YELLOW RAIN-ANALYSIS EVALUATION OF BROWN POWDERS

• Document Type: FOIA
• Collection: FOIA Collection
• Document Number (FOIA) /ESDN (CREST): 00037492
• Release Decision: RIFPUB
• Original Classification: U
• Document Page Count: 3
• Document Creation Date: December 28, 2022
• Document Release Date: September 26, 2017
• Case Number: F-2012-01432
• Publication Date: August 21, 1984

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ANALYTICAL RESEARCH DIVISION
RESEARCH DIRECTORATE
21 August 1984
Analysis/Evaluation of Brown Powders
A shipment designated 10027222 also identified with TH830513-3701, was
received by the Analytical Resatkrch Division 3 June 1983 from FSTC. The
shipment coniisted of one light brown powder and one dark brown powder,
each containerized in individual rubber septum ca ed :ass vials fi
CD t. b
e ight brown powder
was esigna e 272ZZ- an dark rown powder was des-ignated 100272ZZ-2.
Vapor samples withdrawn from within each vial were subjected to analysis
by gas chromatography/mass spectrometry (GC/MS). A portion of each powder
was extracted with chloroform. Another portion of each powder was extracted
with 1:1 methanol:water. The solvent extracts were analyzed by GC/MS,
ion chromatography (IC), thin layer chromatography (TLC) and infrared
spectrometry (I10. The neat powders were also evaluated by scanning electron
microscopy (SEM).
10027222-1 lit-it brown powder
The GC/MS analysis of the vapor associated with the powder contained no
definitive mass spectra. The GC/MS spectra of the chloroform solubles
identified the presence of trinitrotoluene (TNT), hexamethylene tetramine,
aliphatic hydrocarbons from C23 to C,6 and a base peak M/z = 75, 116, 179,
168, 179 which could be nitronaphthatene. Ion chromatography separated
and quantitated the presence of 1 ppm fluoride and a possible trace of cyanide. TLC
separated a UV absorber at Rf 0.8. Reaction of the developed TLC plate for
alkyIating agents gave a purple product at Rf 0.4 and 0.8. Derivatization with
negative ion chemical ionization MS detection for trichoahecenes was negative.- IR
analysis identified the presence of aliphatic hydrocarbons and aromatic
nitrates, primarily TNT. SEM evaluation showed the neat material was a
granular, partially crystalline solid.
1002722Z-2 dark brown solid
The GC/MS spectra of the vapor associated with the powder identified
the presence of diethyleneglycol mono ethylether and 2,6,-di-t-buty1-4-
ethenylphenol as the major components and benzene, benzaldehyde, toluene,
xylene, ronanol and 2,4-di-t-buty-4-ethylphenol as minor components. The
GC/MS analysis of the chloroform solubles identified the major component
as TNT and dinitrotoluene the minor component. Ion chromatography
separated and quantitated 0.5 ppm fluoride and a possible trace of cyanide.
TLC separated one component, a UV absorber at Rf 0.60-0.82 which reacted
with p-anisaldehyde reagent to give a beige color. Derivatization with
negative ion chemical ionization MS detection for trichothecenes was negative.
The IR specfra identified the presence of aromatic nitrates, primarily TNT. SEM
evaluation showed the neat solid was a granular, partially crystalline material,
nearly identical to the 10027222-1 sample.
lassified by; CIA
nprlaccifv: OADR
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Both powders were determined to be primarily TNT. The lighter colored
powder, 100272ZZ-1, appeared to be relatively pure. The darker powder,
10027ZZZ-2, appeared to contain solvents and manufacturing impurities.
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