YELLOW RAIN-ANALYSIS EVALUATION OF RICE AND LEAF CONTROL SAMPLES- ANALYSIS EVALUATION OF DARK LIQUID REPORT DATE 841029 ALSO ATTACHED

• Document Type: FOIA
• Collection: FOIA Collection
• Document Number (FOIA) /ESDN (CREST): 00037497
• Release Decision: RIFPUB
• Original Classification: U
• Document Page Count: 4
• Document Creation Date: December 28, 2022
• Document Release Date: September 26, 2017
• Case Number: F-2012-01432
• Publication Date: September 20, 1984

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ANALyTioutrommvisioN
RESEARCH DIRECTORATE
20 September 1984
Analysis/Evaluation of Rice and Leaf Control Samples
A shipment designated 10027R(4) was received by the Analytical Research
Division, 15 December 1983, from FSTC. The three samples included in the
shipment were identified as reference materials. Each was containerized
in a separate plastic bag. One sample identified with LA8310XX-5RP,
designated 10027R(4)-1, consisted of approximately one cup of glutinous
rice grown and milled in 19831Figure 1). The second sample, identified
with 1A8310XX-6RP, designated 10027R(4)-2, consisted of approximately one
cup of non-glutinous rice grown and milled in 1983 (Figure 1). The third
sample, identified with LA831113-4WT, designated 10027R(4)-3, consisted of
a yellow spotted fig leaf (Figure 1).
A separate vapor sample withdrawn from within each enclosure was subjected
to analysis by gas chromatography/mass spectrometry(GC/MS). A portion of each
sample was extracted with 1:1 methanol :water. The solvent solubles were
analyzed by GC/MS, ion chromatography (IC), thin layer chromatography (TLC)
and infrared spectrometry (IR).
10027R(4)-1 (LA8310XX-5RP) Glutinous rice
The GC/MS spectra of the vapor associated with the rice identified the
presence of benzene, toluene, xylene, branched aliphatic hydrocarbons
(bp 110-160�C), o-cresol, dimethylphenol, methyl benzoate and possibly
benzoic acid hydride. The GC/MS spectra of the chloroform solubles was
similar to that of rubber. IC separated no ions of interest. Two components
were separated by TLC. One, which remained at the origin, fluoresced under
UV light. The other was identical to a component detected in the 100271(4)-1
reference rice samples, Rf 0.37-0.46 giving a purple reaction product with
p-anisaldehyde. Derivatization with negative ion chemical ionization MS
detection gave negative results for trichothecenes. IR spectra identified
the presence of aliphatic hydrocarbons and two carbonyl bands at 1740 and
1706 cm-1.
10017R(4)-2 (LA8310XX-6RP) non- glutinous rice
The analysis data were similar to those of the glutinous rice, with a
few exceptions. The GC/MS spectra of the vapor associated with the rice
identified the presence of xylene, branched aliphatic hydrocarbons
(bp 110-160�C) and methyl benzoate. The chloroform solubles did not give
definitive GC/MS spectra. The IC, TLC and derivatization/MS analysis results
were identical with those of the glutenous rice. IR spectra identified the
presence of high concentrations of aliphatic hydrocarbons, lesser quantities
of aromatic Cefins, 2 carbonyls with bands at 1742 and 1711 0m-1
could be present as an acid ester.
CIA
Declassify: OADR
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10027R(4)-3 (LA831113-4WT) fig leaf pieces
The GC/M5 spectra of the vapor associated with the leaf pieces identified
the presence of xylene, benzaldehyde, phenol,benzonitrile acetophenone
and methyl benzoate. The chloroform solubles did not give definitive
GC/MS spectra. IC separated no ions of interest. TLC separated two components
at Rf 0 and 0.77-0.83 which fluoresced under UV light. No reaction with
p-anisaldehyde was detected. Derivatization with negative ion chemical
ionization M5 detection was negative for trichothecenes. IR spectra identi-
fied the presence of wateri aliphatic hydrocarbons, with two weak carbonyl
bands at 1733 and 1715 cm-4.
Conclusion:
No evidence of any known CW agent, agent degradation product or
trichothecene was detected. The similarity of the analysis data from the two
rice samples was as expected. The slight differences indicate definitive
analyses for the two different types of rice. Each of the samples appeared
to be innocuous and gave excellent, reproducible base line analyses for
reference data.
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Analytical Research Division
Research Directorate ,
29 Oct 84
Analysis/Evaluation of Dark Liquid
A shipment designated.,10027QQQQ was received by the
Analytical Research Dirlaion, 14 December 1983, from FSTC.
The sample WBS also Identified with the number TH
831117-2XX. The rhipment consisted of approximately 4 oz.
of a dark amber liquid containerized in a screw top glass
jar. There was no information available concerning the
B ample.
A vapor sample withdrawn from within the glass bottle
WBS subjected to analysis by gas chromatography/mass
spectrometry (CC/MS.). The neat liquid was analyzed by
Gc-ms, thin layer chromatography AILC1, and infrared
spectrometry(1R).
The CC/MS spectra of the vapor associated with the
liquid identified the presence of 2 isomers of cresol as the
major components, and toluene, xyiene, phenol, ttwo isomers
of dimethyl phenol naphthalene and methyl naphthalene as
minor components. The GC/MS spectra of the neat liquid
identified the presence of a complex mixture. The major
component was phenol. Minor components identified included
toluene, xylenes, thiophenol, two cresols, a series of
substituted phenols, thymol and dimethylbenzaldehyde. TLC
yielded a smear from which components could not be
separated. IR spectre Identified both aromatic and
aliphatic hydrocarbons, carbonyl and OH bonds typical of
phenol, and p-mono or disubstitution.
Conclusions
No evidence of any known CW agents, agent degradation
products, or trichothecenes was detected. The liquid
appears to be an industrial grade of phenol.
Classified b : CIA
Declassify: CADR
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