1 15 1 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