YELLOW RAIN-ANALYSIS EVALUATION OF LEAF-ALSO ATTACHED ARE: ANALYSIS EVALUATION OF VEGETATION AND STONE SAMPLES DATED 840921-ANALYSIS EVALUATION OF YELLOW POWDER DATED 840919-EVALUATION OF LEAVES DATED 840919-

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Document Number (FOIA) /ESDN (CREST): 
00037504
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RIFPUB
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U
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9
Document Creation Date: 
December 28, 2022
Document Release Date: 
September 26, 2017
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Case Number: 
F-2012-01432
Publication Date: 
November 2, 1984
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Approved for Release: 2015/01/05 000037504 Anglytical Research Division Research Directorate 02 Nov $4 Analysis/Evaluation of Leaf A shipment designated 16,027222Z-10 was received by the Analytical Research Division, 23 February 1984, from FSTC. The sample was also identified with the TH number 840209-10DL. The shipment_gonsisted of a single leaf having a 2 mm yellow spot and coniainerized in a plastic bag. No further information was available about the sample. A vapor sample withdrawn from within the plastic bag containing the leaf was subjected to analysis by gas chromatography/mass spectrometry (CC/MS). A portion of the spnt was leached with chloroform. Another portion was leached in 1:1 methanol:water. The solvent soluble materials were analyzed by GC/MS, ion chromatography (IC), thin layer chromatography (TLC), and Infrared spectrometry (IR). The GC/VS spectra of the vapors associated with the loaf identified the presence of dimethyl phenyl indine. The chloroform sclubles did not give a definitive GC/MS spectra. IC was neg3tive for all ions of interest. TLC separated a UV flourescent compound, Rf=.75, and a red colored component, Rf=.80. These separations are similar to those given by reference vegetation samples. Derivatization with negative icn chemical ionization MS detection for trichothcenes was negative. IR spectra identified the presence of aliphatic hydrocarbons and traces of indefinitive components. Conclusions No evidence of any known CW agents, agent degradation products, cr trichothecenes was detected. The sample appears to be innocuous. :assify Decla.sfIfy: OA DR Approved for Release: 2015/01/05 000037504 EWO 1- a Approved for Release: 2015/01/05 000037504 , .f ANALYTICAL RESEARCH DIVISION RESEARCH DIRECTORATE . 21 September 1984 Analysis/Evaluation of Vegetation and Stone Samples A shipment designated 100271(4) was received by the Analytical Research Division, 28 February, 4984, from FSTC. The analysis of five samples, 100271(4)-1 (TH840209-100, 100271(4)-4 (TH840209-401), 100271(4)-5 (TH840209-500, 100271(4)-6 (1H840209-600 and 100271(4)-7 (TH840209-7DL), have been previously reported. Additional analysis have been completed on three samples. These include a small stone with one yellow spot two mm in diameter containerized in a plastic bag identified with TH840209-301. and designated 100271(4)-3, two leaves with white and rust spots from one to nine mm in diameter. containerized in a plastic bag identified with TH840209-901_ and designated 100271(4)-9 (Figure 1) and one leaf with one yellow spot containerized in a plastic bag identified with TH840208-1LP and designated 100271(4)-12 (Figure 1). No further information was available on these samples. A separate vapor sample withdrawn from within each plastic bag was sub- jected to analysis by gas chromatography/mass spectrometry (GC/MS). A portion of each sample was extracted with chloroform. Another portion of each was extracted with 1:1 methanol:water. The solvent soluble materials were analyzed by GC/MS, ion aromatography (IC), thin layer chromatography (TLC) and infrared spectrometry (IR). 100271(4)-3 (TH640209-301) stone The GC/MS spectra of the vapor associated with the stone identified the presence of Otrimethyl phenylindene. The GC/MS analysis of the chloroform solubles gave no definitive spectra. IC separated no ions of interest. No detectable components were separated by TLC. Derivatization with negative ion chemical ionization 115 detection was negative for trichothecenes. IR spectra- identified a trace of aliphatic hydrocarbon and a silicate possibly soil. 100271(4)-9 (TH840209-901) two leaves The GC/M5 spectra of the vapor associated with the leaves identified ithe presence of 2.3 dihydro, 1.1,3-trimethy1-3-phenyl-11-1 indene Chloroform solubles from each of the leaves gave no definitive GC/MS spectra. IC detected no ions of interest from either leaf. TLC detected two components from the small leave with yellow spots, a UV fluorescent component, RF 0.77-0.83, and another reacting with the p-anisaldehyde reagent to give a red spot at Rf 0.83-0.88. Only one component was detected from the large leaf with rust spots, a UV fluorescent material. Rf 0.73-0.79. Derivatization with negative ion chemical ionization MS detection was negative for trichothecenes in both leaves. IR spectra related to the small leaf identified the presence of aliphatic hydrocarbons and a band at 1610 cm-1, tentatively identified as Classified CIA CApproved for Release: 2015/01/05 CO0037504 Approved for Release: 2015/01/05 000037504 a carboxylic acid salt. IR spectra related to the large leaf identified the presence of aliphatic hydrocarbons and a carbonyl band at 1720 cm-1. 100277(4)-12 (TH840208-1LP) one leaf The GC/MS spectra of the vapor associated with the leaf identified the presence of a compound similar to hydroxytoluene, having a di-t-butyl group with one unsaturation. The GC/MS spectra of the chloroform solubles identified the presence of phthalates and six high boiling aliphatic hydro- carbons, bp 250" - 290', > C36. IC Kis negative for all ions of interest. TLC separated one component, which yielded apurple spot Rf 0.1-0.15 on reaction with p-anisaldehyde. Derivatization with negative ion chemical ionizatIon M5 detection for trichothecenes was negative. IR spectra identified the presence of aliphatic hydrocarbons, carbonyl and CO. Conclusions No evidence of any known CW agents, agent degradation products or trichothecenes was detected. The significance of the detection of trimethyl- phenyl indene in two of the samples is not evident at this time. The samples appear to be innocuous. 2 Approved for Release: 2015/01/05 000037504 Approved for Release: 2015/01/05 000037504 A pproved pproved for Release: 2015/01/05 000037504 Approved for Release: 2015/01/05 000037504 ANALYTICAL RESEARCH DIVISION RESEARCH DIRECTORATE Analysis/Evaluation of Yellow Powder A shipment designated 1002744), recPi Division, 23 February 1984, from FSTC, container identified with TH84020-11. - It consisted of a 4 oz wide mouth' (Figure 1) which reportedly conta: � scraped from rocks. 19 September 1984 Analytical Resz..arch _packages. One q/02744)-1. !..c1 glass jar yellow spots A vapor sample withdrawn fro , subjected to analysis by gas chromatography/mass spectrot !, portion of the powder was extracted with chloroform. Anotlii- or the powder was extracted with 1:1 methanol :water. The solvent soluble materials wely analyzed by GC/MS, ion chromatography (IC), thin layer chromatography (TIC) and infrared svztrometry (IR). The GC/MS analysis of the vapors associated with the powder gave no definitive spectra. The GC/MS spectra of the chloroform solubles showed only a possible trace of chloro compounds. IC separated no compounds of interest. No detectable components were separated by TLC. Derivatization with negative ion chemical ionization MS detection for trichothecenes was negative. IR spectra identified the presence of water, traces of hydrocarbons and carbonyl, and silicates,typica1 of soil. Conclusion: No evidence of any known CW agent, agent degradation product or trichothecene was detected. As .eceived by the Analytical Research Division, the sample appears to be innocuous. lassified b : CIA Declassify: OADR 1 Approved for Release: 2015/01/05 000037504 Approved for Release: 2015/01/05 000037504 ANALYTICAL RESEARCH DIVISION RESEARCH DIRECTORATE - 19 September 1984 Analysis/Evaluation of Leaves A shipment designated 10027,Z(4), received by the Analytical Research Division, ;3 February 1984. from FSTC, contained 12 subpackages. One container identified with TH840209-4DL was designated 10027Z(4)-4. It reportedly cosisted of eaves (Figure 1) with yellow spots from 2 to Smm diameter A vapor sample withdrawn s-subjected to analysis by gas chromatography/mass spectrometry A portion of the leaves was leached in chloroform. Another portion of the leaves was leached in 1:1 methanol:water. The solventsolublematerials were analyzed by GC/MS, ion chromatography (IC), thin layer chromatography (TLC) and infrared spectrometry (IR). The GC/MS spectra of the vapors associated with the leaves identified the presence of a series of fatty acids including hexanoic, heptanoic and isooctyl acids, and an unidentified compound of molecular weight 208 having a base peak 123. The 6C/MS spectra of the chloroform solubles showed only a possible trace of chloro compounds. IC separated no ions of interest. No detectable components were separated by TLC. Derivatization with negative ion chemical ionization MS detection for trichothecenes was negative. IR spectra identified the presence of water and aliphatic hydrocarbons. Conclusion: No evidence of any known CW agents, agent degradation products or trichothecenes was detected. The detection of volatilized fatty acids in this sample, 100271(4)-5 and 10027Z(4)-6, but not in the reference vegetation would indicate they are not naturally occurring vegetation components. They are components of the MA thickener for napalm, but the aluminum salts used in the 14r4 Wert not detected. Classified by: CIA c assify: OADR 123 Approved for Release: 2015/01/05 000037504 Approved for Release: 2015/01/05 000037504 LP`I' ANALYTICAL RESEARCH DIVISION RESEARCH DIRECTORATE 19 September 1984 Analysis/Evaluation of leaves A shipment designated 100272(4), received by the Analytical Research Division, 23 FebriAry 1984, from FSTC, contained 12 subpackages. One container, identified with T04029-501. was designated 100272(4)-5. It reportedly consisted of leaves (figure 1) with white spots from 2 to 13Mm in diameter A vapor sample withdra - s subjected to analysis by gas chromatograph ss spectrometry (GC, A portion of the leaves was leached in chloroform. Another portion was leached in 1:1 methanol:water. The solvent solte-le materials were analyzed by GC/MS, Ion chromatography (IC), thin layer chromatography (TLC), and infrared spectrometry (IR). � The GC/MS spectra of the vapor associated with the leaves identified the presence of the same fatty acids, hexanOic, heptanoic and iso-octanoic detected in the vapors of the 100272(4)-4 (TH830209-400 sample. The GC/MS spectra of the chloroform solubles identified only a possible trace of chloro compounds. DC separated no ions of interest. No detectable components were separated by TIC. Derivatization with negative ion chemical ionizatiwi MS detection for trichothecenes was negative. IR spectra identified the presence of water,methyl groups, a trace carbonyl and silicates typical of soils. Conclusion: No evidence of any known CW agent, agent degradation products or trichothecene was detected. The detection of volatilized fatty acids in this sample, 100272(4)-4 and 100272(4)-6. but not in the reference vegetation would indicate they are not naturally occurring vegetation components. They are components of the M-4 thickener for napalm, but the aluminum salts used in the M-4 were not detected. Classiffe CIA C assiff: OADR 3 Approved for Release: 2015/01/05 000037504 Approved for Release: 2015/01/05 000037504 ANALYTICAL RESEARCH DIVISION RESEARCH DIRECTORATE Analysis/Evaluation of Leaves � '17/ 5 e' 19 September 1984 A shipment designated 1002744), received by the Analytical Research Division, 23 February 1984, from ISIC, contained 12 subpackages. One container identified with TH840209-701 was desi nated 100272 -7. It reportedly consisted of reference leav The sample was subjected to the same d on suspect samples. A vapor sample withdrawn subjected to analysis by gas chromatography -try ( A portion of the leaves was leached in chloroforr. Another portion was leached in 1:1 methanol:water. The solvent soluble materials were analyzed by GC/MS, ion chromatography (IC), thin layer chromatography (TLC) and infrared spectrometry (IR). The GC/MS analysis of the vapors associated with the powder identified the presence of dimethyl phenylindene. The GC/MS analysis of the chloroform solubles gave no definitive spectra. IC separated no ions of interest. TIC separated two components Rf 0.15 and 0.40 which reacted with the p-anisaldehyde detection reagent to give a purple color. Derivatization with negative ion chemical ionization MS detection did not detect any trichothecenes. The MS spectra was identical to that of 1002744)-6, indicating a large quantity of an unidentified compound which underwent derivatization. The IR spectra identified the presence of water and fragmentary alkyl hydrocarbons. Conclusion: No evidence of any known CW agent, agent degradation product or trichothecene was detected. Submitted as a reference sample, the components separated by thin layer chroratogra'hy and the component which underwent derivatization afford excellent base iine data for evaluation of suspect samples. h3 lassified b CIA Dec assify: OADR Approved for Release: 2015/01/05 000037504 1709L�0000 90/1-0/91-0Z "10 .././.1,0 110.11000.0 � � 9 ������� � � rro-Pv�aeir- 04 ho� a It 14.)1.1- mod a,. .11/�- 111 Tht - dbol 4.154- op. 01 it (A- es FIGIIRE 1 � 001, 1���.��������� ��������41 .11 b� _a& 111.462haei �"MA. 11143-1