1 15 11 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. 092 Folder The folder containing the original item. 2314 Series The series number of the original item. Series IV Subseries IV 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 Di Domenico, Alessandro Vittorio Silano Giuseppe Viviano Giovanni Zapponi Source A related resource from which the described resource is derived Ecotoxicology and Environmental Safety Date A point or period of time associated with an event in the lifecycle of the resource 1980 Title A name given to the resource Accidental Release of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) at Seveso, Italy Subject The topic of the resource soil testing plant testing building remediation analytical studies 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. 088 Folder The folder containing the original item. 2218 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 Silbergeld, Ellen K. Title A name given to the resource Letter: from Ellen K. Silbergeld to Robert Huffaker, January 25, 1983 Subject The topic of the resource BSOB dioxin analytical studies health monitoring https://www.nal.usda.gov/exhibits/speccoll/files/original/d18c92ba1c7b5858ce473a3255575d2e.pdf fc5119254c705b4269445699dfd21b7f PDF Text Text Item D Number °2212 Author Gierthy, John F. Corporate Author RODOrt/APtlClO TItiB Typescript: A Preliminary Report on the Evaluation of an In Vitro Assay for the Detection of "Dioxin-Like" Activity Using Extracts of Soot from the Binghamton State Office Building, 1982 Journal/Book Title Year Month/Day Color Number of Images D 28 Thursday, September 20, 2001 Page 2212 of 2293 �A Preliminary Report on the Evaluation of an In Vitro Assay for the Detection of "Dioxin-Like" Activity Using Extracts of Soot from the Binghamton State Office Building ~? "by John F. Gierthy and Gerald D. Frenkel New York State Department of Health Division of Laboratories and Research �.V " ' Abstract. As a result of the involvement of an electrical transformer containing polychlorinated biphenyls (PCBs) and chlorinated "benzenes in a fire in the Binghamton State Office Building (BSOB), the structure was contaminated vith soot ladened with dioxin congeners and isomers, which included 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8 TCDD) and 2,3,7,8-tetrachlorodibenzofuran (2,3,7,8 TCDF). A panel of experts, which was convened to examine decontamination procedurestrecommended the development of a short term assay for these compounds, based on an in vitro model of the in vivo chloracne response to dioxin exposure. This assay uses the dioxininduced keratinization of epithelial cell cultures as an endpoint. This endpoint is evaluated by eye, using intensity of the keratin specific stain, Rhodamine B, as a marker. This report describes the evaluation of the potential utility of such an assay as a rapid, semiquantitative screen for monitoring the BSOB decontamination process. Initial experiments using a 2,3,7,8 TCDD standard established that the kera.tinization model could be duplicated in this laboratory. A soot sample from the building for which levels of 2,3,7,8 TCDD and 2,3,7,8 TCDF had been determined by mass spectrometry, was tested in this in vitro system. The resulting activity was of the same order of magnitude as expected from the content of TCDD and TCDF as determined in the mass spectrometry analysis. Twelve extracts of soot from various floors of the building were tested for their activity in the assay. Activity of soot extracts from the various floors ranged over three orders of magnitude with samples from the lower floors generally having lower activity. These studies have also lead to the observation that after exposure to 2,3,7,8 TCDD, cells in the assay undergo a change in morphology characterized by the appearance of flat, apparently nonproliferating cells. This change in morphology, when used as an endpoint, correlated well with the keratinization endpoint and thus �ii may form the basis of an alternative and possibly better in vitro assay for dioxin congeners and isomers. A possible correlation between the keratinization activity and the PCB content of these soot extracts was observed. Preliminary assays on a PCB mixture (Aroclor 125H), which utilized the flat cell morphology as an endpoint, have indicated that this correlation was probably not due to a direct effect of the PCBs on this assay. The effect of a proposed decontamination agent, Triton X-100, was also tested using this endpoint. A concentration of 0.1 vil/ml was toxic while lower levels had no activity in this assay, nor did they affect the sensitivity of the assay to 2,3,7,8 TCDD. The keratinization assay exhibited a decrease,with time, in the magnitude of the response to the point that keratinization was characterized by the appearance of colonies of keratinizing cells on a background of nonkeratinizing cells. These cultures could be evaluated microscopically and there was no loss of sensitivity to 2,3S7»8 TCDD associated with the decline of the response magnitude. Efforts to determine the cause of the decline, and to reverse it, are discussed. �The occurrence of polychlorinated di"benzo-p-dioxins (PCDD) and dibenzofurans (PCDP) in the environment poses a serious potential threat to human health. These compounds are among the most toxic and teratogenic low molecular weight compounds known (Poland et_ al_. , 1976). • Chlorinated dibenzo-p-dioxins are formed from the condensation of two orthochlorophenates under conditions of high alkalinity, pressure and temperature. The combustion, chemical nature and combustion chamber residence time can also lead to the production of PCDDs and PCDFs. This has been verified by the analysis of flue gas emission and fly ash of some municipal incinerators in the Netherlands (Hutzinger et_ al_. , 198l). (Langer et_ al_. , 1973). This process has also been observed in laboratory models The pyrolysis of organohalogens such as chlorinated phenols and PCBs lead to the formation of PCDDs and PCDPs. This observation was evidenced under field conditions recently in New York State. On February 5, 1983., as a result of fire, the Binghamton State Office Building (BSOB) was heavily contaminated with soot; subsequent cleanup efforts were halted when chemical analysis indicated the presence of high levels of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and 2,3,7,8tetrachlorodibenzofuran (TCDF) as well as other possibly toxic congeners (Smith et al., 198l). This contamination was traced to the involvement by fire of an electrical transformer which contained the dielectric fluid Pyranol, a mixture of PCBs composed of Aroclor 125^ and chlorinated benzenes. A number of human exposures to dioxin congeners and isomers have been reported. An acne outbreak in Germany in 195^ was traced to trichlorophenol con- taminated with TCDD and TCDF (.Poland et_ aJU , 1976). Similar outbreaks of chloracne, the most common manifestation of dioxin exposure in humans, were noted in 2,^,5-T production plants in France, Germany and the United States in the 1950"s and 1960's. In 1971 the use of waste oil contaminated with TCDD for dust control in a riding arena lead to the death of a large number of horses and other small animals, as well as some cases of chloracne in children who played in the area (Kimbrough _et_ al_. , 1977). The contamination of rice oil with dibenzofuran analogs lead to many cases of chloracne in Japan (Bradlaw et al., 1979). The explosion of a chemical plant in Seveso, Italy �2 in 1976 lead to exposure of the population to TCDD which was thought to be responsible for the occurrence of chloracne in humans and a number of livestock losses (Hay, 1980; Pocchiari et_ al_. , 1979; Reggiani, 1978). The use of Agent Orange ( a mixture of n-butyl esters of 2,^-D and 2,^,5-T), a defolient, in Vietnam between 1962 and 1969 lead to the contamination of large areas by TCDD (.Poland et_ al_. , 1976). Recent work by Knutson and Poland has demonstrated that the hyperkeratinization response to TCDD exposure which occurs upon exposure to TCDD in vivo could be reproduced in an in vitro model system (Knutson et_ al_. , 1980). The induction of keratinization is thought to be responsible for the in vivo induction of chloracne. They found that although TCDD did not produce an acute toxic response in various cell types in culture (Knutson et_ al_. , 1980a), XB cells, a cloned epithelial line of mouse teratoma cells (Rheinwald et_ al_. , 1975) when co-cultured at high density with irradiated 3T3 mouse fibrablast cells exhibited a keratinization response when exposed to TCDD. Spontaneous keratinization occurs in these cells when they are seeded at low density (.Rheinwald et_ al_. , 1975). High density XB/3T3 cultures not treated with TCDD did not show this response. Other halogenated aromatic hydrocarbon congeners including dibenzo-pdioxins, dibenzofurans, biphenyls and azp(xy)benzenes also induced keratinization in the XB/3T3 system although to a lesser extent than 2,3,7,8 TCDD. Keratinization could also be induced by some non halogenated aromatic hydrocarbons such as benz(a) anthracene and 5,6-benzoflavone (Knutson et_ al_. , 1980). Since 2,3,7,8 TCDD is the most potent, but not the only inducer of this hyperkeratinization response, this effect will be referred to here as "dioxin-like" activity. Unrelated toxins were studied to determine if the keratinization response was due to nonspecific cell damage. The direct acting alkylating agents W-acetoxy-2-acetylaminofluorene and Mi-methyl-N'-nitrosoguanidine; inhibitors of nucleic acid synthesis, actinomycin D, bleomycin and cordycepin; the spindle microtubule inhibitor, colchicine; kepone, a chlorinated hydrocarbon producing a toxic syndrome distinct from that of TCDD; and 2,6-dichlorobenzo-nitrile, and acnegen considered to have a different mechanism �1 * than TCDD all failed to produce keratinization in the XB/3T3 culture system (Knutson et_ aJL , 1980). 3 Furthermore, a correlation has "been demonstrated between the degree of toxicity of various TCDD isomers and congeners and the extent of enzyme induction, receptor landing and hyperkeratinization response (Knutson et al., 1980; Poland et_ al. , 197T; Poland et_ al. , 1976a; Kende et_ al_. , 1971*). The XB/3T3 system is extremely sensitive, giving an induction of keratinization with as little as 3.2 pg of TCDD (Knutson et_al., 1980). In addition, this system is particularly relevant as a model since it deals with an induced differentiation of the intact cell using an endpoint (hyperkeratinization) known to "be relevant to human exposure (i.e., chloracne). This report describes studies which have been carried out to determine the feasibility of using the in vitro XB/3T3 keratinization model as a mass screen of environmental samples for "dioxin-like" activity, i.e., the ability to induce a hyperkeratinization response. Such an assay could be applied to the detection of "dioxin-like" activity in extracts of samples collected at the Binghamton State Office Building. The evaluation and verification of this assay system is being done by the testing of 12 specific soot samples from various floors of the BSOB building and comparing the results with those obtained from high resolution mass spectroscopy of the same samples when they become available. �METHODS Sample Preparation A soxhlet extract of the soot sample in "benzene (Smith et_ al. , 1981) at a volume of 0.5 - 2.0 ml was mixed with 100 yl of dimethylsulfoxide (DMSO) and evaporated at room temperature for 2k- hours in darkness to allow for solvent exchange from benzene to DMSO with a final volume of 100 yl. A solvent exchange was also done with the positive controls (2,3,7,8 TCDD in DMSO) and solvent controls (DM50). The extract, now in DMSO, was diluted 1:1000 in tissue culture medium (Dulbecco's modified Eagles medium supplemented with 20$ fetal calf serum) and four more 10-fold dilutions were made in this medium for application to the cell cultures. This di- lution series was freshly made for each of the twice weekly refeedings. Cells The XB-2 cell line and the 3T3 feeder cells were obtained from H. Green (M.I.T. ) (.Rheinwald et. al_. , 1975). The cultures were grown in Dulbecco's modified Eagles medium with 100 TJ/ml penicillin and 100 yg/ml streptomycin. The XB line was cultured in medium conditioned "by a 2U hour exposure to confluent 3T3 cells (25 ml/ 75 cm2). The medium was supplemented with 20$ fetal calf serum for the XB cells and 10$ for the 3T3 cells. No contamination with mycoplasma was detected by the Hoechst fluorescence staining method (Chen, 197^). Keratinization screen assay for "dioxin-like" activity Initial screening was done essentially as described by Knutson and Poland (.Knutson. _et_ al_. , 1980) for the in vitro keratinization model. Target cells were the XB epithelial clone derived from mouse teratoma cells by Rheinwald and Green (Rheinwald et. al., 1975). When these cells are plated at low cell density (250 cells per 60 mm dish) along with lethally irradiated 3T3 cells (3 X 105 cells per 60 mm dish), the XB cells form epithelial colonies which stain red with Rhodanile blue. Rhodanile blue stains most mammalian tissue blue but keratinized tissues are stained red (MacConaill et al., 196^). When XB cells are plated at high density (lO5 cells/dish) in the pre- �5 sence of irradiated 3T3 cells (3 X 10 cells per dish), the XB cells replicate but 5 keratinization is not seen and therefore the red staining component of Rhodanile blue (Rhodamine B) is absent. Addition of TCDD to cultures of XB cells at high cell density which are refactory to spontaneous keratinization, produces a dose-related keratinization with the associated red staining with Rhodanile blue. TCDD was shown to pro- duce maximal red staining at concentrations of 5 X 10"11 to 1CT7M; 1 X lO'^M TCDD produces an intermediate response while cultures treated with 5 X 10~12M TCDD and untreated control cultures do not keratinize. This response reaches a maximum by day 10-13. When XB/3T3 cells were plated in l6 mm wells containing 1 ml of medium, as little as 3.2 pg of TCDD produced observable keratinization (Knutson et_ aJL., 1980). Confluent cultures of 3T3 cells were lethally irradiated with IfOOO rads by a cesium source and both the irradiated 3T3 and XB cells were seeded together in Costar Multiwell dishes (15 mm) at 5 X 104 XB cells and 5 X 10U irradiated 3T3 cells per ml per well. These dishes were incubated at 37°C in a humidified of 5% COa in air. atmosphere The medium was replaced twice weekly. The dilution series of the sample was added to the assay cultures 2U hr post seeding and with each medium change. Appropriate solvent controls were run as well as 2,3,7,8 TCDD reference samples. After 12 days, the cultures were rinsed with phosplate buffered saline (PBS) fixed for 30 min. in 10% formalin-PBS and stained with 1% Rhodanile blue or 1% Rhodamine B (.Knutson et_ al_, , 1980). The cultures were then observed for the occurrence of red staining material indicative of the keratinization response. The highest dilution of sample capable of inducing keratinization greater than background levels was taken as the endpoint. The endpoint of the 2,3,7,8 TCDD standard was compared to the endpoints derived from the extracts in order to determine the TCDD equivalency of the sample. The range of activity of a sample was calculated from, the endpoint as follows: It has been shown (Knutson et_ al_., 1980) that 10-11M TCDD produces only a moderate keratinization response, (compared to that produced by 10~10M and higher). �6 >•; Furthermore, one half this amount, i.e. 5 X 10~~12M TCDD produces no response at all. Therefore, in all cases production of such a moderate endpoint was taken to indicate the presence of "between 5 X 10~12 and 1 X 10-nM TCDD equivalent. The assumption was made that one fifth the amount of sample which gave the moderate response would give a negative response. Thus the amount of sample which contains "between 5 X 10~12 and 1 X 10~1:1M dioxin-like activity was taken to "be "between 2Q% and 100$ of the actual amount of sample which gave the moderate response. Safety Considerations It is recognized that the safe handling, containment, and disposal of the substances to "be used in this study are essential. Some of the precautions include prohibition of mouth pipetting, subtraction weighting, use of glove box storage cabinets vented with HEPA and charcoal filters, restriction of traffic in hazard-area, no food, smoking or drinking in hazard area, accurate record keeping of hazardous materials from r-eceipt to disposal, use of filter vented biohazard hoods (BioGard Type II B) f°r medium changes and use of commercial hazardous waste disposal facilities. �RESULTS Assay of BSOB Extracts Preliminary studies were performed to attempt to duplicate the in vitro keratinization model in tMs laboratory. XB/3T3 cultures vere exposed to 10~9M TCDD in DMSO or to DMSO alone at 0.01% final concentration to correspond to the level in the TCDD solution. After 12 days of incubation, with refeeding every 3 to h days, these cultures were fixed and stained. Cultures exposed to 10~9M TCDD showed a marked increase in keratin deposition, as shown by intense Ehodamine B staining, as compared to the DMSO negative control [Fig. l). A 10-fold dilution series of authentic 2,3,7,8 TCDD from 10~8 to 10~12M was tested. The minimal concentration capable of inducing a keratinization response greater than background levels was found to be IQ-^M (Fig. 2b). This is equivalent to 3.2pg/ml and is in general agreement with published results for this compound (Knutson et_ al_. , 1980). A BSOB soot extract which had been analyzed by mass spectroscopy for TCDD and TCDF CSmith et_ al., 198la) was also tested in this experiment for its ability to induce a hyperkeratinization response. A dilution series of this extract was applied to the XB/3T3 cell cultures as described in methods. Figure 2a shows that the DMSO solvent control dilution series induced no keratinization. The highest concentration of the DMSO soot extract (l ul/ml, equivalent to 820 ug soot/ml) caused cytotoxicity. The lowest concentration of extract which induced keratinization was 10~3 ul/ml, which is equivalent to 0.82 yg of soot CFig. 2c). From this result the concentration of .dioxin-like activity in the extract vas calculated (as described in Methods)" to be in the range of 2-20 ppm. Analysis of this sample by mass spectrometry (Smith et_al. , 198lb) indicated the presence of 1.2 ppm 2,3,7,8 TCDD and U8 ppm 2,3,7,8 TCDF. 'The latter is 20-fold less potent then 2,3,7,8 TCDD (.Knutson et_ aiU , 1980); therefore, W ppm of this compound is equivalent in keratinization activity to 2.1* ppm of 2,3,7,8 TCDD. Thus, the total keratinization activity,.based on the mass spectrometry data for these two compounds, should be that of 3.6 ppm 2,3,7,8 TCDD. This is within the concentration limits actually ob- tained in the keratinization assay. �• ; 8 In order to further test the ability of the assay to predict the results of mass spectrometric analysis, benzene extracts of 12 soot samples from different floors of the BSOB vere tested for their ability to induce keratinization. Cells were seeded and exposed to dilutions of the extracts in culture medium. The cultures vere refed every 3-^ days with fresh dilutions of the extract. After 21 days, the cultures were fixed and stained with Rhodamine B. It became obvious, however, that a decrease in the magnitude of the hyperkeratinization effect in response to TCBB exposure had occurred, apparently with time, such that induced keratinization could be seen clearly only under microscopic observation. Colonies of keratinizing cells, similar to those described by Rheinwald and Green (1975) could be seen on a background of non-keratinizing cells. (Attempts to determine the reason for this decrease and to regain the earlier level of responsiveness seen in Figure 1 will be described later.) This decrease in magnitude of the keratinization response did not however, decrease the sensitivity of the assay as seen in studies with authentic TCDD. Accordingly, blind microscopic evaluation was carried out on each of three replicates for each sample by two observers for the occurrence of keratinizing colonies. The results, shown in Table 1, are an average of 6 values per sample and showed good reproducibility with variation rarely being greater than one dilution for any of the replicates of any single sample. The solvent controls and blanks showed no false positive response. Calculations for dioxin-like activity were made as described in Methods. The results show a variation of about 3 orders of magnitude in the ^dioxin-like" activity of the various samples. There appears to be something of a trend in that the samples from the lower floors seem in general to have less activity than those from the higher floors. The results of this study will be compared to the mass spectrometric analysis of these samples when this becomes available. The average keratinization results in terms of dioxin-like activity in ppm were plotted against the available PCB analysis data for these samples generated by gas chromatography (Pause, 1981). Figure 3 shows a double log plot of these two sets of data. There appears to be a possible correlation between the PCB content �9 and the keratinization inducing activity of these soot extracts. Possible reasons for this correlation are examined in the discussion section. AttemptG Made to Reverse the Decrease in the Magnitude of the Hyperkeratinization Effect A personal communication from Dr. A. Poland confirmed that a decline in magnitude was also experienced in his laboratory and was alleviated by the use of reconstituted frozen stocks of early passage XB cells. However, such a strategy in this laboratory failed to increase the magnitude of the keratinization endpoint. It has also been shown that the ratio of XB cells to the irradiated 3T3 feeder cells can affect the magnitude of the response (Rheinwald et_ al_. , 1975). Experiments done to optimize this ratio also failed to restore the response to the early levels, as did changing the irradiation time of the feeder cells, changing the refeeding schedule, using culture vessels of different manufacture and lot numbers, changing incubators, altering the pH of the cultures, using stain from various sources or using medium conditioned by unirradiated 3T3 cells rather than co-cultivation of XB cells with irradiated 3T3 cells. Current attempts to increase the magnitude of the keratinization response will be addressed in the discussion section. Morphological Alteration - A Possible Alternative Endpoint The appearance of an altered cell morphology was observed with those cells which had been exposed to TCDD as well as the various soot extracts in the experiment described in table 1. This change was first seen after 7 days of exposure to the samples and was characterized by a flat cell morphology as compared to the more fibroblastoid cells in the unexposed cultures or those exposed to less than 10""11!/! TCDD CFigure U). An apparent cessation in cell growth was also seen in these flat cells, while the unexposed cells continued to proliferate, resulting in more dense cultures. The minimal concentration of each sample capable of inducing the flat cell response was recorded on the 13th day of exposure of the cultures to the extracts. Replicate dilution series were evaluated by phase microscopy of the living cells by two observers generating 10 values for each sample. The agreement between replicates was excellent with variation rarely being greater than one dilution �••; lo for any one sample. One half of the replicates were fixed and stained for a record, while the remaining cultures were later evaluated for the previously described keratinization (table l). The high correlation between the induction of the keratinization response and that of the flat cell morphology'(Figure 5) indicates that it may by possible to use this flat cell morphological change as an alternative and perhaps improved endpoint in the assay for dioxin-like activity. Preliminary experiments suggest that the induction of the flat cell appearence by TCDD is not dependent upon the irradiated 3T3 feeder layer, thus simplifying any proposed assay procedure using this endpoint. The induced flat cell morphology has been found to be apparent after only 6-7 days of exposure to authentic 2,3,7,8 TCDD, thereby allowing the assay to be run without the necessary refeeding needed in the keratinization assay. Effects of Triton X 100 on the Assay Triton 30.00 (TX) has been proposed for use in the decontamination of the BSOB. Since TX is soluble in benzene which is currently used in the soxhlet ex- traction of the samples and could therefore be encountered in samples to be assayed, a preliminary experiment was carried out to deterimine whether TX has any effect on the assay. A concentration range of TX from 10~* - 10~^yl/ml was tested with the standard concentration series of the TCDD standard (10~8 - 10~12M). It was found that TX at 10"1 yl/ml is cytotoxic while levels of 10~2 and 10~3 yl/ml are not. No synergistic or antagonistic effect of TX in regard to the TCDD induced flat cell endpoint was observed. There was also no induction of a false positive result by TX alone at any concentration tested. Experiments to determine the effect of TX on the keratinization endpoint are in progress. �11 DISCUSSION: The fire at the Binghamton State Office Building and involvement of an electrical transformer containing a mixture of PCBs (Araclor 125^-) and chlorinated "benzenes lead to subsequent contamination of the structure with dioxin and dibenzofuran laden soot. A need was established for a rapid semiquantitative assay for "dioxin-like" activity. This would allow prioritization of samples for high resolution quantitative and qualitative analysis in order to monitor the progress, of decontamination. This preliminary report has dealt with the evaluation and verification of such an assay which is based on an in vitro model of the in vivo keratinization response to dioxin exposure. Preliminary studies demonstrated that the published in vitro model was reproducible in this laboratory and that this model was sensitive to levels of dioxin (2,3,758-TCDD) which corresponds to that in the literature (Rnutson et al, 1980) (approximately 10 M). Assay results of a single soot extract for which mass spectrometry data were available indicated a good correlation between these data and the data resulting from the keratinization mo'del. This initial verification lead to the application of this assay to 12 soot extracts for comparison with results of mass spectrometry of the same samples as they become available. However, the decrease in the magnitude of the TCDD induced keratinization effect may reduce the usefulness of this particular endpoint in spite of the readily apparent, microscopically observable, induction of keratinizing colonies. Attempts are currently being made to redone the XB cell line for the desired characteristics of hyperkeratinization upon TCDD exposure/ Successful monitoring of the cell line, cell storage and recloning would insure a stable cell population upon which the keratinization assay could be based. Cloning is being done by identification and isolation of spontaneously keratinizing colonies of XB cells in sparse culture, as well as keratinizing colonies of XB cells induced by TCDD �12 exposure in dense cultures. New XB and 3T3 feeder cell starter cultures will be obtained, since the reconstitution and use of our early passage frozen stocks has failed to increase the magnitude of the keratinization response to that seen in the initial assays. The subjective reading of the endpoint by visual estimation of the minimal concentration of extract capable of keratin induction based on the intensity of Rhodamine B staining or identification of keratinizing cell colonies limits the degree of quantitation possible. Therefore, several other methods of achieving better quantitation of the induced keratin production are being considered and evaluated. One involves extraction of the Rhodamine B stain from the cells and quantitation by fluorometric measurement. Another involves a quantitative radio- immunoassay method for mammalian epidermal keratin protein which has recently been published (Yuspa et_ al, I960). Another possible method for detection of increased keratin production to be explored is based upon the observation (Steinert et al_, 19T8) that in keratinizing cells, keratin represents 20% of the total urea extractable cellular protein. synthesized. Thus, keratin may represent the predominent protein being Furthermore, keratin has been shown to be relatively rich in histidine, methionine and cysteine (Belanger, 1956; Clark, 1968; Hambrick, 1966). Thus, it may be possible to quantitate keratin production by measurement of incorporation of these (radiolabeled) amino acids into cellular protein. The verification of the flat cell morphological change as an indicator of "dioxin-like" activity would allow a second and perhaps improved biological endpoint to be used in a routine screen assay in addition to or in place of the keratinization assay. The Endpoint is apparent after only 6-7 days and can be readily assessed by microscopic observation of living cultures'. Another advantage of the short development time of this endpoint is the lack of the necessity to refeed the cultures, thus reducing both the sample requirement and handling of the cultures. The homo- geneity of these cells may allow use of smaller culture vessels, reducing even further �13 the amount of sample needed. In addition recent experiments have suggested i that the irradiated 3T3 cell feeder layer may not "be needed for the development of this endpoint. Further studies vill be carried out to establish whether the induction of the flat cell morphology is a valid endpoint for the detection of dioxin-like activity. These will include a double blind study to test the ability of the endpoint to quantitate various concentrations of authentic 2,3,798-TCDD and a test of the relative activities of other halogenated polycyclic compounds, e.g. TCDF, biphenylene, PCB, azo(xy)benzenes, as well as nonhalogenated aromatic hydrocarbons. Compounds that inhibit cell proliferation by acting on macromolecular synthesis vill also be tested to determine if the flat cell response in these cells is simply due to the coincidental inhibition of cell growth. Attempts to establish cloned cell lines exhibiting the flat cell characteristic to insure homogeneity are currently underway. The possible correlation which we have observed between the in vitro assay results and the PCB content of the soot samples (Figure 3) lead to concern that the PCBs were responsible for the induction of keratinization. In fact, it has been reported that 2,3,^,2' ,3' ,^' polybrominated biphenyl can induce keratinization in the XB/3T3 system at a concentration 2,000 fold higher than 2,3,7,8TCDD (Knutson et al, I960). To examine this possibility, Araclor 125U, the PCB mixture present in the transformer coolant and thus the presumed source of PCBs in the soot samples, was tested for .the induction of the flat cell morphology. The lowest concentration of Araclor 125^ for which the flat cell induction was observed vas 10 yg/ml. The highest concentration of PCBs found in any of the soot samples tested was 23,000 yg/gm (Pause, 1981}> The lowest amount of this sample which gave an endpoint was 1.5 yg of soot per ml which contains 0.035 Pg of PCBs per ml. Based upon the results with Araclor 125U, this is insufficient to induce the flat cell response. Thus, the observed induction of the flat cell morphology by the soot extracts is unlikely to have been caused by the PCBs contained in the �lit samples. Experiments are in progress to determine if similar results are obtained for PCB induced keratinization. Another explanation for the correspondence "between the PCB data and the in vitro assay results may be a synergistic or additive interaction between PCBs and low levels of TCDD or some other substance in the soot samples. Studies designed to detect such interaction between Araclor 125^ and 2,3,7,8-TCDD are being carried out and studies using PCBs to spike actual soot extracts are planned. The correspondence could also be the result of a similar deposition pattern of the PCBs and the dioxin congeners and isomers in the building. Triton X-100, the proposed decontamination agent for the BSOB, was found to be toxic to the in vitro system at 0.10 yl/ml but not at 0.01 yl/ml. TX is soluble in benzene, and a relatively low, non toxic, concentration in a sample could be concentrated by a benzene extraction procedure to toxic levels and preclude use of the in vitro assay. This possibility should be considered in the development of decontamination and sample collection procedures. The lack, of effect of TX on the induction of the flat cell response does however, decrease the concern of a false positive result from low levels of this compound. In summary, the in vitro keratinization model developed by Knutson and Poland (Knutson et al, 1980) has been examined for use as a screen assay for the detection of "dioxin-like" activity in extracts of BSOB soot samples. After initial verification with authentic TCDD, a preliminary assay was done on the one sample for which TCDD and TCDF data from mass spectrometry'were available. The results of this in vitro assay compared well with the quantitative analysis data. Based on this result, a screen for keratinization induction was carried out on 12 extracts of soot from various floors in the BSOB. These results will be compared to the mass spectrometry data on the same samples, thus allowing a more rigorous validation. A high correlation would indicate that this model may be �-.; 15 used as a semiquantitative mass screen assay for "dioxin-like" activity. The decrease in the magnitude of the keratinization response which we have observed with time gives reason for concern, as the cause for this decline has not been determined. The problem may be solved by the acquisition of new starter cultures, or stabilized for a time by recloning the line for the desired characteristics and/or using reconstituted frozen stocks of those cultures which currently exhibit TCDD induced keratinizing colonies. Alternatively, the TCDD- • induced change in morphology (which is characterized by the appearance of flat, non proliferating cells) which seems to correlate very well with the keratinization endpoint may have the potential for use as an additional or alternative (and possibly better) endpoint for use in mass screening for "dioxin-like" activity. �16 REFERENCES Belanger, L.F. (1956) Autoradiographic Visualization of the Entry and Transit of 6^5 Methionine and Cystine in the Soft and Hard Tissues of the Growing Rat. Anat. Rec_., 12^:555-563 Bradlaw, J.A., and Casterline, J.L. (1979) Induction of Enzyme Activity in Cell Culture: A Rapid Screen for Detection of Planar Polychlorinated Organic Compounds. J_. Asspc. Off. Anal. Chem., 62:90^-915 Chen, T.R. (197*0 Utilization of Fluorescent Hoechst Stain to Effectively Detect Mycoplasma Contamination. In Vitro 10:390 Clark, S.L. (1968) Incorporation of Sulfate by the Mouse Thymus: Its Relation to Secretion "by Medullary Epithelial Cells and to Thymic Lymphopoiesis. J_. Exp. Med. , 128, 927-957Fukuyama, K. and Epstein, W.L. (1966) Epidermal Keratinization: Localization of Isotopically Labeled Amino Acids. J_. Inves. Derm., kj, 551-559. Hambrick, G.W., Lamberg, S.I. and Bloomberg, R. (1966) Observations on Keratinization of Human Skin In Vitro. £. Inves.Derm., Vr, 5^1-550. Hay, A. (i960) Health monitoring endangered at Sev&so. Nature, 283, 237. Hutzinger, 0., Olie, K., Lustenhouver, J.W.A., Okey, A.B., Bandiera, S., and Safe, S. (1981) Polychlorinated Dibenzo-P-Diozins and Dibenzofurans: A Bioanalytical Approach. Chemosphere 10, 19-25. Kende, A.S., Wade, J.J., Ridge, D. and Poland, A. (197*0 Synthesis and Fourier Transform Carbon-13 Nuclear Magnetic Resonance Spectroscopy of New Polyhalodibenzo-p-dioxins. J_. Org. Chem., 39, 931-937. Kimbrough, R.D., Coleman, D.C., Liddle, J.A., Cline, R.E. (1977) Epidemiology and Pathology of a Tetrachlorodibenzodioxin Poisoning Episode. Arch. Environ. Health, March-April, 77-85. Knutson, J.C., and Poland, A. (1980) Keratinization of Mouse Teratoma Cell Line XB Produced by 2,3,7,8-Tetrachlorodibenzo-p-dioxin: an in vitro model of toxicity. Cell, 22, 27-36. Knutson, J.C. and Poland, A. ( 9 0 2,3,7,8-Tetrachlorodibenzo-p-dioxin: 18) Failure to Demonstrate Toxicity in Twenty-three Cultured Cell Types. Toxicol. and Applied Pharmacol., 5^, 377-383. Langer, H.G., Brady, T.P. and Briggs, P.R. (1973) Formation of Dibenzodioxins and other Condensation Products from Chlorinated Phenols and Derivatives. Environ. Health Perspect., 5, 3-7. Lowery, O.K., Rosebrough, N.J., Farr, A.L. and Randall, R.J. (1951) Protein Measurement with the Folin Phenol Reagent. J_. Biol_. Chem., 193, 265-275. �17 MacConaill, M.A. , and Gurr, E. (19610 The Histological Properties of Rhodanile Blue. Ir_. J_. Med. Sci . , June, 2^3-250. Pause, R. ( 1981 ) Personal Communication, N.Y. State Department of Health. Pocchiari, F., Silano, V. and Zampieri , A. (1979) Human Health Effects from Accidental Release of TCDD at Seveso, Italy. Ann. N.Y. Ac ad. Sci. 320, 311-320. Poland, A. and Kende, A. (1976) 2,3,7»8-Tetrachlorodibenzo-p-dioxin: environmental contaminant and molecular probe. Fed. Proc., 35 , Poland, A., Glover, E., Kende, A.S., DeCamp, M. , and Giandomenico, C.M. (I976a) 3,^,3' jV-tetrachloroazoxybenzene and azobenzene: Potent Inducers of Aryl Hydrocarbon Hydroxylase. Science , 19^, 627-630. Poland, A. and Glover, E, (1977) Chlorinated Biphenyl Induction of Aryl Hydrocarbon Hydroxylase Activity: A Study of the Structure -Activity Relationship. (1977) Mol. Pharmacol., 13, 921+-938. Reggiani, G. (1978) Medical Problems Raised by the TCDD Contamination in Seveso, Italy. Arch. Toxicol. , UO, l6l-l88. Rheinwald, J.G. and Green, H. (1975) Formation of a Keratinizing Epithelium in Culture by a Cloned Cell Line Derived from a Teratoma. Cell* 6, 317-330. Smith, R.M., O'Keefe, P.¥., Hilker, D.L., Jelus-Tyror, B.L., and Aldous, K. ( 9 l Chemical analysis of 2,3,7,8-tetrachlorodibenzo-p-dioxin and 2,3,7,8I8) tetrachlorodibenzofuran in a soot sample from the transformer explosion in Binghamton, New York. N.Y. State Department of Health Report. February 20, 198l. Smith, R.M., Hilker, D.L., O'Keefe, P.W., Kumar, S., O'Brien, J., Jelus-Tyror, B.L., and Aldous, K. (I98la) Analysis of a Binghamton soot sample for tetrachlorodibenzofurans and tetrachlorodibenzo-p-dioxins . N.Y. State Department of Health Report, October 1, 1981. Steinert, P. and Yuspa, S.H. (1978) Biochemical Evidence for Keratinization by Mouse Epidermal Cells in Culture. Science , 200, Yuspa, S.H., Poirier, M.C., Harness, J.R., Olsom, D.R. and Steinert, P.M. (1980) Specific Quantification of Mouse and Human Keratin Proteins by Radioimmunoassay. Bio_chem. J_. , 187 » 281-28U. �18 Table I Keratinization Assay of BSOB Soot Samples Floor number Lowest active c o n c e n r a o n owes a c v e concentration of extract (pg soot equivalent/ma)a 3 k 6 1.3 llt.O 15.9 7 8 0.3 1.0 9 10 12 Ik 15 17 1.5 0.5 0.7 12.9 O.It. O.k TCDD , v equivalent ,(ppm) 0.01 1.2 0.11 0.10 - 0.10 - 12 - 1.1 - 1.0 5.3 - 53 1.6 - 16 l.l 3.2 2.3 0.12 k.O k.O - 11 - 32 - 23 - 1.2 - kO - kO a) Activity was determined by the appearance of keratinizing colonies. This result is the average of values from 3 replicates evaluated by two observers. b) .Calculated as described in Methods. �Figure Legends Figure 1 Effect of 2,3,7,8 TCDD on XB/3T3 Cell Cultures Cultures were seeded and cultivated as described in methods. Figure la is representative of an XB/3T3 culture exposed to 10r* M 2,3,7,8 TCDD in the presence of 0.01$ DMSO. Figure Ib is representative of a replicate culture exposed to 0.01$ DMSO alone. The bright red rhodamine B stain, indicative of keratin deposition} shows as dark grey in these photos. Figure^ 2 Keratinization assay of a BSOB soot extract Figure 2a shows the negative response of the DMSO control. Figure 2b shows the effect of 2,3,Tj8 TCDD on this system with keratinization first evident with 10"1:LM. Figure 2c shows the toxic effect of a BSOB soot extract at the highest concentration (l yl/ml) and the induction of keratinization at lower concentrations, with the effect first detected at the fourth highest dilution (10~3 ul/ml), equivalent to 0.82 yg soot/ml. Figure 3 Log-log plot of the amount of PCBs detected in BSOB soot extracts from various floors by gas chromatography (abscissa) and the calculated values of "dioxin-like" activity generated by the keratinization assay of the same samples (ordinate). The values for "dioxin-like" activity were derived by dividing the amount of soot per ml in the lowest soot extract concentration capable of inducing keratinization into 3.2 pg/ml which is the lowest concentration of 2,3,7>8 TCDD found to induce keratinization. Figure k TCDD induced flat cell morphology Figure Ua: XB/3T3 culture after 12 days of incubation with 0.1$ DMSO, showing high density and fibroblast-like organization. Figure li-b: a similar culture exposed to 10~°M TCDD in 0.1$ DMSO, showing flat morphology and relative low density. Phase, l^OOX magnif ifcation. Figure 5 Log-log plot of calculated values of "dioxin-like" activity of BSOB soot extracts from various floors generated by the keratinization assay (ordinate) and by the induction of the flat cell response (abscissa) calculated as in Figure 3. �20 Figure la Figure Ib �21 X .* • •! - o •-- - o' = • Figure 2a Figure 2b �22 Figure 2c �23 4-J •H n •u o «j rt O cd -H OT ?*! a8 p< to ,3 I 1 2 i 3 log ppm PCB in soot samples Figure 3 t 4 JE �Figure 4a Figure 4b �.3 4J 0 I 4J 3 ctf »H W I <U 0 log ppm "dloxin-like" flat cell induction in soot samples Figure 5 � 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. 088 Folder The folder containing the original item. 2212 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 Gierthy, John F. Gerald D. Frenkel Title A name given to the resource Typescript: A Preliminary Report on the Evaluation of an In Vitro Assay for the Detection of "Dioxin-Like" Activity Using Extracts of Soot from the Binghamton State Office Building, 1982 Subject The topic of the resource BSOB PCBs analytical studies https://www.nal.usda.gov/exhibits/speccoll/files/original/0c41c6d2091cb7accae8f4f1a073ab25.pdf c081adff961a2bb80598e7c051cfa2b0 PDF Text Text Item D Number 02207 Author Hilker D R - Toxicology Institute, Center for Laboratories and Resear RopOrt/ArtiGlO TltlB Determination of Chlorinated Combustion Products in Samples from a Contaminated Office Building Journal/Book Tttle Year 1982 Month/Day October Color O Number of Images 13 Descriflton Notes Thursday, September 20, 2001 Page 2207 of 2293 �PROGRESS REPORT: Determination of Chlorinated Combustion Products in Samples from a Contaminated Office Building D.R. Hilker, R.M. Smith, P.W. O'Keefe, and K.M. Aldous Toxicology Institute Center for Laboratories and Research New York State Department of Health Albany, NY 12201 RECEIVED ° ctober ' 1982 OCT131982 DIRECTOR PUBLIC HEALTH �Abstract This report describes additional work that has been completed relevant to the analysis of materials from the Binghamton State Office Building since the March, 1982 document titled "Determination of Polychlorinated Dibenzofurans in Soot Samples from a Contaminated Office Building." Spiked recovery experiments as well as repeat analyses for polychlorinated dibenzofurans (PCDFs) and isomer specific analysis for 2,3,7,8 Tetrachlorodibenzo-p-dioxin (TCDD) in some of the original soot samples have been completed. Improvements in data processing techniques and statistical evaluation of the early high resolution scanning data are discussed. Results are presented from an experiment to measure volatilization rates of TCDD into air and the effectiveness of trapping the vapor on activated silica gel sampling cartridges. -2- �Introduction The analysis of a series of soot samples taken from various floors of the Binghamton State Office Building has already been described. A number of plausible but experimentally verifiable assumptions were made during the interpretation of this data. These include the hypothesis that Tetra CDF recoveries are generally comparable to those of more highly chlorinated PCDFs, that benzene is an effective extraction solvent, that the precision of these analyses was sufficient to permit sample to sample comparison, and that the signals used in quantitation were entirely due to PCDFs. Results of experiments designed to test these assumptions are presented here. In addition, efforts to further characterize the concentrations of additional compounds present in the soot extract are described. Finally, the results of preliminary experiments designed to devleop a well-validated methodology for determination of PCDDs and PCDFs in air at the pg/M level are presented. -3- �1) Recovery of Spiked Soot Samples. Four 10 milligram samples of carbon (active coconut charcoal) were spiked with labelled and unlabelled standards and subjected to the extraction and clean-up procedures already described. Results are presented in Table 1 for the recovery of Tetra CDF and Hexa CDF. Sample S-2 was spiked with only unlabelled standard (2 ng of Tetra CDF and 13.4 ng of Hexa CDF). Carbon samples S-3, S-4 and S-5 were, in addition, fortified with 95.2 ng of Cl-TCDF. Generally, recoveries were good showing that extraction and clean-up were effective and confirming the earlier assumption that 37Cl-Tetra CDF recoveries gave reasonable estimates for Hexa CDF recoveries when Tetra-CDF recoveries were good. The poor recovery (3%) for Tetra CDF in S-5 was also seen in the 12th Floor sample and results from the critical nature of one of the steps of the clean-up procedure. ' 2) Comparison of the Efficiencies of Benzene and Toluene Extractions Published data indicates that toluene soxhlet procedures 2 produce superior recoveries from certain matrices. Since benzene has been used in these studies, a comparison of the extraction efficiencies of these two solvents was appropriate. Table 2 presents recovery data and quantitation of PCDFs in the soot homogenate following the two different extraction procedures. The only difference in the procedures was the substitution of toluene for benzene in the first extraction step. Results show a near equivalent extraction efficiency for PCDFs and, additionally, provide a measure of the reproducibility of the overall analysis procedure. -4- �3) Standard Response Factors. Several additional standards have been analyzed by GC/MS to obtain response factor so that further quantitations can be made on soot sample extracts. Solutions of a tetrachlorobiphenylene (Tetra GBP) and octachlorobiphenylene (Octa CBP) have been analyzed and response factors for each have been computed. Tetra CBP gave a response factor of 619 counts/ng and Octa CBP 263 counts/ng using nominal concentrations for the available standard solutions. The concentrations of these standards have yet to be accurately established. An EPA standard Halowax 1051 was also analyzed and found to contain only Hepta and Octa Chloronaphthalene. The standard contained 92% Octachloronaphthalene which gave a response factor of 592 counts/ng of standard injected on-column. These response factors can be used in the quantitation of soot extracts once recoveries for these compounds have been established. 4) Chloronaphthalene Quantitation. Quantitation of Chloronaphthalenes in the soot homogenate sample has been made based on the response obtained for a Halowax 1051 standard. Assumptions made in this quantitation that are the recovery of these compounds is comparable to that of the PCDFs and that response factors of the congeners are related to the response factors of the PCDF congeners. Based on the Halowax 1051 standard response for Octachloronaphthalene and the recovery of Cl-TCDF, the concentration of Chloronaphthalenes in the soot homogenate is as follows: -5- �Polychloronaphthalenes (ppm) in soot (corrected for recovery) Tetra-CN 37 Penta-CN 143 Hexa-CN 176 Hepta-CN 105 Octa-CN 5) 11 Repeat Analyses To investigate the reproducibility of the methodology three of the original soot samples were reanalyzed. these analyzes are shown in Table 3. The results of A reproducibility figure was generated by averaging the per cent variation from the mean of each set of two values. The results for TCDF in the soot was calculated using an internal standard and exhibit better reproducibility ( 15%). The same Cl.-TCDF standard solution was used for both the original and the reanalysis. The concentration of HXCDF and OCDF were calculated by an external standard method using different standard solutions and they are less reproducible. The reproducility of the method should increase as the availability and amount of the labelled and native PCDFs and PCDDs improves. 6) Mass Assignment in High Resolution Scanning Experiments. High resolution mass spectrometry permits the assignment of elemental compositions to each resolved measured exact mass in each high resolution mass spectrum. The certainty of structural assignments and quantitation of concentration levels are improved by this technique. -6- �In this phase of the Binghamton work we have analyzed more carefully our high resolution data for accuracy of mass assignment. Table 4 compares the accuracy of mass assignment in a standard injection and three samples of soot taken from the BSOB. The average error and standard deviation of the standard injection run on the same day as the samples and the sample injections are similar and within one standard deviation of the mean. This suggests that the signals used to quantitate these compounds are entirely due to these compounds and not to interferences. 7) Air Sampling for 2,3,7,8 TCDD In order to extend our 2,3,7,8-TCDD analytical method to air analysis in the Binghamton State Office Building, experiments using C radiolabeled 2,3,7,8-TCDD have been performed to investigate TCDD volatilization, trapping efficiency, and breakthrough. Results obtained under laboratory conditions show that 60-70% of a 2 ng. TCDD standard is volatilized from the surface of a quartz-glass tube held at 150°C for 10 min while being swept by air (23°C inlet temp, 37°C outlet temp) at 20 L/min. The volatilized TCDD can then be trapped by an activated silica gel cartridge with a trapping efficiency found to be 80-96% (80% = 72 hr breakthrough study). Experiments are underway to test the use of a glass fiber prefilter to trap air-borne particulate matter separately. 8) Analysis for 2,3,7,8-TCDD. Three soot samples were analyzed for 2,3,7,8-TCDD after 4 isomer specific clean-up described elsewhere. The mass -7- �spectrometer was used in the High Resolution Multiple Peak Monitoring (HRMPM) mode to enable the most sensitive detection of 2,3,7,8 TCDD to be made. Signal measurements were taken in the mass region about each of the selected ions in the parent cluster for 2,3,7,8 TCDD and labelled C-TCDD so that exact mass chromatograms of native TCDD and internal standard TCDD could be obtained after the samples were run by this GC/MS technique. quantitations from this analysis are given in Table 5. The The concentrations of 2,3,7,8 TCDD found in the soot confirm the finding of other laboratories that the 2,3,7,8 TCDD/2,3,7,8 TCDP ratio is the order of .01 and supports the assumptions used in discussions of chemical and biological data. —8— �CONCLUSIONS Data presented for spiked sample recoveries indicate that comparable recoveries are obtained for Tetra CDF and Hexa CDF and thus earlier quantitations based on this assumption have been shown to be valid. The extraction efficiency of benzene has been shown to be comparable to toluene for the analytes of interest. Repeat analyses of several soot samples have indicated that good precision is obtained and that sample to sample comparisons are valid. Evaluation of accurate mass assignments of both sample and standard runs by the high resolution mass spectrometer system form a basis for proving that interferents were not present or were resolved from the signals produced for PCDFs and that valid quantitation was obtained from these data. Additional quantitation of 2,3,7,8 TCDD and preliminary data for PCNs add to the characterization of the soot samples. TCDD levels found were consistent with earlier data and predicted levels. The preliminary experiments on volatilization and trapping of TCDD in air show analytical promise and will be further evaluated and validated for PCDF and PCDD determinations in air o at the pg/M levels. �REFERENCES Determination of Polychlorinated Dibenzofurans in Soot Samples from a Contaminated Office Building. R.M. Smith, D.R. Hilker, P.W. O'Keefe, S. Kumar and K.M. Aldous. New York State Department of Health, CLR Report, March 1982. Reversed-phase liquid-solid chromatography on Modified Carbon Black. M. Colin, C. Eon and G. Guiochon. Journal of Chromatography 122 (1976) 223-242. Comparison of Chemical and Biological Data on Soot Salmples from the Binghamton State Office Building. G. Eadon, K.M. Aldous, G. Prenkel, J. Gierthy, D. Hilker, L. Kaminsky, P. O'Keefe, J. Silkworth and R.M. Smith. New York State Health Department, CLR Report, March 1982. Modification of a HPLC-GC Procedure for Separation of the 22 Tetrachlorodibenzo-p-dioxin isomers. P. O'Keefe, R. Smith, C. Meyer, D. Hilker, K. Aldous and B. Jelus-Tyror. of Chromatography 242 (1982) 305-312. Journal �TABLE 3 Re-analysis of Soot Samples Sample # Series Concentration (ppm) TCDF Recover; HxCDF OCDF 290 35 49 310 197 74 21 1 70 32 3.0 50 36 19 4.0 51 1 100 70 4 17 2 Soot Homogenate 320 2 713 8th Floor 1 2 715 9th Floor 92 44 16 48 Series 1 analyzed 3/82, Series 2 10/82, 2 37 Based on Cl-TCDF internal standard. Values corrected for recovery. �TABLE 4 Comparison of Mass Accuracy Errors 8th Floor Injection Description Theoretical Masses Standard 9th Floor Soot 713 715 Homogenate Errors (ppm) (Standard Deviation of Error, ppm) of Interest 371.8237 ) -6 (11) -7 (13) -4 (14) -2 (10 373.8207 )HxCDF -3 ( 7 ) -4 (13) -7 (12) -2 (10 375.8178 ) 0 (13) -6 (10) -9 (12) -2 ( 9 ) 441.7428 ) -3 (14) -8 (13) -5 ( 9 ) -2 (14 443.7398 )OCDF 0 (9) -1 (12) -7 (14) -3 (15 445.7369 ) 0 (9) 1 (8) -7 (16) -5 (10 L Soot Homogenate used in Animal Toxicology Studies. �TABLE 5 Analysis of Soot Samples for 2,3,7,8 TCDD Sample Soot Horaogenate Cone, (ppm) RRT D.L. (ppm) 320/322 Ratio .46 1.0 .05 86% .26 1.0 .03 80% 1.0 .15 69% % Recovery 7.0 (floor 3-4) 713 16 (8th floor) 715 2.2 (9th floor) Soot Homogenate used in animal toxicology studies. 8% � 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. 088 Folder The folder containing the original item. 2207 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 Hilker, D. R. R. M. Smith P. W. O'Keefe K. M. Aldous Description An account of the resource <strong>Corporate Author: </strong>Toxicology Institute, Center for Laboratories and Research, New York State Department of Health, Albany, New York Date A point or period of time associated with an event in the lifecycle of the resource 1982-10-01 Title A name given to the resource Determination of Chlorinated Combustion Products in 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/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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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 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. 066 Folder The folder containing the original item. 1799 Series The series number of the original item. Series III Subseries III 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 Holmes, Nan S. Title A name given to the resource Letter: from Nan S. Holmes to Joseph J. Breen, August 8, 1983 Subject The topic of the resource Vietnam Experience Twin Study analytical studies ao_seriesIII https://www.nal.usda.gov/exhibits/speccoll/files/original/46d7e8c1116de53f865536a8067e89d2.pdf 63a37902c59369ab5873526d5b2db506 PDF Text Text RBDID Number °2193 Author Eadon G > - Center for Laboratories and Research, New York State Report/Article TltlB Comparisons of Chemical and Biological Data on Soot Samples From the Binghamton State Office Building Journal/Book Title Year 1982 Month/Day March Color Number of Images D 24 Dascrlpton Notes Thursday, September 20, 2001 Page 2193 of 2293 �Comparisons Of Chemical and Biological Data on Soot Samples From the Binghamton State Office Building G. Eadon, K. Aldous, G. Frenkel, J. Gierthy, D. Hilkerr L. Kaminsky, P. O'Keefe, J. Silkworth and R. Smith Center for Laboratories and Research ( New York\State Department of Health Albany, N^ 12201 March, 1982 �Soot samples from two separate samplings of the Binghamton State Office Building (BSOB) have been the objects of a coordinated interdisciplinary study at the New York State Health Department. On May 26, 1981, replicate soot samples were collected from above the ceiling panels of 16 of the 17 floors of the BSOB. Each sample was subjected to exhaustive soxhlet extraction (benzene). One portion of each extract was analyzed for polychlorinated biphenyls (PCBs), another for polychlorinated dibenzofurans (PCDFs) and related compounds. A third portion of all extracts not spiked with PCDDs and PCDFs as part of the chemical analysis procedure was examined using the cell keratinization assay. Another set of experiments utilized a much larger soot sample collected by a vacuum cleaner on the 3rd and 4th floors of the BSOB shortly after the fire occurred. The bulk of this sample has been used in animal toxicology studies. However/ portions of this soot were extracted and analyzed for PCBs, PCDFs, 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) and 2,3,7,8-tetrachlorodibenzofuran (2,3,7,8-TCDF). The cell keratinization assay was also applied to an extract of this sample. The results of each of these studies have been described in detail in separate reports (Smith et al. , 1981a, 1981b, 1982; Silkworth et al., 1982; Gierthy et al., 1982). This paper will seek comparisons among the various chemical and biological data sets generated with these samples, and will attempt to determine whether the results are mutually consistent. �Chemical Data The number of samples which could be analyzed for PCDFs and related trace contaminants is severely limited by the difficulty of the analytical procedure. In contrast, the quantitation of the much more abundant PCBs is a fairly straightforward process; more than 800 PCB analyses have already been reported on BSOB-related samples. If the ratios of PCB to PCDF are approximately constant then the results of the PCB analyses can be used to estimate PCDF levels, with a considerable savings in time and manpower. Table I contains analytical data relevant to the PCB and PCDF (tetra through octa chlorinated) concentrations on soot samples collected from 16 of 17 floors of the BSOB, and on the soot sample used in animal toxicology experiments. The PCB concentrations vary by nearly 3 orders of magnitude, while total PCDF levels vary from not detected approximately 1200 ppm. «1.0 ppm) to For the 11 samples in which the ratio of total PCDFs to total PCBs has been determined, the total PCDFs measured ranges from 51 ppm to 1200 ppm, and the ratio of PCDF to PCB averages .066 * .024 (error limits represent one standard deviation). t Thus, the total PCDF levels correlate with PCB levels. More detailed consideration of the data in Table I indicates that the total concentrations of tetra CDFs, penta CDFs and hexa CDFs (groupings which include the isomers predicted (see later) to be most active with respect to acute oral toxicity and keratinization) relative to the total PCDF concentration is relatively constant (Table II). In the 11 samples for which these ratios have been determined, tetra CDFs constitute 33 + 5% �of the total PCDF mixture, while penta CDFs constitute 40 + 3%, and the hexa CDFs constitute 18 ± 7% of the total mixture. Thus, the PCB concentration can be used to predict approximate concentrations of each family of chlorinated dibenzofurans in these samples. For illustrative purposes, Table III contains the measured and predicted concentrations. Further studies will be required to rigorously validate the use of PCB analysis as a surrogate for the more elaborate analytical procedures. Since concentrations of dibenzodioxins and biphenylenes (Stalling, 1981) have not yet been determined in these samples, it cannot be demonstrated that the concentrations of these compounds correlate with PCB concentrations. Further, the samples analyzed to date have all been collected before May, 1981 and have been predominantly obtained from the same location on the 17 floors. The validity of the observed correlation must be tested with more recent samples and with samples taken at other locations; the similarity of the ceiling panel samples and vacuum cleaner sample is encouraging in the latter regard. Finally, the validity of the observed correlation in the very slightly contaminated samples likely to be generated during the ! final phases of the clean-up should also be tested. �Biological Data Evaluation of the consistency of the chemical data and the biological data requires knowledge of the concentrations and toxicities of particular congeners believed to be especially active. Because of the very few reference standards available, the laboratories of the Health Department have produced little congener-by-congener analytical data. Therefore, in the following discussions it will be necessary to assume that within a particular isomeric series the relative concentration of a given isomer is comparable to its concentration in a sample earlier subjected to congener by congener analysis (Stalling, 1981; Rappe, 1981). Among the tetra CDFs, the isomer believed to be most toxic is 2,3,7,8-Tetra CDF (Poland et al., 1977). Stalling and Rappe report that this isomer constitutes 68% and 41% of the tetra CDFs. Based on these results it will be assummed that 2,3,7,8-TCDF constitutes 50% of the total tetra CDF concentration in these samples. Given the greater toxicity of 2,3,7,8-chlorinated isomers (Poland et al., 1977) the most toxic penta CDF isomers are predicted to be 1,2,3,7,8- and 2,3,4,7,8-penta CDF. Stalling and Rappe report that these congeners comprise together 47% and 53% of the penta CDF mixture. A value of 50% will be assumed in subsequent discussions. Given the greater toxicity of 2,3,7,8-chlorinated isomers (Poland et al., 1977), the most toxic hexa CDF isomers are predicted to be 1,2,3,4,7,8-, 1,2,3,6,7,8-, 1,2,3,7,8,9- and 2,3,4,6,7,8-hexa CDF. Rappe reports that the total concentration �of three of these isomers in a BSOB sample was 49% of the total hexa CDF concentration. A value of 50% will be assumed here for the four isomers. Knowledge of the relative concentrations of dibenzodioxins and dibenzofurans will also be required for these discussions. In the soot sample used in animal toxicology experiments, the 2,3,7,8-TCDD/2,3,7,8-TCDF ratio was determined to be .025 (Smith et al., 1981b). this sample. This ratio will be used in connection with However, since analytical data on the dioxin levels in the remaining samples is not yet available, an estimate of these concentrations must be made. In a sample analyzed by Rappe and Stalling, Rappe concluded that the tetra through octa PCDD/PCDF ratio was about .01, and Stalling concluded that it was less than .02. In a heavily contaminated soot sample, Smith et al (1981a) concluded that the 2,3,7,8-TCDD/2,3,7,8-TCDF ratio averaged .015. The average ratio observed in the three samples was .017; this value will be assumed for the ceiling panel derived soot samples. Based on Stalling's report (1981), the biphenylene/dibenzofuran ratio in a sample was less than .067. This value will of i necessity be used in subsequent discussions. Efforts are presently underway to obtain experimental data on the soot samples currently under discussion to place these estimates on a firmer basis. a. Animal Toxicology Experiments It is difficult to rigorously demonstrate consistency between results obtained via chemical analysis and acute toxicity data for a number of reasons. The chemical data is incomplete; �7 not all classes of toxicants have been quantified,and the concentrations of individual congeners have not been established. More important, however, very limited data is available on the acute oral toxicities of individual PCDFs, PCDDs or Polychlorinated Biphenylenes. Nevertheless, despite these and other difficulties, crude comparison of this data will be attempted. A useful first step is to express the observed acute oral toxicity of the soot in terms of "2,3,7,8-TCDD equivalents", i.e., the concentrations of 2,3,7,8-TCDD, that, in an inert matrix, would produce the observed LDgQ. An extract of soot when administered to guinea pigs in aqueous suspension exhibited an LD5Q equivalent to 327 mg soot/kg. When 2,3,7,8-TCDD was administered under identical conditions, it exhibited an LD50 of 19 ug/kg. If the soot in fact had contained only 2,3,7,8-TCDD at 58 ug/g, its extract would be predicted to exhibit an LD,-n of 327 mg soot equivalents/kg. Therefore, the "2,3,7,8-TCDD equivalent" contamination of the soot is 58 ug/g. The chemical data can then be used to "predict" the "2,3,7,8-TCDD equivalent" concentration of the soot, based on known toxicities of the components. This is a complicated task, since no data is available on the LDcris of dibenzofurans in bu guinea pigs other than 2,3,7,8-tetra CDF, and since very limited data is available on the PCDDs. The following assumptions will therefore be made about the I<DCQS of these compounds: (1) The ratio of the LDcQs of a particular PCDF congener and 2,3,7,8-tetra CDF will be the same as the ratio of the LD5Qs oE the correspondingly substituted PCDD congener and 2,3,7,8-TCDD. �8 There is no direct experimental data to support this assumption. (2) The LD50s of PCDFs and PCDDs lacking chlorines on all four lateral positions will be sufficiently high that their influence can be ignored in this calculation. This assumption is based on the LD5Qs in guinea pigs of 2,8-diCDD, 2,3,7-triCDD, and 1,2,4,7,8-penta-CDD. All have LE> s more than 450 times higher than that of 2,3,7,8-Tetra CDD itself (Table IV). (3) Introduction of a single additional chlorine substituent on a 2,3,1,8-substituted congener has essentially no effect on the congener's guinea pig LD . This assumption is based on comparison of the LD5Qs of 2,3,7,8-TCDD and 1,2,3,7,8~tetra-CDD (Table IV). (4) Introduction of two additional chlorine substituents on a 2,3,7,8-chlorinated congener raises its LD,-0 by a factor of at least 29. The assumption is based on comparison of the LD5Qs of 1,2,3,4,7,8-, 1,2,3,6,7,8-, and 1,2,3,7,8,9-hexa CDD and 2,3,7,8-tetra CDD (Table IV). (5) The LDf-QS of compounds with more than 6 chlorines will be sufficiently large that their influence can be ignored in this calculation. This assumption is based on comparison of the LD5Qs of 1,2,3,4,6,7,8-hepta CDD and 2,3,7,8-tetra CDD (Table IV). These assumptions require that attention be focussed only on the tetra, penta, and hexasubstituted PCDDs and PCDFs. The concentration of 2,3,7,8-TCDF in the sample used in animal toxicology experiments was measured at 48 ppm; since the data in Table IV indicates that the LD5Q of 2,3,7,8-tetraCDF is about three times that of 2,3,7,8-TCDD, this is equivalent in terms of acute toxicity to a 2,3,7,8-TCDD concentration of ca. 16 ug/g. �Based on assumption (2), other tetra CDFs can be neglected in this calculation. The penta CDFs were measured at 120 ug/g. If 1,2,3,7,8- and 2,3,4,7,8-penta CDF together constitute 50% of the penta CDFs, and if their LDcQS are equal to that of 2,3,7,8-TCDF, this is equivalent in terms of acute toxicity to a 2,3,7,8-TCDD concentration of ca. 20 ug/g. Based on assumption (2), other penta CDFs can be neglected in this calculation. hexa CDFs have been measured at 70 ug/g. The The isomers believed to have the lowest LD5Qs (1,2,3,4,7,8-, 1,2,3,6,7,8-, and 2,3,4,6,7,8-hexa CDF) are expected to comprise 50% of the total hexa CDF mixture. Since, based on assumption (4), their LD^s are 29 times higher than that of 2,3,7,8-TCDF, this is equivalent to a 2,3,7,8-TCDD concentration of 0.4 ug/g. calculated Thus, the PCDFs are to constitute a "2,3,7,8-TCDD equivalent" concentration of 36 ug/g. The concentration of 2,3,7,8-TCDD itself has been measured at 1.2 ppm in this sample. Other tetrachlorinated dibenzodioxins are predicted to have much higher LD,-QS and can be ignored. The concentration of other PCDDs in this sample are unknown, but are likely to be comparable to the TCDDs. Thus, the dioxins as a whole probably have a negligible influence on the soot's "2,3,7,8-TCDD equivalent" concentration. Stalling (1981) has reported on the presence of polychlorinated biphenylenes in a soot sample from BSOB; he cites unpublished results by Dr. Alan Poland that suggests that the toxicity of the 2,3,6,7 congener is comparable to that of 2,3,7,8-tetra CDD. If Stalling's ratio of biphenylene to dibenzofuran is (.067) is assummed to hold for all of these �10 compounds, and if it is assummed that the biphenylenes have acute oral toxicities three times that of the corresponding dibenzofurans, it can be calculated that the biphenylenes will contribute about 0.2 times as much "2,3,7,8-TCDD equivalent" activity as the dibenzofurans. Thus, to a very crude approximation, the polychlorinated biphenylenes account for a "2,3,7,8-TCDD equivalent" concentration of 7 ppm. In summary, the dibenzofurans and the tetra CDDs are estimated to constitute a "2,3,7,8-TCDD equivalent" activity of 37 ug/g. Together, the remaining dibenzodioxins and the biphenylenes probably provide a significant but smaller "2,3,7,8-TCDD equivalent" activity. This calculation is in good, probably somewhat fortuitous agreement with the observed activity in the soot-equivalent to a 2,3,7,8-TCDD concentration of 58 ug/g. Since considerable effort has been devoted to animal toxicology experiments on a single large sample of soot, it is important to assess whether this sample is reasonably typical. The data in Table I indicates that the average PCB concentration in 16 samples collected above the ceiling panels at the BSOB is ( 7200; the PCB concentration in this sample is 5,000 ppm. " The average total PCDF concentration on 14 such samples was ppm; the total PCDF concentration in this sample is 320 ppm. The average ratio of total PCDF to PCB in the 12 samples for which this is well defined is .066; the ratio for this sample was .063. The proportions of tetra- penta-, and hexa CDFs in this sample are similar to those in the ceiling panel samples (Table II). the sample used in animal toxicology experiments appears Thus, �11 comparable to the samples collected from above the ceiling panels, based on presently available data. b. Cell Keratinization Assay Development of the cell keratinization assay based on an in vitro keratinization model (Knutson et al., 1981) has been pursued because of its potential use as an alternative or supplement to chemical analysis. Both applications demand that the biological and chemical methods generate mutually consistent results. One question can be answered fairly readily. Do the two methodologies agree which samples fall into particular broad categories of contamination? The samples and blanks run as part of this program exhibit four broad categories of contamination. Blanks did not exhibit positive responses in this assay. A single sample (floor 1) exhibited activity equivalent to 0.01 0.10 ppm 2,3,7,8-TCDD; chemical analysis detected only 0.2 ppm Tetra-CDF. Three samples (floors 4,6, and 14) exhibited activities near 0.10 - 1.0 ppm; chemical analysis confirmed low levels of PCDFs in these samples (total PCDFs of 51, 76, and 87 ppm). The remaining samples in which PCDFs were detected chemically exhibited activities ranging from 1.1 - 11 ppm to 5.3 ! - 53 ppm. Chemical analysis confirmed that these samples were more heavily contaminated (total PCDFs of 410 , 200, 320, 1200, 400, 750, and 670 ppm). Table V. These results are collected together in They suggest that the keratinization assay results correlate with chemical data. It is markedly more difficult to determine whether the activity observed in the cell keratinization assay is quantitatively consistent with chemical analysis. Little �12 published information exists to relate the keratiniation activities of the various compounds present in the soot to one another. However, the following assumptions will be made to permit a crude calculation: (1) The ratios of the activity of a particular dibenzofuran congener to 2,3,7,8-TCDF is equal to that of the ratio of the activity of the corresponding dibenzodioxin congener to 2,3,1,8-TCDD. assumption. (2) There is no direct support for this 2,3,7,8-Tetra CDF is 1/20 as active as 2,3,7,8-TCDD (Knutson et al., 1980). (3) Congeners not substituted at all four lateral positions are sufficiently inactive to be neglected. This assumption is based on comparison of the activities of 2,3-, 2,7-, 1,6-, 1,3,6,8-, 1,3,7,8-, and 2,3,7- chlorodibenzodioxins to 2,3,7,8-tetra CDD. al., 1980) (Table VI). (4) (Knutson et Introduction of a single additional chlorine on a 2,3,7,8 chlorinated nucleus decreases activity by a factor of 2. This assumption is based on a comparison of the activities of 1,2,3,7,8-Penta CDD and 2,3,7,8-tetra CDD (Knutson et al., 1980) (Table VI). (5) Introduction of two or more chlorines depresses activity sufficiently to make the activity of such compounds negligible. This assumption is based on comparison of the activities of 1,2,3,7,8,9-hexa CDD and 2,3,7,8-tetra CDD (Knutson et al., 1980) (Table VI). (6) Polychlorinated biphenylenes are 1/2 as active as the corresponding dibenzodioxin. This generalization is based on comparison of the activities of 2,3,6,7-tetra CB and 2,3,7,8-tetra CDD (Knutson et al., 1980) (Table VI). As a direct result of assumptions (3) and (5), the bulk of keratinization activity will reside in tetra- and penta- �13 chlorinated compounds. As already discussed, 2,3,7,8-tetra CDF is predicted to be by far the most active tetra CDF, and expected to constitute 50% of the tetra CDF mixture. Since 2,3,7,8-tetra CDF is 1/20 as active as 2,3,7,8-TCDD, the "2,3,7,8-TCDD equivalent" activity due to this compound can be obtained by dividing the total tetra CDF concentration by 40. Similarly, the "TCDD equivalent" activity of the two most active penta CDFs can be estimated by dividing the total penta CDF concentration by 80. The calculated "2,3,7,8-TCDD equivalent" activity due to PCDFs is compared to the experimentally observed value for a number of samples in Table VII. The PCDDs will make a significant contribution to the cell keratinizing activity of these samples; although they are estimated to be 1/50 to 1/100 as abundant as the PCDFs, they may be 20 times as potent in the assay. The polychlorinated biphenylenes may be even more important factors in this analysis. Stalling's data suggests that they may be 1/10 to 1/20 as abundant as the PCDFs. as active. However, they are reported to be 10 times Thus, the calculated values in Table VII are likely to be below the values that would be calculated if more complete t analytical data were available. However, in view of the large uncertainties present in these calculations and the data upon which they are based, the calculated and experimental data are in fair agreement. It should be noted that the soot sample used in the animal toxicology experiments exhibited a cell keratinizing activity of 2-20 ppm "2,3,7,8-TCDD Equivalents", and a calculated activity of 4 ppm due to PCDFs. This differs from the "2,3,7,8-TCDD �14 equivalents" calculated and observed in the animal toxicology experiments This does not represent a discrepancy in the data. Rather, it is due primarily to the large difference between the ratios of the guinea pig LD5Qs for 2,3,7,8-TCDF and 2,3,7,8-TCDD, and the corresponding ratios of cell keratinization activity. Conclusions (1) Available chemical data indicate that the relative concentrations of PCBs, tetra-, penta-, and hexa-CDFs, and total PCDF are similar in soot samples taken from above the ceiling panels of the BSOB, and in a sample collected by vacuum cleaner during the early stages of the clean-up. If this relationshiip is valid for samples collected at other times and from other locations, the PCB analysis can serve as a useful surrogate for the more difficult analytical procedures. (2) A soot sample exhibited an LDcQ in guinea pigs equivalent to 58 ppm 2,3,7,8-Tetra CDD. If certain assumptions are made about the chemical composition of this sample and the LD s of the compounds therein, it can be calculated that the PCDFs, tetra CDDs, and the biphenylenes should account for ca. 45 ppm "2,3,7,8-TCDD equivalent" activity. Since this calculation ignores other chlorinated dioxins, it is in good (probably fortuitous) agreement with the observed value. Based on these results, there appears to be no basis for proposing unusual synergistic or antagonistic effects among the components in this mixture. (3) The cell keratinization assay can reliably distinguish among samples containing widely differing concentrations of PCDFs. If certain assumptions are made about �15 the chemical composition of compounds therein, it can be calculated that the observed keratinizing activity in these extracts is generally plausible. (4) Chemical analysis and the cell keratinization assay suggest that the soot used in animal toxicology studies is fairly typical of the soot samples collected from above the ceiling pannels of the BSOB. �TABLE I Concentrations (ppm) of Polychlorinated Biphenyls and Polychlorinated Dibenzofurans in. Soot Samples Taken From the Binghamton State Office Building Floor # PCBsa PCDFsb Tetra CDF 2 28 3 4 1300 1 6 5 840 7 8 9 2800 6600 1800 23000 10 11 12 9600 21000 11000 13 3400 14 15 930 10000 16 9200 17 Ave 3-4* 6500 7200 5000 0.2 <8g 16 220 23 190 70 320 140 250 d d 32 300 h 220 145 100 Penta CDF <0.2g <9g 21 280 36 180 79 440 170 360 d d 31 310 150h 260 165 120 Hexa CDF <0.3g <llg 13 180 14 35 32 290 84 260 d d e 56 89h 140 86 70 Hepta CDF <0.3g <12g 1.2 62 3 3.7 14 100 6.5 97 d d 5.8 71 33h 32 31 20 Octa CDF <0.3g <14g 1.2 21 0.5 -- 3 35 2 31 d d 2.8 17 llh 15 11 4 51 760 76 410 200 1200 400 1000 — 87 750 670 438 310 .027 .062 .11 .052 .042 .048 .094 .075 .103 .066 .062 Total PCDF Ratio Total PCDF cone. PCB c o n e . . 0 6 1 (a) quantitated as Arochlor 1254; data uncorrected for recovery (b) correction for recovery incorporated ( ) not sampled because of dissimilar ceiling construction c (d) data not used because of poor recovery of internal 37 C1-Tetra CDF standard (<10%) (e) data lost because of instrumental malfunction; for purposes of calculation of total PCDF, it is assummed that hexa CDF is % the concentration of penta ( f Table 2) c. (f) soot collected by vacuum cleaner and used in animal toxicology studies (g) detection limits are per congener, not per chlorination number data not corrected for recovery. Instrument malfunction caused loss of data on 37C1-Tetra CDF recovery �Table II Relative Proportions of Tetra-, Penta-, Hexa-, Hepta- and Octachlorodihenzofurans in Soot Samples Taken from the Binghamton State Office Buildinga Floor # 4 5 6 7 8 9 10 11 14 15 17 Aveb Tetra CDF 31 29 30 46 35 27 35 25 37 39 33 33 ± 5 32 Penta CDF 41 37 47 44 40 37 41 36 36 41 39 40 ± 3 38 Hexa CDF 25 24 18 9 16 24 21 26 -- 7 21 18 ± 7 22 2 8 4 1 7 8 2 10 7 10 5 6 ± 3 6 Hepta CDF 3-4° _ Octa CDF <1 3 1 <1 1 3 <! 3 (a) Expressed as percent of total PCDF in sample.' (b) Error limits represent one standard deviation. (c) Soot sample used in animal toxicology studies. 3 2 2 _-— 1 �CO Table III Comparison of Predicted3 (and Observed) Concentrations (ppm) of PCDFs in BSOB Soot Samples Floor # 1 3 4 9 6 10 11 14 15 17 3-4 Jetra CDF 0.6(0.2) 26( 8) 17(16) 56(23) 133(190) 39(70) 60(320) 190(140) 420(250) 19(32) 200(300) 130(220) 100(100) Penta CDF 0.9(<.2) 30(<9) 19(21) 64(36) 151(180) 45(79) 130(440) 220(170) 480(360) 21(31) 230(310) 150(260) 115(120) Hexa CDF 0.3(<.3) 16(<11) 10(13) 33(14) 79(35) 23(32) 70(290) 115(84) 250(260) 11C") 120(56) 78(140) 60(70) Hepta CDF 0.1(<.3) 5.6(<12) 3.6(1.2) .6(1.2) 12(3) 28(3.7) 8.4(14) 99(100) 41(6.5) 90(97) 5(5.8) 43(71) 28(32) 22(20) Octa CDF .04(<.3) 1.3(<1.2) 4.2(0.5) 10(--) 35(35) 15(2) 32(31) 1.4(2.8 15(17) 10(15) 84 () Total PCDF 1.9 2(<13) 80 51(51) 3(3) .400(1200) (a) Prediction based on PCB levels and average ratio calculated in Table I and II 580(400) 1300(1000) 57(87) 610(754) 400(670) 300(310) �19 Table IV Influence of Structure and Chlorination Pattern on Guinea Pig Oral LD5Qs (Male, Hartley, 200-250g) Compound LD3 U • <f «— cn(ug/kg) 2,3,7,8-Tetra CDD 2.5a 2,3,7,8-Penta CDF 5-10b 1,2,3,7,8-Penta CDD 3.1° 1,2,3 ,4,7,8-Hexa CDD 73C 1,2,3,7,8,9-Hexa CDD 60-100° 1,2,3,6,7,8-Hexa CDD 70-100° 1,2,3,4,6,7,8-Hepta CDD >600° 1,2,4,7,8-Penta CDD 1,125° 2,3,7-Tri CDD 29,444° 2,8-Di CDD 730,000° a J.B. Silkworth, D. McMartin, A.P. DeCaprio, R. Rej, S. Kumar and L. Kaminsky (1981). Acute toxicity in guinea pigs and rabbits of soot from a polychlorinated biphenyl-containing transformer fire, N.Y. State Dept. of Health Report, January 6, 1982. J.A. Moore, E.E. McConnell, D.W. Dalgard, and M.W. Harris (1979). Comparative toxicity of three halogenated dibenzofurans in guinea pigs, mice and thesus monkeys. NY Acad. Sci. 320, 151-163. °E.E. McConnell, J.A. Moore, J.K. Baseman, and M.W. Harris (1978). The comparative toxicity of chlorinated dibenzo-p-dioxins in mice and guinea pigs. Toxi co 1. Pharmacol. 44, 335-356. 0 �Table V o CSl Comparison of the Observed Keratinization Activities with Total PCDF Concentrations Observed Floor I "2,3,7,8-TCDD Equivalents(ppm) Total PCDF Concentrations 1 . 1 1 0 - 6 0.1-1.0 76 4 .11-1.1 51 14 .12-1.2 87 3 1.2-12 b 9 1.1-11 1200 8 1.6-16 200 3-4a 2-20 310 10 3.2-32 400 15 4.0-40 750 17 4.0-40 670 7 5.3-53 410 a Soot used in animal toxicology experiments •L^ Total concentration not defined, (cf. Table I) b (ppm) �21 Table VI Influence of Structure and Chlorination Pattern on Relative Activity in the Cell Keratinization Assay3. Compound Relative Activity 2,3,7,8-Tetra CDD 1 2,3,7,8-Tetra CDF 0.05 2,3/6,7-Tetrachlorobiphenylene 0.5 1,2,3,7,8-Penta CDD 0.5 2,3,7-Tri CDD 0.01 1,3,7,8-Tetra CDD 0.01 1,2,3,7,8,9-Hexa CDD 0.005 1,3,6,8-Tetra CDD < .003 1,6,-DiCDD < .001 i 2.7-DiCDD < .001 2.3-DiCDD < .001 (a) Data adapted from J.C. Knutson and A. Poland (1980). Keratinization of mouse teratoma cell line XB produced by 2,3,7,8-tetrachlorodibenzo-p-dioxin: an in vitro model of toxicity, Cell 22, 27-36. �Table VII Comparison of the Observed Keratinization Activity in BSOB Soot Samples with Value Predicted based on PCDF Concentrations « Floor # Observed "2,3,7,8-TCDD equi Lents" (ppm) Calculated "2,3,7,8-TCDD equivalents" (ppm) PCDFs only 1 .Ol-.l (b) 6 0.1-1.0 1 4 .11-1.1 1 14 .12-1.2 1 3 1.2-12 (b) 9 1.1-11 10 8 1.6-16 3 3-4a 2-20 4 10 3.2-32 6 15 4.0-40 10 17 4.0-40 9 7 5.3-53 7 (a) -(b) Sample used for animal toxicology studies, PCDFs not detected in chemical analysis. �; 23 REFERENCES Gierthy, J.P. and Prenkel, G.D. (1982). A preliminary report on the c.,-aluation of an In Vitro assay for the detection of "dioxin-like" activity using extracts of soot from the Binghamton State Office Building. New York State Department of Health Report, January, 1982. Knutson, J.C. and Poland, A. (1980). Keratinization of mouse cell line XB produced by 2,3,7,8-tetrachlorodibenzodioxin: an in vitro model of toxicity. Cell, 22, 27-36. Poland, A., and Glover, E. (1977). Chlorinated biphenyl induction of aryl hydrocarbon hyudroxylase activity: the structure-activity relationship. a study of Mol. Pharmacol., 13, 924-38. Rappe, C. (1981) Report on the analysis of Binghamton soot. Report, University of Umea, Sweden, 1981. Silkworth, J. , McMartin, D., DeCaprio, A., Re j, R. , O'Keefe, P., and Kaminsky, L. (1982). Acute toxicity in guinea pigs and rabbits of soot from a polychlorinated biphenyl-containing transformer fire. January 6, 1982. New York State Department of Health Report, �'> • I A 'i 24 i Smith, R.M., O'Keefe, P.W. , Hilker, D.L., Jelus-Tyror, B.L., and Aldous, K. (1981a). Analysis of 2,3,7,8-tetrachlorodibenzofuran and 2,3,7,8-tetrachlorodibenzo-p-dioxin in a soot sample from a transformer explosion in Binghamton, New York. New York State Department of Health Report, February 20, 1981. Smith, R.M., Hilker, D.L., O'Keefe, P.W., Kumar, S., O'Brien, J., Jelus-Tyror, B.L., and Aldous, K. (1981b) Analysis of a Binghamton soot sample for tetrachlorodibenzofurans and tetrachlorodibenzo-p-dioxins. New York State Department of Health Report, October 1, 1981. Smith, R.M., Hilker, D., O'Keefe, P.W., Kumar, S., Aldous, K., and Jelus-Tyror, B. (1982). Determination of polychlorinated dibenzofurans and polychlorinated dibenzodioxins in soot samples from a contaminated office building. New York State Department of Health Report, March, 1982. Stalling, D.L., (1981) Chlorinated dibenzofurans and related compounds in soot formed in a transformer fire in Binghamton, ( N.Y., Preliminary Report, Columbia National Fisheries REsearch Laboratory, U.S. Fish and Wildlife Service. � 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. 2193 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 Eadon, G. K. Aldous G. Frenkel J. Gierthy D. Hilker L. Kaminsky P. O'Keefe J. Silkworth R. Smith Description An account of the resource <strong>Corporate Author: </strong>Center for Laboratories and Research, New York State 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 Comparisons of Chemical and Biological Data on Soot Samples From the Binghamton State Office Building Subject The topic of the resource BSOB PCBs analytical studies 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. 2191 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 Carpenter, David O. Title A name given to the resource Letter: from David O. Carpenter to Alvin L. Young, March 17, 1982 Subject The topic of the resource BSOB building remediation analytical studies PCBs 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. 2185 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 Roberts, Gail Source A related resource from which the described resource is derived The Sun-Bulletin Date A point or period of time associated with an event in the lifecycle of the resource October 8 1981 Title A name given to the resource Expert Says More Tower Tests Needed Subject The topic of the resource BSOB analytical studies building remediation popular press 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 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. 2180 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 Schecter, Arnold J. Title A name given to the resource Letter: from Arnold J. Schecter to Alvin L. Young, August 6, 1981 Subject The topic of the resource BSOB PCBs analytical studies building remediation