YELLOW RAIN-ANALYSIS EVALUATION OF WHITE POWDERS-ANALYSIS EVALUATION OF PAPER DATE 841106

Document Type: 
Collection: 
Document Number (FOIA) /ESDN (CREST): 
00037505
Release Decision: 
RIFPUB
Original Classification: 
U
Document Page Count: 
6
Document Creation Date: 
December 28, 2022
Document Release Date: 
September 26, 2017
Sequence Number: 
Case Number: 
F-2012-01432
Publication Date: 
November 19, 1984
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PDF icon YELLOW RAIN-ANALYSIS EVAL[13984481].pdf162.82 KB
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�o� Approved for Release: 2015/01/05 000037505 alytical Research DiVi5i0i Research Directorate Analysis/Evaluation of White Powders 6,1 , 19 Nov 84 A shipment designated 10027PPPP was received by the Analytical Research Division 13 December 1983 from FSTC. The shipment was identified with TH831117-1XX. No identification was made, of the four subsamples. No information was available concerning the samples. Subsamples 10027PPPP-1 and -2 consisted of white powders, each individually containerized in plastic bags. 10027PPPP-1 weighed approximately 200 g and 10027PPPP-2 weighed approximately 50 g. (Figure 1). A spot report has previously been issued on these samples. Vapor samples withdrawn from within each bag of powder were subjected to analysis by gas chromatography/mass spectrometry (GC/MS). Portions of each powder sample leached in chloroform formed a gel. Portions leached in 1:1 methanol:water did not gel. The solvent soluble materials were analyzed by GC/MS, ion chromatography (IC), thin layer chromatography (TLC), and infrared spectrometry(IR). Portions of each neat powder were analyzed by Atomic Absorption spectroscopy (AA). 10027PPPP-1 The GC/MS spectra of the vapor associated with the powder identified the major components as hexanoic acid and heptanoic acid. Minor components detected included octanoic acid, methyl naphthalene, toluene, benzaldehyde and t-butyl-isobutyl hydroxytoluene. The GC/MS spectra of the chloroform solubles identified the presence of propanoic, pentanoic, hexanoic and octanoic acids, their aldehydes, and aliphatic hydrocarbons from C25 to C30. IC was negative for all ions. No components were separated by TLC. Derivatization with negative ion chemical ionization MS detection for trichothcenes was negative. IR spectra identified the presence of the aluminum salts of hexanoic and octanoic acids. Elemental analysis by AA detected 7.89$ aluminum. Classified b : CIA Declassify: OADR Approved for Release: 2015/01/05 000037505E412T L / .40 Approved for Release: 2015/01/05 000037505 b 10027PPPP-2 The GC/MS spectra of the vapors associated with the powder identified only traces of xylenes. The GC/MS spectra of the ch3oroform solubles identified .the presence of hexanoic and octanoic acids. IC detected no ions. No components were separated by TLC. Derivatization with negative ion chemical ionization MS detection for trichothecenes was negative. IR spectra identified the presence of the aluminum salts of hexanoic and octanoic acids Elemental analysis by AA detected 8.75S aluminum. Conclusions No evidence of any known CW agents, agent degradation products, or trichothecenes was detected. The detection of hexanoic, heptanoic and octanoic acids and related compounds with approximately 8% aluminum agrees with the-formulation of the M-4 thickener for Napalm. Each of these powders is a diacid aluminum soap of octanoic acids used in the M-4 formulation. Approved for Release: 2015/01/05 000037505 Approved for Release: 2015/01/05 000037505 wtcter 0 0 .11 Approved for Release: 2015/01/05 000037505 Approved for Release: 2015/01/05 000037505 Analytical Research Division Research Directorate 06 Nov 84 Analysis/Evaluation of Paper A shipment designated 10027PPPP was received by the Analyti,-al Research Division 13 December 1983 from FSTC The shipment was identifiecl with TH831117-1XX. No identificationwas made 'of the four subsamples. No Information Was available concerning the samples. Subsamples 10027PPPP-1 and -2 have previously been identified and reported. Samples 10027PPPP-3 and -4 each consisted of paper containerized in a wide mouth screw top glass jar. 10027PPPP-3 was shredded paper,-4 was -e folded piece of paper with Thai writing on it (Figure 1). Vapor samples withdrawn from within each jar containing paper were subjected to analysis by gas chromatography/mass spectrometry (GC/MS). Portions of each _paper sample were leached in chloroform. Other portions of each were leached in 1:1 methanol:water. The solvent soluble materials were analyzed by GC/M51 ion chromatography (1C), thin layer Chromatography (TLC), and infrared spectrometry(1R). 10027PPPP-3 The GC/MS spectra of the vapor associated with the paper Identified the major components as o-creso: and three isomers of dimethyl phenol. Minor components detected included benzaldehyde, phenol, benzonitrtle, methyl heptanoate, p-cresol, aceLophenone, methyl benzoate and methyl octanoate. The chloroform soluble materials did not give a definitive GC/MS spectra. IC was negative for all ions. No components were separated by TLC. Derivatization with negative ion chemical ionization MS detection for trichothcenes was negative. IR spectra identified the presence of aliphatic hydrocarbons, a carbonyl at 1720 cm-1, and possibly pctassium nitrate, C-00 cellulose and inorganic Si licate. pproved for Release: 2015/01/05 000037505 Approved for Release: 2015/01/05 000037505 10027PPPP- 4 The CC/ M'i pee,�1, of the vapors associated with the folded papers ide..ntafied methyl hexinorte as the major component. Mino: components detected included hexane nitrile, acetic acid, furanccrboxaldehyde (2-fura1dehydc), ethyl ether, xytene and possibly ethyl hexanoate. The chloroform soluble, did not give a definitive GC/MS �pectrs. IC detected co ions. No components were sepn71110iv TLC. Derivatization with negative ion chemi....e! detection for trichothecenes was negc.;... identified the presen.c.e, of alipha, a carbonyl and possibly C-0: Conclusions No evidence of any known CW agents, t_gradation products, or trichothecenes was detected. the detection of hexanoic, heptanoic and octanoic acid esters could be related to :he identification of 10027PPPP-1 and -2 as diacid aluminum soaps of octanoic acids. it is possible that the papers were in contact with the other two samples. without any information about the samples, no further conclusions can be drawn from the analyses. Page 2 Approved for Release: 2015/01/05 000037505 Approved for Release: 2015/01/05 000037505 � .1 Approved for Release: 2015/01/05 000037505