1 15 2 https://www.nal.usda.gov/exhibits/speccoll/files/original/f208d78a1de1cbeafdf9b658efc6fca2.pdf 525c40d27c227cdf281229ddc7d68c1a PDF Text Text Item D Number °2194 Author Smith R M Corporate Author Toxicology Institute, Center for Laboratories and Resear ' - ' Roport/Artldo TltlB Determination of Polychlorinated Dibenzofurans in Soot Samples from a Contaminated Office Building Journal/Book TltlB Year 1982 Month/Day March Color Number of ImaQBS n 68 Descripton Notes Thursday, September 20, 2001 Page 2194 of 2293 �Determination of Polychlorinated Dibenzofurans in Soot Samples from a Contaminated Office Building R. M. Smith, D. R. Bilker, P. W. O'Keefe, S. Kumar and K. M. Aldous Toxicology Institute Center for Laboratories and Research NYS Department of Health Albany, NY 12201 March 1982 �ABSTRACT The identification and quantitation of polychlorinated dibenzofurans (PCDF) in soot samples from the Binghamton State Office Building is reported. The analytical techniques and sample clean-up procedures are discussed and the identification of other major chlorinated combustion products given. INTRODUCTION I On February 5, 1981, a soot-producing fire involving a ^transformer i occurred in an office building in Binghamton, New York. The transformer contained a dielectric fluid with the trade name "Pyranol" consisting of polychlorinated biphenyl (PCB) Aroclor 1254 (65%) and chlorinated benzenes (35%) together with some trace additives. Preliminary analyses of a soot sample showed high levels of PCB and the presence of 3 ppm 2,3,7,8 TCDD and 100 ppm 2,3,7,8 TCDF (1). TCDFs and PCDFs are commonly found as contaminants in PCB formulations (2,3) and have also been shown to occur when PCB is heated under certain conditions (4). Subsequent samples analyzed in our laboratory (5,6) include a soot homogenate used for animal toxicity studies and an air particulate sample taken inside the building using a high-volume air filter. TCDFs. Both samples were found to contain a mixture of The analysis of soot sample by two other dioxin laboratories verified the presence of Tetra Chlorodibenzodioxin (TCDD), TCDF and heavier chlorinated PCDDs and PCDFs (7,8). Several of the polychlorinated biphenylene compounds were also identified. �The present report describes the analysis of a representative soot sample from each of the 17 floors of the building and a soot homogenate used in animal toxicology experiments for PCDFs. Provision has been made in the clean-up and in data aquisition for the analysis of PCDDs but this will be discussed in a subsequent report. �METHOD Sampling Because a large portion of the contaminated building had already been cleaned to some degree, the particulate matter which had accumulatd undisturbed on the upper surface of suspended ceiling panels was sampled on each level. One half (2 ft. x 2 ft.) of a ceiling panel was wiped clean using a dry cellulose filter paper. Both the obtained particulates and the filter paper were stored inside a screw-capped glass test tube for analysis. Often adjacent samples were combined in the laboratory to provide enough weighable material for testing. A group of 8 samples was collected in the same building area for each of 16 floors. A sample of soot homogenate from several floors which was used in animal toxicology experiments was also included. Extraction Six to eighty milligrams of particulate were weighed out and placed into a glass extraction thimble containing 5 mm of silica gel (Bio Rad). Internal PCDD or PCDF standard in benzene was added to only 2 samples prior to extraction (added to all other samples after extraction) so other extracts could also be used for animal and cellular testing experiments. A glass soxhlet extraction apparatus was then charged with 100 ml benzene and the particles were continuously extracted for 16 hours. A solvent blank, a carbon blank (active coconut charcoal), and four recovery control samples were similarly extracted and analyzed. All extracts were stored in the dark. �Collaborative Studies Separate portions of each crude extract were provided for PCB analyses and for use in cell keratinization studies. Sample Clean-up The benzene extract was concentratd to 5 ml using a boiling water bath. An aliquot of the sample was spiked with 80 1 of mixed, labeled internal standard (13C 2,3,7,8 TCDD, 37C1 37 TCDF, Cl OCDD) and cleaned-up using three sequential liquid chromatographic columns as follows: Each sample was diluted with acetone to 20% benzene and injected onto a low pressure LC system using a column of 50 mg PX-21 adsorptive carbon mixed with 600 mg celite. This column is known to strongly adsorb planar, halogenated aromatics. sample was washed with 40 ml of 20% benzene/acetone. The Flow through the column was reversed, and the fraction containing PCDDs and PCDFs was eluted with 30 ml toluene. The toluene was removed in boiling water bath using a stream of N_ and the solvent was changed to dodecane. The sample was then applied to a 1 cm id x 8 cm long column containing 2% deactivated silica gel (Bio Rad) and eluted with hexane. The 0-10 ml fraction containing the PCDDs and PCDFs was collected. This chromatographic step is effective at eliminating relatively polar, highly colored components. The sample was then directly applied to a 1 cm x 8 cm long column containing activated Florisil (180° overnight). The column was washed with 20 ml benzene to remove PCBs and PCDD/PCDF fraction was eluted using 20 ml of 3% CH.CN, 47% CH2C12, 50% Hexane. The sample was then concentrated to 80 1 in �benzene prior to capillary Gas Chromatography/high resolution Mass Spectrometry (GC/HRMS). Instrumental Conditions Gas Chromatography - A Carlo-Erba Model 4160 Capillary Gas Chromatograph with on-column injection was used with a 30m x 0.32 ram i.d. fused silica "Durabond" DB-5 column ( & W Scientific) j and helium carrier gas. The effluent from the GC column was coupled via an open-split interface to the mass spectrometer source re-entrant using a length of 0.16 mm i.d. fused silica tubing de-activated with 2% Carbowax 20M in Methylene Chloride and coated with a 15% OV-17 in Methylene Chloride then conditioned at 50°C to 300°C at l°C/min. programmed during analysis as follows: The GC oven was 70 C to 180° at 10°C/min then 3°C/min to 270°C and hold isothermal for 20 minutes. The GC/MS interface region was held isothermally at 275 C and typical on-column injection volumes were 2 1. Mass Spectrometer - A Kratos MS-50 mass spectrometer operated in full scanning mode was used to acquire GC/MS data. The spectrometer was tuned to 10,000 (10% valley) dynamic resolution and scans were taken at 3 seconds per decade over the mass range scan. /Z = 600-150 resulting in a 4 second cycle time Perfluorokerosene (PFK) was used as a mass standard for high resolution scanning and was introduced concurrently with the GC effluent into the source of the mass spectrometer which was operated in electron impact (El) mode at 70 eV, 8kV accelerating voltage and a source temperature of 250 C. Data was acquired during GC/MS runs using the DS-55 data acquisition system via the �preprocessor interface at a sampling rate of lOOkH z and stored on disk as sample-time data for subsequent mass conversion. Each run comprised ca 800 scans each of which contained data from the mass standard reference peaks and mass peaks generated by compounds eluting from the gas chromatograph. The file of sample-time data was mass converted after acquisition producing a file of mass measured peaks and associated intensities, the exact mass being computed for the unknown peak by reference to the mass standard peak with a precision of ca lOppm, The data system then allowed each GC run to be displayed in various graphical forms or as exact mass listings. Post-Run Data Processing To generate useful quantitative and qualitative information from the acquired GC/MS run, several data processing routines were employed. Firstly, sample-time data was mass converted to generate high resolution scanned data files. A total ion current (TIC) and exact mass chromatogram was then generated for mass ions of each compound group of interet along with a computer-generated worksheet. This worksheet then allowed the operator to select scan windows which encompassed GC peaks of interest. The scan windows were then fed into a software program which generated scan by scan exact mass-intensity reports ever specified mass ranges. These reports were then used to allow quantitation of the exact mass ions over the GC peak of interest by summing the intensity for each scan over the deviation of the GC peak. The facility to do this with software had not yet been developed for exact mass data. The resulting areas of the exact �mass chromatogram were used for guantitation and verification of ion abundance ratios. in Figures This process for a standard run is shown 1-27. Quantitation of PCDFs The only available labelled reference standard for PCDF was a [U-37 Cl.l-TCDF sample obtained from KOR Isotopes Inc. As can be seen from Figure 3 the material was not pure and contained several Tetra isomers. Previous work had indicated that it contained less than 2% unlabelled material for all PCDF and PCDD congeners. This material was therefore used as internal standard and provided a method for calculating recovery of the clean-up procedure. Native PCDFs were available for Tetra CDF, Hexa CDF and Octa CDF and these compounds were used for external standardization. A mixture of native and labelled PCDF was run each day and data was collected on samples to verify response factors and instrument performance. Quantitation of the samples was therefore performed using response factors obtained from the calibration run for Tetra, Hexa and Octa CDF. Response factors for Penta and Hepta CDF were linearly interpolated from adjacent congener responses. The recovery of each sample through the clean-up procedure was also *5 A calculated from the [U- C1.]-CDF response. Quantitation was therefore not isomer specific but represents a total quantity of each congener group and assumes equivalent responses for isomers within each group and the validity of the response interpolation for Penta and Hepta CDF. �Quality Control and Detection Limits The Mass Spectrometer was tuned to 10,000 (10% valley) Resolving Power daily using PFK as mass standard and High Resolution Calibration was performed before the start of each run. A standard injection of PCDF and PCDD reference compounds was then run and calibration of response factors was performed. Table 2 lists the standard runs used for quantitation over the period of ca 2 months indicating an overall RSD of ca 25% for the various measured response factors. Detection limits were also calculated using the standard runs assumming a typical GC peak width of 6 scans and noise level of 250 counts per scan for g a signal to noise level of /N=2. In addition for positive identification the 3 most intense ions in the parent cluster must show close agreement to the theoretical ion ratios and exact masses, retention time must agree with standard runs and mass spectrum obtained must match that of the standard reference spectrum. �Results and Discussion Table I lists the quantitation for PCDFs in the 16 samples collected from each floor of the Binghamton State Office Building and the soot homogenate used for animal toxicology experiments. Recoveries based on [U-37Cl.J-Tetra CDF are reported and values for the samples are not corrected for recovery. The significance of these data and correlation with other testing is presented elsewhere (9). Data from three GC/MS runs are presented in more detail to indicate the information that is available for each sample run. The extract of the soot obtained from the 5th floor and the soot homogenate is presented to be representative of the sample data and a standard used to quantitate the soot homogenate is also shown. Figures 1-27 correspond to the standard run and show the Total Ion Current (Figure 1) and exact mass chromatograms for each compound and congener present. The tabular reports (Figures 2 and 10) are worksheets which allow the analyst to enter the scan ranges visually determined to contain the components for quantitation. Quantitative reports are then generated for these scans which give the exact mass and intensities of peaks within the specified mass range. These have been included for the Hexachlorodibenzofuran (Hexa CDF) standard Scans 437 to 446 over the time period when this compound was eluting from the GC (Figures 17-27). Summing the intensities for the three most intense ions in the parent group, i.e., 371.8236, 373.8207, 375.8177, give the total intensities of 113,735, 211,168, 158,794, respectively which agree well with the theoretical ion �ratios. The intensity of the 100% ion (373.8207) is used for computing the response factor and quantitation of samples. This method of peak integration was used for the quantitation of GC peak area for all standard and sample runs. Scan were only included in the summation if the exact mass of the 3 ions was in good agreement (better than lOOppm) and ion ratios were consistent with theoretical ratios (Table 4). Figures 28-37 correspond to the GC/MS data from the 5th floor sample processed in a similar way to the standard. Figure 28 is a total ion current chromatograph the most intense GC peak being due to diisooctylphthalate is a contaminant found in all sample runs and to a lesser extent the standard runs. Figure 29 shows the exact mass chromatograms for each of the Cl-,-Clo 0 J congeners of PCDF simplified by plotting only the most intense ion in the parent group. Figures 30-34 are mass spectra obtain from each congener group identified in the exact mass chromatograms. Figure 30 indicates the presence of Pentachloronaphthalene (exact mass 299.8648) as well as Trichlorodibenzofuran (exact mass 271.9376), in the spectrum of scan #242. Polychloronaphthalenes appears to be major components in the soot samples and are also found in the soot homogenate sample. Figures 38-51 correspond to the data obtained for the soot homogenate sample. The total ion current chromatogram again indicates as a major GC peak the diisooctylphthalate (Figure 38). Figure 39 shows exact mass chromatograms for PCDFs and Figures 40-45 give typical full scan spectra for each congener. 46 indicates the exact mass chromatograms for Figure �Polychloronaphthalenes with intense peaks for Cl,., Cl, and C17 Chloro congeners. Figure 47-51 again shows full can spectra for each of the Chloronaphthalene congeners. Quantitation has only been made for the PCDPs but as indicated qualitative evidence for Polychlorinated naphtahlenes has been shown and trace levels of Pentachlorobiphenylenes (see Figure 36A) at exact mass 323.8647 we indicated in the 5th floor sample. Carbon and solvent blanks showed no evidence of contaimination at the detection limits indicated. The vast amount of high resolution data is continuing to be reviewed to complete the data analysis and software development continues to aid in the process of data reduction and quantitation. �References 1. R.M. Smith, P.W. O'Keefe, D.L. Hilker, B.L. Jelus-Tryor, K. Aldous, NYS Health Dept., Toxicology Institute Report, Feb. 20, 1981. 2. C. Rappe, H.R. Buser and H.P. Bosshardt, CIPAC Symposium, Baltimore, June 5-6, 1979. 3. C. Rappe, N.R. Buser, D.L. Stalling, L.M. Smith, R.C. Dougherty, Submitted to Nature. 4. B. Janson and G. Sundstrom, Dioxins and Related Compounds in the Environment, Rome, October 22-24, 1980. 5. R.M. Smith, P.W. O'Keefe, J. O'Brien, D. Hilker, K. Aldous, B. Jelus-Tyror, NYS Dept. of Health, Toxicology Institute Report, June 2, 1981. 6. R.M. Smith, D.L. Hilker, P.W. O'Keefe, S. Kumar, J. O'Brien, B.L. Jelus-Tyror, K. Aldous, NYS Health Dept., Toxicology Institute Report, October 1, 1981. 7. C. Rappe, University of Umea Report, 1981. 8. D.L. Stalling, Columbia National Fisheries Res. Lab., Preliminary Report, March 31, 1981. 9. G. Eadon, K. Aldous, G. Frenkel, J. Gierthy, D. Hilker, L. Kaminsky, P. O'Keefe, J. Silkworth and R. Smith, NYS Health Dept., Toxicology Institute Report, March, 1982. �TABLE I Concentration (ppm) of Polychlorinated Dibenzofurans in Soot Samples Taken from the Bing Floor # PCDFs4 Tetra CDF 1 2 3 4 2.5 5 44 6 5.1 7 77 8 9 1 0 35 160 47 9.6ng 1.9ng 6.5ng 0.06 1.8 37 10.7ng 3.8ng 7.2ng Penta CDF <0.06 <2.0 3.2 55 8.0 75 40 220 55 Hexa CDF <0.07 <2.4 2.0 36 3.0 14 16 140 28 Hepta CDF <0.08 <2.8 0.2 12 0.6 1.5 7.1 51 2.1 Octa CDF <0.09 <3.1 <.2 4.2 <.2 -- 1.4 17 0.56 29 22 16 20 22 41 50 "A. C1 Tetra CDF (ng)1 5 Recovery %' 4.4ng •"•Internal standard amount recovered (ng) ^Quantitatecl as Arochlor 1254 0 Data lost due to instrument malfunction 4 Data unconnected for recovery ^Recovery based on -^Cl Tetra CDF internal standard 8.6ng 14.2ng 49 35 �TABLE 2 Reproducibility of Standard Runs Response Factors [Counts/ng] Date of Run Tetra CDF C14 Tetra CDF Hexa CDF Octa CDF 1/26/82 1380 4938 771 630 1/29/82 1193 3987 834 913 1/30/82 1475 4904 815 660 2/10/82 1803 5358 953 793 2/15/82 1306 4777 919 754 2/15/82 1802 6568 2/16/82 1354 5926 1225 837 3/3/82 1880 7017 1339 1075 3/4/82 1961 6690 1492 1178 3/5/82 1978 6794 1271 1193 3/10/82 2616 9606 1700 1336 3/11/82 2293 8622 1472 1147 Average Response 1753 6265 1163 978 430 1645 320 217 25 26 27 22 Standard Deviation %RSD — 874 �TABLE 3 Average Detection Limits For PCDFs" Average Response Factor counts/ng DL(ng)S/N=2 'PPM in Soot 0.17 Tetra-CDF 1753 1.7 37 6265 0.5 Pent a -CDF 1458 2.0 0.2 Hexa-CDF 1163 2.6 0.26 Hepta-CDF 1070 2.8 0.28 978 3.0 0.30 C14-TCDF Octa-CDF "Based on GC peak width 6 scans noise level 250 counts/scan "Assuming an injection volume equivalent to lOng of extracted sample �Table 4 Exact Masses and Intensities of Molecular Ions of Chlorinated Dibenzofurans Chlorination Number Exact Mass (Molecular Formula) (3) Monochloro 202.018539 100.0 C 204.015590 32.5 235.979568 100.0 237.976618 65.0 269.940596 100.0 271.937647 97.5 373.934697 31.7 303.901625 76.9 305.898675 100.0 307.895726 48.7 337.862653 61.5 339.859704 100.0 341.856754 65.0 371.823682 51.2 373.820732 100.0 375.817783 81.2 407.781761 100.0 409.778811 97.5 411.775861 52.8 Octachloro 441.742789 87.9 C 443.739840 100.0 12H7OC1 Dichloro Trichloro Tetrachloro Pentachloro Hexachloro Heptachloro 12°C18 Intensities �DS-55 CROSS SCflN REPORT, RUN: TD1S1 -5- f *- f\- 1 ~ a * 'CA* TIC 38:00 .i i i i t i I i i i i i t I i i I t i i i i i i t I i i ii i i i i i t i i l i t i i i 44:49 t » i .1 l i t i i i I t i i i i i 80 70 68 50 43 30 10 i i i i i t i i i I i i i i i i 1 100 |- i i i • ! i- 1 i i i i i i i 1 i i-i -i i i r i i T-I i " i i i 200 300 400 50Q 680 �<T*\ T O»»»«j»»fcc»\0S at TfiBLE OF^POlYCHLORODIBENZOFURflN MftSSES, INTENSITIES ftND SCftN" NUrCERSCFROM XSCftN DflTfl) TRICHLORO- 270(100.0),272(97.5) SCANS: REFINED SCfiNS: DICHLORO- 236(180.0),238(65.0) SCANS: : REFINED SCflNS: MONOCHLORD-202(130.Q),204(32.5) SCftMS: >;, REFINED SCflNS: TETRftCHLORO- 304,(76.9),385(100.0),312(INTERNAL STfiNDftRD) SCflNS: ^^.^c,- ,'>Vt30V3V../) REFINED SCANS: PENTftCHLORO- 333(61.5),340(100.8) SCfiNS: j- REFINED SCfiNS: HEXflCHLORO- 374( 100.0),376(81.2) SCflNS: i 3 5 " ••;.,' (m'--i'^)i-^I REFINED SCRHS: HEPTflCHLORO- 493(100.0),410(97.5) SCflNS: . REFINED SCAMS: OCTflCHLORO- 444(100.0),442(87.9) SCftNS: t-ID-^D^'J-v'?- .- ,-.).') : (\Jcivt c- REFINED SCftNS: T*i LD f -— �, 3v Ot )S-55 "CROSS SCRN REPORT, RUN: TDlsl iero*. T . U it 304 L88 # 385 I—1—1__! 0 312 i ' i + TIC ' ' I ' i—I I I t - t 1—!_!—1_J I—I—!—I—I—L_l 90 80 78 60 50 48 30 20 18 i—T—T—rn—i—i—!—i—(—1—i—i—i—i—i—i—i—T—i—i—i—i—i—i—i n—i I t I t 1 I I I I 1 I 1 I I I I 1 1 I I t I • I I t t t • t t �f ' 3 . THIS 1.306 CTIO4723S8, 100%=6655G3 El 100 312 70 SO 50 40 30 20 15S 10 247 209 , , , i , , I 200 , 230 493 43 i i , 31 rr!-rfrflri'l V'rmV'. mSVr n 4m i I I ii i I :i 100 150 ?75 i j f n V i rfn r ; t rVrr i i M i MI 450 500 �iv\ T i\ * TD1S1.314 CTIC=S72688, 100^=86756] El ' 312 18B 78 60 50 » 28 173 10 CD 247 -1 en 210 !• i ... | I I ! I I M M ' ] iTT'l 103 ISO ,i . 1 I I 1 j 1 00 250 309 i_i . il. i -i . it. -.1 i i i i - . . i . . i i. ,.h it i...t t . . . ] iii 11 ij i iiiii iii iii i i iiii ri11 1 1 ii i ii 350 AQQ 450 �S cK/"0vw.vToevf T - C& F, JJS-55 CROSS SCAN REPORT, RUN: TD1S1 * 338 * 348 0 374 a 376 $ 408 % 410 + TIC 10:44 31:11 180 38:80 I I !..__!_ I I I 4:9 44 I I I I t...._! 1 ] I I 1002=737424 93 lG8?i=56484 88 78 sa 58 4B 38 28 18 8 kj.,* <U<h i ^ » * MPW\M_oA^^>A....|F> t_ ro OT ('••> inn i —i —i —i —i —i —i —i —i —i —i —i — i —i 200 A r—|—\—r""f—I* i t—i—i 300 -i—i—i—r1-!—i—r—r 400 500 i—|—i—r—i—r—T—r 600 �TDIS 1.442 CTIC=656808, IOOri=5S0453 El 100 374 88 70 J 38 28 _ 241 155 IE 8 18 207 i i i i i i i i i 100 r ]150 ' i 'i'-"/ 1 < I i.!,1TT f,nfl.t~i'i 1 i 'T 209 J I II p i i ri I~TTTI rr 489 459 I.. , i. I I IT 509 �DS-55 CROSS SCHN REPORT, RUN: TD1S1 # 442 ;;; 444 + TIC 10:44 *™ J ! I 17:33 I I I . I . I I t I I 24:22 I - -I I I I I I l i l t 31:11 I ' » ! ' ' ' ! ! 1 lOOr: =737424 i 100;; =20464 80 78 50 W^MJV^ 30 20 10 f _ . r ...—J—r 33:00 1 1 1 1 ' I I I I 1 44:49 1 1 1 ! l.....,t.,, I I . ,I I t I I I �TD1S1.622 CTIO581008, 100^=346263 El 100 90 444 80 70 G3 58 207 156 20 379 10 472 - ITT I 11I I I 1I 1 I j I 100 150 200 250 3CQ 400 450 508 �TftBLE OF POLYCHLORODIBENZO-P-DIOXIN MftSSES,INTENSITIES ftND SCflN NUMBERS(FROM XSCflN DflTfl) TRICHLORQ-283(100.0),235C37.5) SCRHS: ^ SICHLORO-252(103.0),254(65.0) SCftNS: £ MONOCHLORO-218(100.0),220(32.5) :X- REFINED SCftNS: REFINED SCftNS: REFINED SCftNS: TETRftCHLOP r '-72G(76.9),322(182.8),334(INT.STD.) SCPNS: . REFINED SCfiNS: N {^«e MTO. 6vv4f>vl WTtDJ*") PENTACHLCRO-356( 160.0), 358(65.0) SCflNS: ^ REFINED SCflNS: HEXftCHLORQ*3SWtlB8.0),392(81.2) SCftNS: . , « / M / , e - ., X U to- ^7-5 (^l-t^ti-Vot?) HEPTftCHLORO-424(lB0.0), 426(97. 5) SCftNS; /M, <- REFINED SCflNS: REFINED SCftNS: OCTftCHLORO-453(B7. 9), 4GO( 109.0), 452(65. 0),472( INT. STD.) SCftNS: . REFINED SCHNS: �TCD{> DS-55 CROSS SCHN REPORT, RUN: TD1S1 * 320 toe * 322 0 334 + TIC 4:80 i 18:44 t i i t i t i t L i i 17:33 J r t i i t i f f i 31:11 24:22 ! I I I I I I l i i i t 38:< 44:49 i i i I i i t t i t i i i I i i i i i i i t i I i i i i t i 1882=737424 90 1802=66155 88 78 68 50 toWfyW 4B 38 28 18 ' ^AAvWWjvAj^JUA 3. ]—i—i—n—i—r~i—i—r-*|—r—i—r 1 100 200 "i-i "f | r i 300 r. n i rVi—A—fM^_«_ .tfUVvJUI—A <D CO C' /U_A-/lA fn ] i i- i - .rA i i i i. f\ 11 1 „,*! . - .n*.i ' i i ti * i r i i 1 p 480 500 T I I 600 1 I I I T �Fid.. TDISI.325 CT!C=S78848, 10BX-65720] El 103 322 9B 70 60 58 30 259 28 160 194 10 1 229 0 ! J/ M>! i i i i i i i i i"( j l I J ,'*! 100 200 150 ^Vrh^Hfr1! 250 300 'n i I'-i'n pm i f-rf 350 498 • 450 500 �fc, ssDS-55 CROSS SCAN REPORT, RUN: TD1S1 * 356 * 358 0 398 & 392 $ 424 X 426 + TIC 10:44 17:33 31:11 38:80 44:49 100 1002=737424 90 1082-17096 80 78 68 53 40 39 28 18 100 I—I—I—1 I—I—1—I—I—I—I—I—I—I—I—I 200 300 1 I 59Q I ft I I . I. f<I , I . !. I y.. I . I . I I 603 �TB1S1.4S6 CTIC=42S944, 100^=139853 El 100 390 80 70 68 50 207 327 38 262 28 243 10 282 163 1 150 'T200 " ^r-m-' il M F T" 2'50 o u 431 300 V 1/JfWf innr i ii!V 350 400 IT UJ I I I I i il T 450 I I I I 500 �TD1S1.539 CTIC-413920, 1002*170953 El 1GO 426 90 80 70 207 50 38 2S9 361 10 298 H 158 323 ti-WW 15G 200 300 JihUuii 350 'inn I i [ I T i l 450 i i ii 500 �DS-55 CROSS SCRN REPORT, RUN: TD1S1 * 450 tt 460 0 4G2 & 472 + TIC ] 0:44 17:33 24:22 3S:0Q 31:11 103 i 44:49 i i l i i i t t l t t f t l t t t t 10Q;<=737424 93 1092=7307 BO 78 GO i 50 1 ~ i if v/V'*' H/ WHuA^ 40 Ji *«J il i \ *jsv t \V/f \\'\ u IjVVi/i j ? }/ 1 \V V ^Yt^^\}'i^jl ' ' ' i j 30 i .: 20 10 1 _ .1 1* 0 . f i i l 1 ,\ il i / i fi I j i (j t f. ,\ > i A ,\ \ i i ! /, /, !. j '. 1! .1 t. b'jfj �JD151.G22 CTIC=50I008, El iee 444 90 -I 70 60 -I 50 33 207 - 15S 20 379 309 472 a u 222 18 II I ISO 200 350 1QO 450 500 �i* DP0:TD1S1.MS O SCfiN: 437, 3/11/02 14:51 lONISfTTION: El \V\TUA: NO. PGfiKS: 308/ 11 BflSE/NKEF INT: 38693./ G315. TIC: 350512./ 30193. P. MOSS RHNGE: 149.9904 RETN TINE/MI5C: 33:43/ PEftK NO. 1 2 3 4 5 G 101 182 103 134 185 1QG 107 103 103 110 111 112 113 114 115 116 117 118 MEASURED fiHGS 31376. 33530. 33033. 147089. 103009. 1941559. 302 . 0065 301.SG92 3:11.0130 300.9761 300.0102 379.3008 370.9742 377.8208 376.3074 37G.040G 376.0304 375.0275 375.0317 374.0165 373.9791 373.G45I? 373.3194 371.0334 NO. POINTS G G 5 G 5 5 0 8 8 17 G 5 8 21 5 4 4 25 0 4 5 0 12 21 G54.9G01 53/ O/ t>r Ct\ V A*-. 50 fl!30QLUTE INTENSITY 4GO. 310. 292. 344. 243. 255. 713. 543 . 3G5. 2558. 376. 205. 745. 1617. 270. 142. 154. 6101. 729. 151. 228. 1903. 4943 . 6315. ^- p^»V.» "A INT. BflSE 1.2 0.8 0.0 0.9 0.6 0.7 1.8 1.4 0.9 G.G 1.0 0.5 1.9 4.2 0.7 0.4 0.4 15.0 1.9 0.4 0.6 5.1 12.0 1G.3 HREF 11.3 5.0 6.0 3.2 25. G 44 . 2.2 2.4 9G.6 11.5 2.4 3.G 31.5 70.3 100.0 ION 0.1 0.0 0.0 0.1 0.0 0.0 0.2 0.2 0.1 0.7 0.1 0.1 0.2 0.5 0 0 . 0 0 . 0.0 1.7! 0.2 0.0 0.0 0.G*! 1 . 4-:1.0! ^ A\\ )A 4U M* �DP0:TDlSl.nS SCnN: 430, 3/11/02 14:51 IDNISnilOH: El NO. PEHKS: 301/ 7 BOSE/NREF INT: 40093./ 120GO. TIC: 35BG5G./ 13803. MASS RANGE: 143.9304 - 654.3601 RETN TII-E/MISC: 33:47/ 69/ 4/ 47 PEHK HO. NEriSURED 1 2 3 4 5 6 7 8 101 102 103 104 105 106 107 103 103 110 111 112 113 114 1 15 116 117 1 10 113 32446 . 33041. 34067. 76607. 102010. 105693. 135216. 195009. 38 1.9746 3G 1.7038 301.0170 300.9761 300.9263 379.0357 370.0160 377.0127 377.0045 376. OS 39 375.0533 375.0025 375.7232 374.9751 374.0092 373.9663 373.3103 372.0033 371.0035 mss NO. POINTS 5 4 4 4 5 5 4 3 6 4 6 17 6 6 6 17 5 12 6 21 5 5 10 0 25 14 21 % INT. X INT. K TOT. ION NREF BflSE _ 0 0 . * 225. O.G 0 0 . 150. 0.4 0.0 140. 0.4 0.0 151. 0.4 8.0 0.7 274. 0 0 . O.G 243. 0.0 171. 0.4 0.1 1.2 472. 0.1 379. 0.9 0.0 1.2 149. 0.4 2.3 0.0 0.7 202. 1.1 ' 10.1 4050 . v 3.3 0.1* 365. 0.9 0.1 3.7 442 . 1.1 0 0 . 0.6 1.9 228. 0.8 7.2 24.0 2098. 0 0 . 231. 0.6 1.9 0.5! 15. S 1304. 4.7 0.0 0.6 1.9 220. 06 . 4 2.9 26.0 10424. 1.7 0.1 0.5 286. 0.0 209. 0.7 1409. 12.3 0.4 3.7 5.6 0.2 670. 1.7 3.4 100.0 12068. 30.1 0.4! 4.0 13.3 1603. 37.9 1.3 4560. 11.4 R8SOLUTE INTENSITY �DP8:TD1S1.NS SCftN: 439, 3/11X82 14:51 IDNISflTIDH: El NO. PEfKCO: 323/ G BfiSE/NREF I N T : 41123./ 24250. TIC: 42GOG4./ 33GO. MASS RANGE: 143.9504 - G42.9G01 RETH TII-E/MISC: 33:51X 81X 3/ 50 PEH!< HO. 1 2 3 4 5 6 7 8 34 95 96 37 38 93 100 181 182 103 104 105 186 107 103 103 110 NEnSLJRED nnss 30024. 31417. 33002. 105320. 102959. 193934. 134529. 13G917. 383.594G 381.9915 330.9761 379.8131 379.917G 370.9053 370 . 0209 377.0433 377.0878 37G.047G 37G.0502 375.0139 374.0230 373.01G7 372.05'JG 372.0U9S 371.0170 NO. POINTS G 5 G 5. 8 4 17 4 4 5 21 14 G 8 10 18 17 0 10 25 21 25 4 12 25 RRSOLUTE INTENSITY 432. 240. 412. 195. 598 . 1G3. 791. 105. 1G4. 219. 5G35. 1161. 414. 703. 850. 1804. 7120. 574. 1345. 16640. 2347. 24258 . 170. 303. 14002. % INT. % INT. X TOT. ION DftSE NREF _ 0.1* 1.1 0.1 0.6 0.1 1.0 0.5 8.0 0.1 1.5 0.8 8.4 0.2 1.9 0.0 0.4 0.7 8.0 0.4 8.1 0.5 1.3 13.7 0.3 2.8 4.8 1.7 8.1 1.0 0.2 1.9 3.5 0.2 2.1 8.4*! 7.4 4.4 17.3 29.4 1,7* 0.1 1.4 2.4 5.5 0.3 3.3 3.9 49 . 5 GO. f, 9.7 0.G 5.7 5.7 100.0 59.8 0.0 0.4 0.7 2.4 4.1 0.2 3.3 34.0 57.7 �DPBrTDlSl.NS SCDH: 440, 3/11/02 14:51 lONIGHTlQH: E! NO. P!-:nKS: 354/ 10 DACE/HREF INT: 41393./ 36504. TIC: 513632./ 47000. MHSG RflHGE: 143.9904 - 654.3601 RETN TIME/NISC: 3 33:S5/ EflK HO. MEASURED 1 2 3 4 5 G 7 8 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 120 129 130 32345. 33642, 34077. 35731. 120190. 159326. 105341. 105505. 303.5280 30 1 . 9626 38 1 . 0270 309.3761 380.7943 303.2530 373.0384 379.7974 370.0180 377.8037 37G . 05 1 1 376.0105 376.0170 375.0150 375 . 6740 374.8268 373'. 0171 373.7535 372.0286 371.0229 mss NO. POINTS 8 G 5 4 5 5 D 4 5 8 5 25 8 5 10 12 17 35 10 17 4 29 0 25 35 G 17 25 71/ 4/ 47 OBSOUJTE INTENSITY % INT. BflGE 1.6 1.2 0.5 186. 0.4 0.5 203. 8.6 230. 0.5 215. 146. 0.4 0.5 204. 1070. 2.6 0.5 204. 3932. \/ 7.5 1.2 511. 0.6 261. 2.8 1147. 2.8 1167. 1650. 4.0 34.9 14440. 730 . 1.0 9.3 3853. 0.4 157. 64.8 26830. 0.9 358. 17.6 7277. 83.2 36504. 0.8 327. 7.7 3205. 46.2 19106. 674. 504. 210. % INT. X TOT. NREF _ ION 0.1* O.G 3.0 O.G e.i 1.4 0.7 3.1 3.2 4.5 39. G 2.0 10. 6 0.4 0.1 0.8 0.0 0.8 0.0 0.0 0 0 . 8.0 0.2! 0 0 . 8.6 73.5 1.0 19.9 100.0 0.3 0.8 52.3 8.1 0.2* 0.2* 0.3 2.8 0.1* 0 . 0* ! 0.0 5.2 0.0 1.4! 7.1 0,0 8.6! 3.7 �r~t A • BP0:TB1S1.MS SCrtN: 441, 3/I1/C2 14:51 : El NO. PEHK'J: 3G2/ 10 BSSE/Hk'EF INT: 52611./ 4GGD6. riC: 5G1264./ 25336. MftSS RflNGE: 143.8904 - 654.9G01 RETN TliiE/tllSC: 33:59/ 81/ 2X 41 PEHK NO. 1 riEftSURED iinss 107 ICO 13S83. 1 5030 . 30657. 31120. 32338. 117G1G. 194130. 135G95. 383.8052 302 . 9759 301.9015 330.3761 3C0.02GG 109 110 111 373.8181 370.8106 377.0165 2 3 4 5 6 7 0 184 105 106 112 377. 1345 113 114 115 116 117 118 119 12B 121 376.0139 375.8207 375.75G3 374.3701 122 123 124 125 126 127 374.8225 374.2363 373. SGI 5 373.8134 373.7541 373.4754 373.2477 372 . 0404 371.3722 371.0194 371.5324 NO. POINTS % INT. ABSOLUTE BflSE INTENSITY G 0 5 4 0 6 10 4 334. GIG. 234. 147. 404. 350. 503. 143. 8 G 17 552. 323. 1169.. 3035v^ 645. 2513. 17 8 21 17 29 1G021. 4 14 183. 2692. 23 4 0 21 G 34202 . 158. 471. 3507. 4 35 G 4 G 17 5 25 5 2157. 294. 150. 4GG9G. 441 . ISO. 375. 2157. 272. 21210. 243. 0.7 1.2 0.4 8.3 0 0 . 0.7 1.8 0.3 1.0 0.6 2.2 5.9 1.2 4.8 4.1 32.0 0.3 5.1 65.0 0.3 0.9 G.7 0.6 0.3 88.0 0.8 8.3 0.7 4. 1 0.5 40.3 0.5 n INT. NREF _ ?i TOT. ION 0.0=* 1.2 0.7 1.4 5.4 4.6 3G.0 0.4 5.3 73.2 0.3 0.1 1.0 0.0 7.5 0.6 0.6 0.1 0 0 . 0.3 10Q. 0 0.9 0.4 0.8 4.6 O.G 45 . 4 0.5 0.0 0.0 0.0 0.0 0.0 8.0 8.1 0.1 0.2 8.6 0.1 0.4 0.4 3.0 0.8 8.5 6.1 0 0 . 8.3 0.8 8.0 8.0 0.4 0.8 3.0 0.0 �BPB:TDlSl.riS .SCAN: 442, 3/11/02 14:51 IGMISflTION: El NO. PEAKS: 397/ 42 BflSE/HRLF INT: 5G045./ 5G043. TIC: 656330./ 276120. 13SO RANGE: 149.9904 - 654.9201 IETN TiriE/riISC: 34: 3/ SO/ 2/ 51 PEftK HO. NEftSURED I 2 3 4 5 G 132977. 4 1^0512. 103174. 5 6 6 mss 1S5757. 19G04G. 19G572. ~7 I 19G843. 110 111 333.0175 112 113 114 115 116 117 110 119 381.0945 128 121 122 123 124 125 126 127 120 129 130 131 132 133 134 135 136 137 133 139 140 381.9047 301.7877 380.3761 300.0361 303.8097 383.5241 373.0450 379.0074 370.9777 370.0209 377.9242 377.0139 377.4177 377.0211 376.0448 376.8120 376.6392 375.8207 375.7563 374.9383 374.0636 374.8249 374.5739 373.0232 373.7567 373.3094 372.0259 37 1 . 8393 370.I395G NO. POINTS 4 5 6 5 12 5 6 25 8 4 6 8 ABSOLUTE % INT, Z INT. * TOT. HREF ION INTENSITY BflSE 174. 257. 455. 29G. 207. 218. 334. 206. 1219. 247. 290. 732 l.V" 637. 172. 423. S09. 0.3 0.5 8.8 0.5 0.4 9.4 e.G 0.5 2.2 0.4 0.5 13.1 1.1 0.3 0.8 1.6 17 10 4237. 473. 7.6 21 5 25 4 6 3746. 6.7 0.5 33.7 0.3 0.5 2.8 7.3 8.3 77.5 0.4 0.3 2,7 12.5 8.3 10 12 4 29 5 0 0 17 4 29 6 6 17 35 4 2G3. 13075. 158. 290. 1505. 4116. 149. 43409. 212. 442. 1506. 7016. 172. 56045. 439. 406. 5474. 34259 . 153. 0.0 100.0 0.8 0.7 9.3 61.1 0.3 — 0.5 0.4 0.5 1.1 0.3 0.3 1.6 7.6 6.7 0.5 33.7 0.3 0.5 2.8 7.3 0.3 77.5 8.4 2.7 12.5 0.3 103.0 0.0 0.7 9.8 Gl.l 0.3 8.05= 0.0 0.8 9.0 0 0 . 0.0 0.1 0.8 0.2 0.0 e.0 1.1 0.1 0.8 0.0 0. 1* 0 . 6* ! O.t) O.G! 0.0 2.9! 0.0 0 0 . 0 . 2* 0 . 6* I 0.8 6.6! 0.8 0.0 0 . ?.# ! 1.1*! 0.0 3.5! 0.8 0.1 0.8! 5.2! 0.0 u c �):T%1S1. DP0:TD1S1.MS SCftN: 443, 3/11/02 14:51 l O N I S A T I O r i : El NO. PfmiCJ: 314/ 7 BftGE/NREF I N T : 41005./ 14330. TIC: 379200./ 943G. MPS5S RnHRE: 143.9904 - G53.0029 RETN TINE/NISC: 34: 7/ 03/ O/ 41 PEAK NO. MERSURED MHSG j 2 3 4 5 G 90 99 100 4H654. 120001. 175536, 194751. 135363. 193454. 302.8541 331.9636 331.GDG2 331.6930 300.3761 379.0144 379.5494 373.9053 373.0759 378.3295 377.0033 376.0093 375.0207 374.3054 374.0201 373.0726 373.0137 373.7593 372.8559 372.0143 372.Q1GG 37 1 . 0790 371.0150 101 182 183 104 185 IBS 107 138 103 110 111 112 113 114 115 116 117 118 119 120 NO. POINTS 6 4 5 5 5 5 6 3 6 0 17 6 4 4 0 G 29 12 23 5 14 6 25 4 6 14 6 5 21 ftDSOLUTE % INT. X INT. HREF BflSE INTENSITY _ i.e 431. 0.5 200. 0.6 235. 0.0 347. 0.6 233. 0.7 282. 2.7 0.9 396. 433. 1.0 2.3 O.S 341. 1.4 4.0 575. 9.4 3912. 2.5 365. 0.9 1.2 0.4 170. 107. 0.4 3.6 1.2 510. 1.0 0.6 260. 16.9 40.7 7077, 4.2 12.0 1745. 25.3 72.0 10573. 0.5 200. 11. G 40 . 1679. 3.0 1.1 443. 34. G 1QO.O 14530. 1.4 204. 0.5 2.2 0.8 317. 6.0 074. 2.1 2.6 301. 0.9 1.6 233. 0.6 54.4 10.9 7301. TOT. ION 0. 0. 0. 0.0 0.1 8.0 0.1 0.1 0.0 0.2 1.0 0.1 0.0 0.0 0.1 0.0 1.3 0.5 2.0 0.1 0.4 0.1 3.8 8.1 0.0 0.2 0.1 0.1 2.1 o �*.. DP0:Tnisi.MS SCON: 3/11/02 14:51 lONISHTIOH: El NO, PEOKS: 278/ 2 DftSE/NuEF INT: 43571./ 7635. TIC: 330112./ 2553. I^SS RftllGE: 149.SS04 - 654.0452 RETH TIME/MISC: 34:ll/ G5/ I/ 56 PERK NO. 1 2 3 4 5 6 90 91 32 93 94 95 96 97 98 99 100 181 132 103 194 105 186 287 103 103 HEnSURED MftSS 13514. 31749. 34225 . 92946 . 194961. 195553. 384.4293 383.8317 302.9715 301.0258 300.9761 379.8166 378.9773 378.0634 377.8338 377.315B 376.8212 375.0262 374.9922 374.8219 373.9602 373 . 8244 372.C190 371.5204 371.8335 371.6604 MO. POINTS ABSOLUTE INTENSITY 6 5 6 6 10 5 5 5 5 12 17 6 5 5 25 4 5 25 4 437. 276. a 8 21 0 5 17 4 380. 314. 646. 250. 256. 213. 258. 715. 5089. 314. 272. 268. 2387. 191. 305. 4512. 140. 326. 627. 7635. 363. 277. 3360. 174. X INT. % INT. ?{ TOT. ION HREF BftSE _ 0.1* 1.1 0 0 . 0.7 0.0 0.7 8.3 0.1 0.2 1.6 0.0 0.6 8.0 0.6 3.4 0 0 . 2.8 0.5 3.4 fl.fi 0.6 0.2 1.8 9.4 1.5 12.5 0.1 0.8 4. 1 0.0 0.7 0 0 . 0.7 3.5 0.7 5.9 31.3 0.1 0.5 2.5 0.0 4.0 0.8 1.4 11.1 59.1 0.0 0.3 8.1 8.8 4.3 0.2 8.2 1.5 2.3 100.0 18.3 0.1 4.8 0.9 0.8 3.G 0.7 44.0 1.0 8.3 2.3 e.i 0.4 �PP0:TD151.M3 SCflN: 445, 3/11/02 14:51 TON I G O T I O N : El HO. PEHKS: 273/ 6 BaSE/HREF I N T : 44193./ 3419. TIC: 333G64./ 10673. MflSS RflHGE: 149.9904 - 654.2093 RETN TI1G/NISC: 34:15/ 72/ 3/ 41 t-EHSURED HftSS • HO. POINTS ABSOLUTE INTENSITY : INT. BHGE % INT. NREF X TOT. ION _ 1 2 3 4 5 6 94 95 96 97 90 99 180 181 1B2 103 184 105 106 107 108 103 14750. 31467. 33745 . 93326. 113296. 102609. 3C i . 9603 300.9761 \ 300.9513/ 30:0.0020 370.9693 377. 7965 376.G327 375.8399 375.0062 374.0065 373.0586 373.0129 372.0947 371.9090 371.0300 370.9711 8 6 6 4 4 8 4 14 0 13 6 6 4 0 14 8 10 14 B 4 21 5 462 397 366 151 174 464 134 3245 357. 350. 175. 407. 3419. 561. 1800. 3245. 408. 167. 2344. 204. 1.0 0.9 0.0 0.3 0.4 1.0 8.4 7.3 4.3 0.5 0.3 0.0 0.4 1.1 7.7 1.3 2.3 7.3 0.9 0.4 5.3 0.5 0.1* 5.7 55.3 G.5 10.2 5.1 14.2 100,0 16.4 29.2 94.9 11.9 4.9 68.6 6.0 0.1 0.1 8.0 0.1 0.1 0.1 1.0;!0 . G:::1 0.0 0.1 0.1 0.1 0.1 1.0! 0.2 0.3 1.0 0.1 0.1 0.7 0.1 �DPQ:TDTS1.MS SCflN: 44G, 3/11/02 14:51 lONISnTIO!!: E l NO. P!£n!<3: 259/ 0 8nSE/NREF : INT: 42934.x 3739. TIC: 307584./ 14414. MSSS RflNHE: 143.9904 - 654.9601 RETN TIME/MISC: 34:20/ 73/ I/ 38 PEOK HO. MEASURED HflSS HO. fiBGOLUTE n INT. % INT. POINTS INTENSITY BH3E NREF 4 G 5 G G 6 6 10 4 6 10 4 25 8 5 6 8 f\ 4 25 5 10 17 6 G 8 165. 504. TOT. I OH _ I 2 3 4 5 6 7 30 91 32 93 94 95 96 37 98 33 100 101 102 103 1G4 185 10G 107 100 32271. 33033. 33C22 . 1204S3. 134800. 195273. 136530. 3Q3.7321 303.0029 302.3130 301.9313 301.7953 3G0.9761 379.9918 379.0442 379.8212 370.9361 377.9578 377.8260 375.0229 373.9038 373.0603 373.0126 373.5048 372.0154 371.0227 217. 209. 313. 352. 2^6. 1392. 135. 49 1 . 45 1 . 160. 3027. 516. 190. 333. 420. 159. 140. 2678. 219. 530. 2255. 334. •430, 670. 0.4 1.2 0.5 0.5 0.7 0.8 0.6 3.2 0.5 1.1 1.1 0.4 7.1 1.2 0.4 0.8 1.0 0.4 0.3 G.2 0.5 1.4 5.3 0.9 1.1 1.6 37.2 5.2 13.1 4.3 13.0 5.1 9.0 11.2 4.3 3.7 71.6 5.9 15.5 GO. 3 10.5 13.1 17.9 0.1 0.2 0.0 0.0 0.1 0.1 0.0 0.5 G.O 0.2 0.1 0.1 1.0 0.2 0. 0. 0. 0. 0.0 0.9 0.0 0.2 0.7 0.1 0.2 0.2 �DS-55 CROSS SCflN REPORT, RUN: FDS3 + TIC ,„, . 4 : 0 8 10:44 17:33 24:22 ^c 31:11 38:60 44:49 51:38 58:27 90 89 79 60 50 40 30 20 10 108 T" n~ TT-T"T"r~r"i~"r T~T~ TTT 200 300 300 �.'• ari> 'BS-55 CROSS SCflH R E P O R T , RUN: * 270 w 366 0 346 100. 4:Q0 10:44 17:3? 24:22 100^=77948 90. C. :11 33:00 44:49 51:33" 53: 27 B0e 600 revj j 1 80 70. 60. li 40. 39. 19. , n 1 1.A.A i r . -i & i i if i i L* $v \ i i 50. ^Afvi^H*!i^^^..von-^uY«i^wi*V J Ar ' y^/| VVi^M^, L 1 ^ f i^,. iM . ^.-...J^T/ W^^vw^^Mi i 100 see see 400 R 3 _£'%<& HS-55 CROSS SCflH R E P O R T , R U M : FBS3 ~ " * 374 * 408 0 444 + TIC 16:44 17:33 24:22 31:11 33:00 100 4:08 90. ^100/. = 2972736 ~ 44:49 51:38 5r j;^^ ^^ 53: 27 j 100-^78156 80. 'see . 1 T 60. 40. 30. 20. 10. ALU^^^'V^-, Q. • s L fi'i / "' it * 1 i'lftLli " i_l *"""' i i T7| jlJ i ' 1 100 20Q 3ou 4 1 'J "Vv^jL- •^-»"1 l^jcjl j*-*»•i-^f.-L^.*- ^.-i--v^-. ._ TtC ' CG i ^5-£- — — J _ f — ^ -«> — ,, _ — - . - . 1. H 1 1 �:>VA or ^'V'J-\t\ 1> i-'i FDS3.242 C T I C = 6 1 2 9 9 2 , lv3Q':=315413 El 272 80 308 229 '150 280 250 i^HwmL—,,—. .—, .300 R . 00 F B S 3 . 3 1 1 C T I 0 7 9 S 7 1 2 , 10^=433433 F.I 3 06 400 '450 00 �•" Vj^CfK^v. "t~L*- c 'ti 3-' FDS3.311 C T I C = 795712, 10f1"i=4i3433 El 396 <%.CDF 90_ 4~ "_ 334 60_ 50_ 49_ 30_ 2«. 241 264 153 171 10_ i 1 jliJui^LLJi^^ lujL isL^^y i4^ 158 290 258 300 | | | 1 0 L I i 'n 4^V-MwWr^'l-^1HfVt^H-T--rtl '. 1 .' , )', 'l • 480 50 '450 '400 4 SO FDS3.454 CTIC=868320, 100'-S=772243 374 109 09 70 40 311 137 0 I 150 f76 I JJ^LwSf4fJri!t^^iijL^^v^^ 200 250 }> .309 « ^ . 5 3 0 001 �F B S 3 . 4 3 0 C T I C = 430960. 1 00-:- 1 1 532 ] El 106_ 374 "-, 80_ 7Q_ c.ft bu_ 59_ 207 49_ 30_ 239 350 ^'|7t t« 1* . 394 1®.. 1S2 493 425 0 R lijWilii.1uLiliLjiij i i r i i ] i t ri 00 ^ ~rr"r lL '459 �498 98 8. 8 78. 68. 58. 49. 39. 275 £0. 173 343 204 18. l 1E0 -2Qe 258 '380 L 3GO 400 .',,'. , j, Jl 4Se FDS3.520 C T I C = 524329, 1 9 ' = 19637] F.I 0'. 468 100. 90. 89 79 6,0 172 347 150 200 ^ see .300 bco Ueo teoo �J FDS3.617 CTIC=467296, 100^=86793 El 444 109 287 *• 90_ 89_ 70. 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I 44:50 I » < 1 I I I I I ,| 30 30 70 :o jj 40 30 20 10 0 A_A_./U.— <>: — i �co/rYA- <j<lf \'-£u I v \ ' - u Ivyf TxH.i CTIC=372336, 100?J=424n E! rift. 'V7 - - • f- O^S tool., 4 <v>i\*f» '. \] 100 CO 70 1G9 ! 101 20 134 254 ?07 10 213 2P9 -HT-:n n IT"] i i ion Ti i I i I 241 n i rr 2-10 i l i �PN255.1 CTIC=38148S, 100r;=75173 El 100 ~00 90 CO 70 GO 40 -I 230 20 207 10 1G9 1 50 2G3 ;93 j i • 175 : iiS i I I I T I I I I 350 �0 HXN.l CTIC=155G44, 100%=1C9523 E! 100 334 CO 70 GO 50 264 20 10 f 312 1 7 192 i I J 229 !! i I i j 1 I | i 200 ! i i l! i ! . I ! i 2E7 ,,, !• j I ! I h ! 1 j | i 1 1 2:"0 1 !i t 1 , I ! 1 1 275 I I 1 1 . 1I 1 ! 1I 1 i!Ui i i i i •350 �>< . ro Cl ?.26 TV' i i ~]rJT i < I^T^ i " i j i i'-r-.f "y~"r"r-T-rT •;•<-.-> L —•- �• 3 . CTIC-Toj'lj, 1002=2159:1 El T 332 fr n~ 'i~!Ti I i i I I rr i 1 1 M i i i M i r'i i i i "i T 1 1 "iTn 1 1 1 1 1 1 M i 1 1 i i i i M i 1 1 1 rn iT"n"n"rrrnTr'f!T!'i r � Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Title A name given to the resource Alvin L. Young Collection on Agent Orange Description An account of the resource <p style="margin-top: -1em; line-height: 1.2em;">The Alvin L. Young Collection on Agent Orange comprises 120 linear feet and spans the late 1800s to 2005; however, the bulk of the coverage is from the 1960s to the 1980s and there are many undated items. The collection was donated to Special Collections of the National Agricultural Library in 1985 by Dr. Alvin L. Young (1942- ). Dr. Young developed the collection as he conducted extensive research on the military defoliant Agent Orange. The collection is in good condition and includes letters, memoranda, books, reports, press releases, journal and newspaper clippings, field logs and notebooks, newsletters, maps, booklets and pamphlets, photographs, memorabilia, and audiotapes of an interview with Dr. Young.</p> <p>For more about this collection, <a href="/exhibits/speccoll/exhibits/show/alvin-l--young-collection-on-a">view the Agent Orange Exhibit.</a></p> Text A resource consisting primarily of words for reading. Examples include books, letters, dissertations, poems, newspapers, articles, archives of mailing lists. Note that facsimiles or images of texts are still of the genre Text. Box The box containing the original item. 087 Folder The folder containing the original item. 2194 Series The series number of the original item. Series IV Subseries II Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Creator An entity primarily responsible for making the resource Smith, R. M. D. R. Hilker P. W. O'Keefe S. Kumar K. M. Aldous Description An account of the resource <strong>Corporate Author: </strong>Toxicology Institute, Center for Laboratories and Research, NYS Department of Health, Albany, New York Date A point or period of time associated with an event in the lifecycle of the resource 1982-03-01 Title A name given to the resource Determination of Polychlorinated Dibenzofurans in Soot Samples from a Contaminated Office Building Subject The topic of the resource BSOB PCBs analytical studies https://www.nal.usda.gov/exhibits/speccoll/files/original/853b047330bd474a0bc02eb0ee2e5c84.pdf 73689b98be00e93815db3d804a567c57 PDF Text Text Item D Number 02133 Author Smith, P.M. Corporate Author ROport/APtlClO HUB Typescript: Analysis of a Binghamton Soot Sample for Tetrachlorodibenzofurans and Tetrachlorodibenzo-pdioxins, October 1, 1981 Journal/Book Title Year Month/Day Color Number of Images D 21 Descrfyton Notes Thursday, September 20, 2001 Page 2183 of 2293 �Analysis of a Binghamtcm Soot Sample for Tetrachlorodibetizafurans and ;" --Tetrachlorodibenzo-p-dloxins R.M. Smith., D.L. Hilker, P.W. O'Keefe, S. Kumar, J. O'Brien, B.L. Jelus-Tyror, K. Aldous October 1, 1981 �INTRODUCTION A fire caused by a malfunctioning PCB-filled transformer in the Binghamton state office building on February 6, 1981 released an unknown amount of incomplete combustion products into the 18-story building. A sample of soot (Tox. No. 811711965) was collected from an unspecified area * u of the building using a vacuum cleaner. " A portion of the homogenized soot, intended to be used for animal toxicology studies, was soxhlet extracted for 16 hrs in benzene and analyzed for TCDF's and TCDD's by capillary GC/High resolution mass spectrometry (HUMS). PROCEDURE Fifty yl of the benzene extract (corresponding to 46 mg soot) was spiked with 6 ng of 13 C labelled 2,3,7,8-TCDD and cleaned-up prior to GC/HRMS injection using sequential liquid chromatographic columns containing PX-21 adsorptive carbon, 2% deactivated silica gel, and activated Florisil. An .-.-!. ;. aliquot of the concentrated sample was then injected onto a 40 m x 3 mm OV275 coated soda glass GC capillary which is interfaced to the MS-50 HRMS through a jet separator. The temperature was appropriately programmed and mass profile data was accumulated for the m/e 306 CTCDF), 322,320 (TCDD) and 334 (13C TCDD) ions. 13 Standards ( C 2,3,78-TCDD and unlabelled 2S3,7,8-TCDF) were run. prior to sample injection. A control sample of Fisher activated coconut charcoal was similarly spiked and analyzed. RESULTS AND DISCUSSION The sample was found to contain a complex mixture of TCDFs as shown in the chromatogram in Figure 1. present. At lea'st twelve distinct TCDF peaks are 2,3,7,8-TCDF eluted as peak No. 12 as determined by comparison with an injection of authentic 2,3,7,8-TCDF. Trie presence of amounts of tetrachloroclibenzo-p-dioxicis in the sample are indicated by the M3 chroma tog ram �—3- in. Figure 2. Closer inspection of the data revealed the presence of an interferent. However the data system allowed consideration of -the intensity due to tetrachlorodioxin ions which were partially resolved from the interferents (Figure 3 . ) The interferent appears at an m/e value very similar to that of the [M ~C1] fragment of heptachlorobiphenyl. Signal detected in the dioxin ion position in the m/e 321.8936 mass region, which occurred at the same time in the chromatogram as the being due to native 2,3,7,8-TCDD. C-2,3,7,8-TCDD were taken as This implies a relative retention tine of 1.00 for native 2,3,7,8-TCDD. The quantitative results of the analysis of the. samples are summarized in Table I. and TCDD. The figures given in the table denote only "detectable" TCDF The sample cleati-up procedure that was used requires the use of isotypically labelled standards to correct for low recovery. Presently, no labelled TCDF is available and the assumption was made that the recovery of all TCDF and TCDD isomers was the same as that of the 13 C labelled 2,3,7,8- TCDD internal standard based on preliminary TCDF recovery experiments. Although the capillary GC column gives a high degree of isomer separation, the analysis should not be considered completely 2,3,7,8-TCDD or TCDF isomer specific as other isomers may co-elute. The unexpectedly large amounts of TCDFs found in the sample exceeded the linear range of the HEMS, making a second injection using less sample necessary (Fig. 4) for proper quantitation (All calculations and several important mass profiles are included in the appendix). No TCDDs or TCDFs were found in the control carbon. The results show that concentrations of TCDDs and TCDFs in this soot appear to be similar to those found in soot TOX No. 811710280 and air particulate sample Tox No. 811710977 previously taken from the Binghamton state office building. �u TIME: Ml 166 �B-S55 HIGH RESOLUTION MPM .» • RUNNRME FDHM3 DOTE 7/10/81 TT-H TIME G9:30 L 05:30 1 1 10:30 1 TIME 21 :11 20:30 1 ,* ?5:30 ric Ml 12 13 14 . 105 1 209 313 41? *DL * DRTE 7/10/81 TIME 21:11 RUNHRME FDHM8 SWEEP 300 (PPM) SCRNTIME 0.3 (SECS) MRSS 305.8936 SCflNS 194-205 100'-S INTENSITY 143676 100 75 305.8527 305,8986 395.9445 �R U N N f l M E FTJHM9 •MBSS 321.893B SC.RNS 149-433 IIRTE 7/1D/81 TlM'E 21 i l l SWEEP 389 ( P P M ) S C f l N T I M E 0.3 I N T E N S I T Y 442547 CSECS) 109 25 321.8452 *BL HOU KRNY RRERS73* 321.8935 DSSS HIGH RESOLUTION MP« PERK SUtlilRTION REPORT RUNNflJIE FBHM8 DOTE 7/10/81 TIME 21 i l l MOSS 321.8935 389 PPM SCflN WIDTH SCRN TIME 6.3 SECS SCRN NUMBERS 149- 438 STRNDflRD FflCTOR 0.6899 0 KflMINSKY'S BING. SOOT 2.S5 OF 9.0UL MPSS ITEM CENTROID ' 321.8789 TOTRL 321.8733 1 321.9021 2 321.9331 3 RREfl - 'BRSELIHE BRSELINE SUBTRflCTED SKIMflED 32772100. YES NO 27343790. YES NO 5367326. YES NO 61077. YES NO •<TOTfiL RELATIVE RRER TO STflNBRRB 95.17 0.00 79.41 0.00 IS.59 0.G0 Q.18 0.00 �bfcC0JUft • 720 SCITSS6A HIGH RESOLUTION MPM •„• RUNNflJlE TDHM4 DflTE 7/16x81 "I vit -*- *>/ ** TINE 12i28 RETN TltlE ,60:39 , ,03:39 ^16:39 n- .* 2 : 3 a . f t20130 TIC 305.8986 '^l 060255 Ml M2 ?=Ty^y2^?" 1 • ~T r- 105 1 1 209 *DL * DS55 HIGH RESOLUTION MPM RUNNflJIE TDHM4 DfiTE 7/16/81 RETN TIME 69:39 rw r"' •™""r"—r* 313 r 417 TIME 12:28 04 ;39 20! 38 . 313 *DL * 180'-S» 1869255 '4 1 ? �Table I. Results for Sample 811711965* TotalVpuran Concentration - 597 ppm (Detection Limit = 2.3 ppm) 2,3,7,8-Furan Concentration - 48 ppm (D.L. - .45 ppm) Total Dioxin - 1.8 ppm (D.L. = .04 ppm) Ratio 320/322 = 0»87 2,3,7,8-Dioxin - 1.2 ppm (D.L. =.008 ppm.) Ratio 320/322 = 0.86 Recovery - 4% Amt. of 13 C-2,3,7,8-TCDD spike - 6000 pg Weight of Sample - 46 ing Cone, of Spike - .13 ppm Relative Retention Times: 2,3,7,8-tetrachlorofuran - Standard: .1.264 Sample: 1.269 2,3,7,8-tetrachlorodioxin - Sample: 1.00 No TCDF or TCDD was found in the control carbon sample �_APPENDIX: Supplementary Data 1. Carbon blank 2. External standards 3. Mass profiles 1st injection-Runname FDHM8 4. Second injection data-Runnarae TDHM4 5. Calculations �DS55 HIGH RESOLUTION MPM RUNNRME: FBHM? DRTE RFTH TIME 60; 30 t • 85; 39 r1"" TINE 20»26 15i39 . f 25:38 'TIC Ml M2 «3 N4 101 **> 201 301 T" �BS55 HIGH RESOLUTION MPM •RUMNRME FBHMb DOTE 7/18/81 RETt) TIME 03:39 J TIC M2 M3 M4 03:39 j i 06:30 J TIME 19:43 L 89:38 j L. 12:39 15 �-T<rr>1L linear ravine m » sT RUNNflME FDHN8 DflTE 7/10/81 TIME 21jll MflSS 395.8986 SUEEP 300 (PPM) SCRNTIME 8.3 CSECS) SCRNS 149-438 188'< INTENSITY ?9?1778 108 305.8986 395.8527 *SK OREO IBt2 DS55 HIGH RESOLUTION MPtt PERK SUMMRTION REPORT RUNNflUE FDHM8 DflTE 7/10/81 TIME 21 ill MOSS 3D5.8987 SCRN UIDTH 300 PPM SCflH TIME 0.3 SECS SCflN NUMBERS 149- 438 STflNDflRD 6.0000 FRCTOR 0 KRMIHSKY'S BING. SOOT 2.55 OF 9.8UL MRSS CEHTROID 305.9972 3Q5.8716 385.9972 305 .9333 ITEM TOTRL 1 2 3 RREfl 585240398. 1871699. 551408180. 1415924. BRSELINE BRSELINE SUBTRRCTED SKIMMED YES HO YES NO YES YES YES NO '•iTOTRL RELRTIVE RRER TO STflNDRRD 98.97 6.00 0.32 0.0Q 93.25 0.60 0.24 0.C0 �FHHK§ DATE! 7/10/81 TIME: 21111 MOSS 333.9335 SUEEP 399 (PPM) SCRNS 279-307 10ET-S INTENSITY 4589 SCRHTIME 0.3 CSECS) 333.9335 333V8835 333.983^ BS55 HIGH RESOLUTIOH MPJ1 PEflK SUMMflTION REPORT RUNNfiME FDHM8 DflTE '7/10/81 TIME 2It'll MflSS 333.9336 SCflH U1TJTH 309 PPM SCflN TIME 8.3 SECS SCRN NUMBERS 279- 307 STRNBflRD 0.0000 FflCTOR 0 KflMIHSKY'S BIHG. SOOT 2.SS OF 9.0UL MfiSS CENTROID 333.9351 333.8982 333 .9402 333.9746 ITEM TOTOL 1 2 RREfl 319029. 44037. 223488. 17729. BRSELINE BflSELINE SLIBTRRCTED SKItlMED HO YES NO YES YES YES NO YES •<TOTPL RELRTIVE RRER TO STRHDRRB 66.S4 e.ea 9.19 0.00 46.61 0.08 3.70 0.08 �U.3 ISECS) •SCRNS 279-397 188** INTENSITY 83676 109 25 321.8935 321.84S2 321.9418 DSB5 HIGH RESOLUTION MPW PEflK SUMMRTIOH REPORT RUNHRME: FDHMS DRTE TIME MflSS 321.8935 SCflN WIDTH 308 PPM SCffN TIME 8.3 SECS SCflN NUMBERS 279- 307 STBMDflRD 0.8008 FflCTOR 0 KRMINSKY'S BIHG. SOOT 2.55 OF 9.8UL MflSS CEHTROID 321 .8323 321 .8748 321 .9023 321 .9319 ITEM TOTflL 1 2 7275879. 5220057. 2050417. 5485. BRSELINE BRSELINE SUBTRfiCTEET S K I M M E D HO YES YES YES YES HO NO NO RELfiTIVE flREfl TO STRNBflRD 97.33 8.00 69.83 0.QO 27.43 0.08 0.07 0.00 v.TOTOL �•RUNNRME FDHMB J3RTE 7x10x81 TIME 21 11 MRSS 319.8964 SUEEP 300 (PPM) SCflNTIME 0.3 (SECS) SCflNS 149-438 1.00*4 INTENSITY 89622 180 25 319.8483 *SK RREfl JD:2 319.94?S ~3T9.89~S"4" DSB5 HIGH RESOLUTION MPM PERK SUMMATION REPORT RUNNRtlE FDHM8 BflTE 7/10x81 TIMESltll HflSS 319.8965 SCflN UIBTH 300 PPM SCRN TIME 0.3 SECS SCON NUMBERS 149- 438 STflNDflRB 0.8009 FfiCTOR 8 KflMINSKY'S BING. SOOT 2.55 OF 9.0UL MflSS CENTROID 319.8972 319.8596 319.8930 319.9319 ITEM TOTRL 1 2 E364537. 79597. 46853S7. 66501 . 3RSELINE BRSELINE SUBTRflCTED SKIMMED HO YES NO YES YES YES NO YES "sTOTflL RELPT1VE RRER TO STRNDflRD 72.82 6.00 1.98 C.B0 63.60 0.B8 8.99 0.0B �.MOSS 305.8936 SWEEP 390 (PPMl SCPHS 338-406 109'-: INTENSITY 31138 SCFWTINE 0.3 (SECS) 1,39 305.852? 305.8986' DS55 HIGH RESOLUTION MPM PERK SUMMflTION REPORT RUHNflME TDHM4 BRTE TIME 12»28 MOSS 305.8987 SCOH UIDTH 309 PPM SCON TIME 0.3 SECS SCflH HUMBERS 388- 406 STflNBPRD 0.0009 FflCTOR 0 l.PUL D-ILUTIOH OF KflMINSKY'S SOOT MPSS ITEM CEHTROID 395.8933 305 .8613 305.8938 335.9392 TOTflL 1 2 3 flRER 2859185. 14863, 1917649. 11737. BflSELIHE BRSELIHE •SUBTRflCTED SKIMMED HO YES HO YES YES YES NO YES VTOTflL RELfiTIVE RREfl TO STRHDP.RB 6.00 95.36 0.00 0.69 89.20 0.00 0.55 0.00 �I 1 1 t n I I !_ i JJ I 1 1 > I •MOSS 305.8986 SUEEP 300 (PPtli SCRHS 214-478 189V: INTENSITY 379262 SCflNTIME 8.3 (SECS) TcD'f Joe 306.8527 30'6.8986 80S. 9445 DS65 HIGH RESOLUTION MPtt PERK SUMMflTION REPORT RUNNflME TBHM4 DflTE .7/16x81 T I M E 12$28 MflSS 385.8987 SCflN W I D T H 300 PPM SCPH TIME 8.3 SECS SCflN NUMBERS 214- 478 STflHDBRB 8.0080 FflCTOR 8 1.0UL B'lLUTIOH OF KRMIHSKY'S SOOT MRSS CENTROID 305.8948 305.8611 305.8948 385.9309 ITEM TQTflL 1 2 3 flREfl 25127260. 64216. 24077639. 73307. BRSELINE EflSELINE 'SUBTRflCTED SKI TIMED YES NO YES HO YES YES YES HO '-iJOTRL RELRTIVE RRER TO STRNDR.RB 92.56 0.08 0.24 0.08 88.70 8.08 0.27 8.00 �Calculation of Response Factor of Furau to Dioxia Asit of TCDF injected = 1.2 yL of 150 pg/uL Int of TCDF con = 677482 Sensitivity = 677482/180 = 3764 counts/pg Amt of 13 C TCDD injected ~ 1.0 uL of 600 pg/^L Int. of TCDD ion = 1949179 Sensitivity = 1949179/600 = 3249 counts/pg. Response Factor of Furan is 3764/3249 « 1.16 For equal amounts of material, the response of TCDF is 1.16 times 13 C TCDD, �Calculation, of Furan in peak number 1 (this peak was used as internal furan standard for the second injection) Amt Furan = X305 x <Amt 13c I / 334> *R -F- 1305 = intensity of m/z 305 ion for peak no. 1 (the small peak delimited which has not saturated the amplifier) = 8596844 Anit|, = Amt of 1J C = 6 ng C-TCDD spike (internal std.) added to sample I334 = intensity of m/z 334 ion (int. std.) = 223480 R.F. = response of 2,3,7,8-TCDF compared to 13C 2,3,7,8-TCDD =1.16 Amt Furan = 8'597x ^6 ng/.223480) x 1.15 - 268 ng �Calculation of 2 , 3 , 7 , 8-TCDF ^ 3 8 = J2378X 2 7 Amt2378 = amt of 2, 3 ,7, 8-TCDF I 2378 = intensity of 2,3,7,8-TCDF ions = 1917649 , « amt of furan in peak 1 = 268 ng I = intensity of furan in peak 1 = 235188 = 1.918 x (268/235) - 2187 ng Conc2378 = 2187 ng/46 mg «= 48 ppm Calculation of Total TCDF - ITOT = 24. -78 x (268/.23S) *= 27459 ng Cone = (27459 ng/46 mg) = 597 ppm �Calculation, of 2,3,7,8-TCDD (scans 279-307) 1 2378 X -^Vj » 2.050417 x (6/.223480) =* 55.04 ng Conc___ — 55.0 ng/46 mg Z3/O =1.2 ppm CalcualtiQn of Total TCDD (scans 149-438) Ant TOT =1 x (Ant 13 C/Io ) = 5.367 x (6/. 395528) = 80.4 ng ac23 - = 80.4 ng/46 mg — 1 . 8 pptn � Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Title A name given to the resource Alvin L. Young Collection on Agent Orange Description An account of the resource <p style="margin-top: -1em; line-height: 1.2em;">The Alvin L. Young Collection on Agent Orange comprises 120 linear feet and spans the late 1800s to 2005; however, the bulk of the coverage is from the 1960s to the 1980s and there are many undated items. The collection was donated to Special Collections of the National Agricultural Library in 1985 by Dr. Alvin L. Young (1942- ). Dr. Young developed the collection as he conducted extensive research on the military defoliant Agent Orange. The collection is in good condition and includes letters, memoranda, books, reports, press releases, journal and newspaper clippings, field logs and notebooks, newsletters, maps, booklets and pamphlets, photographs, memorabilia, and audiotapes of an interview with Dr. Young.</p> <p>For more about this collection, <a href="/exhibits/speccoll/exhibits/show/alvin-l--young-collection-on-a">view the Agent Orange Exhibit.</a></p> Text A resource consisting primarily of words for reading. Examples include books, letters, dissertations, poems, newspapers, articles, archives of mailing lists. Note that facsimiles or images of texts are still of the genre Text. Box The box containing the original item. 087 Folder The folder containing the original item. 2183 Series The series number of the original item. Series IV Subseries II Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Creator An entity primarily responsible for making the resource Smith, R.M. D.L. Hilker P.W. O'Keefe S. Kumar J. O'Brien B.L. Jelus-Tyror K. Aldous Title A name given to the resource Typescript: Analysis of a Binghamton Soot Sample for Tetrachlorodibenzofurans and Tetrachlorodibenzo-p-dioxins, October 1, 1981 Subject The topic of the resource BSOB PCBs analytical studies