed in the methanol-water leach. The GC/MS spectra
of the vapor associated with the sample identified the presence of
acetone, trichlorofluoromethane, either.trimethyl benzene or propyl
benzene, aliphatic hydrocarbons, naphthalene and one sesquiterpene G1511 24
Analysis of the chloroform solubles by GC/MS identified toluene as tbe
major component, with lesser quantities of TNT arid traces of butanol and
benzaldehrie. No detectable ions were separated by IC. TLC separated
two UV absorbers similar to those detected in 10027C(6)-6, having
Rf=0.72-0.82 and 0.81-0.82. IR analysis identified the presence of TNT
and hydrocarbons. Derivatization with negative ion chemical ionization
NE detection for trichothecenes was negative.
10027C1:6)-8 (Large Solid Chunks) (CB850215-002/1XA)
A chunk having white and black surface colorations was leached in
chloroform. Other chunks having white, black and red surface colorations
were leached in 1:1 methanol:water. A degassing phenomenon similar to
those of the previous two samples was observed in the methanol-water
leach. GC/MS spectra of the vapor associated with the sample identified
the presence of acetone, rylene, ethyl toluene or propyl benzene,
naphthalene, natrotoluene, a sesquiterpene C1A4and diphenyl. Analysis
of the chlorofora solubles by GC/MS identified TNT as the major
component, with a trace of toluene. No detectable ions were separated by
IC. TLC separated the same UV absorbers detected in 10C27C(6)-7. IR
identified the presence of TNT. Derivatization with negative ion
chemical ionization XS detection for trichothecenes was negative.
10027C(6)-9 (Dark Brown Granules) (CB 850215-002XA)
A few granules were leached in chloroform. Another portion of
granules were leached in 1:1 methanol:water. The GC/MS spectra of the
vapor associated with the sample identified the presence of acetone,
trichlorofluoromethane, rylene, either diethyl benzene or tetramethyl
benzene, naaphthalenes, methyl naphthalenes, several aliphatic
hydrocarbons and 4 or 5 sesquiterpenes, each C15F64. Analysis of the
chloroform solubles by GC/MS identified toluene, TNT and an alcohol. No
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detectable ions were separated by IC. TLC separated only one component,
a UV absorber at Rf 0.76-0.84 similar to one of the compcpents detected
in samples 10027C(6)-6,7 and 8. IR identified the presence of aliphatic
hydrocarbons, aromatic nitrates, TNT and silicates which appear to be
sand from the environment. Derivatization with negative ion chemical
ionization MS detection for trichothecenes was negative.
10027.7(6)-11 (Surp_eon's Gloves) (CB850215-0071)
The blackened area of two fingers were cut out. One was leached in
chloroform, the other in 1:1 water:methanol. The GC/MS of the vapor
associated with the gloves identified the presence of acetone, a compound
similar to C10H1802' B-hydroxy toluene (BHT) and dehydro BHT. GC/MS
spectra of the chloroform solubles identiried toluene, BHT 4nd
1,1,3-trimethy1-3 pbenylindene. No detectable ions were separated by IC.
TLC separated one component, identical with that detected in sample
10027C(6)-9. IR spectra identified the presence of high concentrations
of hydrocarbons, possible aromatic structures, a C-0 band and C=0 band
(1745 cm-1), with no evidence of nitrocompounds. Derivatization with
negative ion chemical ionization MS detection for trichothecenes was
negative.
Conclusion:
No evidence of any known CW agent, agent degradation product or
trichotbecene was detected. The primary component of each of these
samples was TNT and structures normally associated. with it in a munition
propellant. The detection of sesquiterpenes in several samples could be
indicative of either a natural contamination of the samples or inclusions
Of a natural product, eg. trichothecenes, in the munition fill. As
evidenced from the photographs, it is difficult to determine the source
Of the terpene structures.
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