Analytical Methodology for Herbicide Orange. Volume II - Special ...

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TABLE IXCHARACTERISTIC GAS CHROMATOGRAPHIC PEAKS FORIDENTIFICATION OF HERBICIDE ORANGE BY TRANSPORTATION CONTROL NUMBERRetention , , . _ „ . a_.Analysis Sequence NumberTime ' ~(sec.) 8 14 18 11 1 10 10 3 5 4 626+2 0.96+.0.4 0.78±0.1 1.00+0.1 0.86+0.1 0,4310.1 0.36+0.3 0.27+0.1 1.53+0.1 1.60±0.40 0.71+0.2 0.7842+2 1.51+0.2 2.52+0.3 0.36+0.3 1.01±0.2 0.66+0.1 1.72+0.3 0.9469+2 0.12 b 0.13 1.87+0.1 2.39+0.4 0.13 0.0675+2 0.8210.1 0.93+0.2394+5 0.62*'*500±15 0.42+0.1 0.70+0.2 1.37+0.2 1.23±0.1 0.9310.1 0.2710.1 4.97±0.8 4.1710.5 0.9010.1 1.8310.1631+11 0.7010.2 0.88+0.1 0.16890+10 0.12 0.11 0.06909110 0.171744+10 0.19 0.17 1.95+1 0.42+0.2 0.22 0.06 0.24 0.061773120 3.33+0.1 0.10 0.25 0.22 0.23 0.121816+16 0.10 0.10 0.44±0.1 0.3810.1 6.08+1 1.5710.3 0.14 0.31 0.661875+20 0.33 0.26 0.10 0.06 0.111933+20 2.2210.2 0.11 0.16 0.15 0.53 0.16 0.101984+15 0.14 0.16 0.35 0.29 0.37±0.1 0.3510.1 0.41 0.262024+8 0.11 0.09 10.711.42070121 24.5+4.0a See Table I to relate TCN to Analysis Sequence Number. Results listed represent relative peak areas of respectivecomponents.The typical range is ± 202, unless otherwise indicated.
11) Analysis Sequence Group 6 (Monsanto Company, see Figure 11) isuniquely identified by three peaks at the beginning of the analysis (largepeaks at 26 and 42 sec. and a small peak at 69 sec,)., by the absence of peaksat 900 * 50 sec., and by the small peaks at 1744 and 1933 sec.The identification of Herbicide Orange by the characteristic chroir.atogra-nof each analysis sequence group as described above has already proved tobe highly successful. As an example, one barrel of. herbicide used indegradation studies was indicated by extant records to belong to AnalysisSequence Group 18 (Diamond Company). Subsequent fingerprinting of the barrelresidue following these tests clearly established that the herbicide inquestion was from Analysis Sequence Group 8 (Hercules Company). Knowledge ofthe original source of the herbicides is vital if valid conclusions are to bedrawn regarding the effectiveness of degradation techniques, because the compositionof the various lots varies quite markedly. If the decomposition ofspecific herbicide components is being monitored, obviously it is necessaryto know the quantities of these components present in the original herbicidetest sample.IIn summary, the data indicate that among the 15,200 barrels of HerbicideOrange stored at Gulfport, Mississippi, homogeneous groups can be identifiedby using a simple temperature-programmed gas-chromatographic analysis of the'/olatile components of this herbicide. It is thus possible to determine theoriginal manufacturer of any herbicide sample in these stocks by a rapid,simple analysis. This identification does not depend upon knowledge of thechemical identity of any component of the Herbicide Orange. In another, moreextensive report from this laboratory, however, identification of allIndividual components in selected lots of the herbicide stocks has been made byusing combined gas chromatography-mass spectrometry instrumentation.28
Page 1 and 2: Item I Number 04848 D NotScann8dAut
Page 4 and 5: A D - A 011 5 y 8ANALYTICAL METHODO
Page 7 and 8: UnclassifiedSECURITY CLASSIFICATION
Page 9 and 10: PREFACEThe research and development
Page 11 and 12: LIST OF TABLESTABLEPAGEIIIIIIIVVVIV
Page 14 and 15: SECTION IINTRODUCTIONCommercial her
Page 16 and 17: SECTION IIEXPERIMENTALSAMPLING PROC
Page 18 and 19: TABLE IIDENTIFICATION DATA ON HERBI
Page 20: 59 Hercutes 14I900 1800 2700TIME, S
Page 23 and 24: m—is900t1800 2700TME.SecFigure 5.
Page 25 and 26: 251 Dow 10s900 1800 2700TIME.SecFig
Page 27 and 28: o CL OO900 1800TIME, SecFigure 9.Ch
Page 29 and 30: 263 MONSANTO 6BOO27QOTOE.SECFigure
Page 31 and 32: TABLE IIICOMPARISON OF ANALYSES OF
Page 33 and 34: TABLE VCOMPARISON OF DUPLICATE SAMP
Page 35 and 36: TABLE VIICOMPARISON OF DUPLICATE SA
Page 37 and 38: TABLE VIIISUMMARY OF ANALYSES OF HE
Page 39: TABLE VIII (Continued)RetentionTime
Page 43: 19. R. Baughman and M. Meselson, Ad

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