YELLOW RAIN-ANALYSIS EVALUATION OF YELLOW POWDER

• Document Type: FOIA
• Collection: FOIA Collection
• Document Number (FOIA) /ESDN (CREST): 00037494
• 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: September 18, 1984

Approved for Release: 2015/01/05 000037494
ANALYTICAL RESEARCH DIVISIOU
RESEARCH DIRECTORATE
18 September 1984
Analysis/Evaluation of Yellow Powder
A shipment designated 10027A(4), also identified with Tii830513-38DL,
was received by the Analytical Research Division, 3 June 1983, from FSTC.
Information concerning th2 sample indicatad it could be the residue from a
chemical attack. The sample consisted of approximately Sang of a yellow
powder containerized in a glass vial fitted with a rubber septum closure
(Figure 1).
A vapor sample withdrawn from within the glass tube was analyzed by
gas chromatography/mass spectrometry (GC/MS). A portion of the powder
was extracted with chloroform. Another portion was extracted with
1:1 methanol:water. The solvent extracts were subjectee to analysis by
GC/MS, ion chromatography (IC), thin layer chromatography (TLC) and infrared
spectrometry (IR). In addition, a portion of the neat powder was examined
by scanning electron microscopy (SEii).
The GC/MS spectra of the vapor associated with the powder identified
the presence of the solvents toluene and xylene. The GC/!S spectra of the
chloroform solybles detected a series of aliphiztic hydrocarbons, C23. C25,
C27, C29, C31 with the C25and C27 having the highest concentration. This
is similar to the spectra of beeswax. In addition, pentanol and cyclopropyl
methylketone were detected. Ion chromatography detected 9 ppm fluoride and
possible traces of cyanide. Thin layer chrematogrephy separated two
components which reacted with the detection reagent for alkylating agents
to yield purple spots at Rf 0.28 to 0.36 and 0.00 to 0.84. Known beeswax gave
a similar reaction at Rf .80 to .84. A reference rice sample gave a similar
reaction at approximately the same Rf as the 0.28 to 0.36 component.
Derivatization with negative ion chemical ionization, MS detection was
negative for trichothecenes. Gas chromatography gave a separation of
components with retention times identical to those of beeswax. IR spectra
identified the presence of aliphatic hydrocarbons, two carbonyl bands at
1735 and 1710 cm-1, possible aromatics and esters. The SEM examination
(Figure 2) showel the powder consisted of tightly packed clumps of pollen.
Five different pollen species were detected. Each pollen species had been
detected in one or more previous samples.
Conclusion.
No evidence of any known CU agent, agent degradation product or
trichothecene was detected. The various analyses suggest the major components
are pollen and beeswax. Although this combination could be indicative
of bee feces, the detection of (1) trace levels of fluoride. (2) an unidenti-
fied alkylating agent not a component of beeswax or bee feces, and (3) five
species of pollen rather than one or two species normally found in bee
feces suggest another, at present, unidentified source.
lassified by: CI
eclassify: OADR
A/4!
. Approved for Release: 2015/01/05 000037494
Approved for Release: 2015/01/05 000037494
I ir
---
Approved for Release: 2015/01/05 000037494
17617L�0000 90/1-0/91-0Z :eseeIej -104 panaiddV
Z 3tIfIDIJ
(17)1/000t
MATE- "- e."."11M.111. t'-',.`r7 79, "�;#747,.. � . �
s �
1 �
�
�
���� �
17617L�0000 90/1-0/91-0Z :eseeIeI -104 panaiddV