Document 5kZ4qO8Gb3EprM50wxy8zrQVD

Monsanto 11052 COPY/ Environmental Services Report /<> 04- t. ?Z_ JOB/PROJECT NO.: 462.2070 DATE: 23 April 1982 TITLE: ANALYSIS Of WATER AND SEDIMENT SAMPLES FROM THE SAUCET. ILLINOIS WASTE TREATMENT PLANT AUTHOR: Robert F. Ivory ABSTRACT: Water and sediment samples from the Sauget. Illinois Waste Treatment Plant were analysed Cor the U.S. Environmental Protection Agency's for the priority and non-priority pollutants. The results of this analyses are presented in this report. RECEIVED APR 2 tK--' MONSANTO-DAYTON CENTRAL files Monsanto Rasaarch Corporation. Station B. Bo* 8 o Dayton. Ohio 45407 (513) 268,3411 MONS 022392 COPY NUMBER 1 Carl Marciante 2*3 Steven Smith 4 R. F. Ivory 5 Central Filaa Sauget. 1L Sauget, 1L Dayton Dayton ABSTRACT ONLY R. K. Flitcraft/Dayton R. H. Scott/Dayton ACKNOWLEDGEMENT Contributions of the following Dayton Laboratory personnel to this project are gratefully acknowledged: Analyses: s. A. Barksdale A. Ford D. R. Crothe F. D. Hileman B. M. Hughes P. Hughes S. J. Johnson J. T. Miller S. Mitrosky Morrow D. E. Sharp H. M. Strickland G. Thomas T. E. Wcosley MOWS 022393 CONTENTS Fm 1. INTRODUCTION.............................................................................................. 1 2. SAMPLING....................................................................................................... 1 3. SAMPLE EXTRACTION AND SCREENING FOR ORGANIC POLLUTANTS.............................................................................................. 3.1 Volatile Priority PollutantAnalyse* .......................... 3.2 Extractable Or9anic PriorityPollutants..................... 3.3 wide Scan Organic Analyses........................ 3.4 Discussion of Priority Pollutant and Wide Scan Analyses .................................................................................... 4. ANALYSES FOR CHLORINATED DIBENZO-F-DIOXINS AND DIBEKEOFURANS .................................................................................... 5. ANALYSIS CF OIL SAMPLE FOR PCBs............................................... 1 2 2 3 3 3 4 6. STATIC DAFHN1A MAGNA BIOASSAY..................................................... S 7. EP TOXICITY TESTING OF SLUDGE................................................. 6 8. ADDITIONAL ANALYSES OFSLUDGE SAMPLE ................................... 7 9. ANALYSES FOR PRIORITY AND NON-PRIORITY METAL POLLUTANTS IN WATER...................................................................... 7 1C ANALYSES FOR TOTAL CYANIDE AND TOTAL PHENOL IN WATER SAMPLES................................................................................................... 11. NON-PRIORITY POLLUTANT COMPOUNDS ........................................... 7 7 12. REFERENCES.............................................................................................. 8 APPENDIX A. GC/MS analyses of extractable organics ............................ A-l 0183/A-D ill HONS 02239* Humber FIGURES Nw 1 Capillary GC/F1D chromatogram of surrogate compound spiking standard added to each sanple before extraction............................................... 9 2 Capillary GC/FID chromatogram of the base/ neutral extact of the aethod blank (Burdick and Jackson Water, distilled in glass)................... 10 3 Capillary cc/FlD chroaatogram of the acid extract of the aethod blank (Burdick and Jackson Water, distilled in glass)........................ 11 4 Capillary CC/FI0 chroaatogram of the base/ neutral extract of influent sample froa Sauget, IL Treatment Plant, diluted ten tiaes before analysis................................................... 12 5 Capillary GC/FID chroaatogram of the acid extract of the influent sanple from Sauget, It Treatment Plant, diluted ten times before analysis.................................................................................... 13 6 Capillary GC/FID chromatogram of the base/ neutral extract of the effluent sample from Sauget. IL Treatment Plant, diluted ten times before analysis .................................................................. 14 7 Capillary GC/FID chromatogram of the acid extract of the effluent sample from Sauget, IL Treatment Plant, diluted ten times before analysis.................................................................................... IS 8 Capillary GC/FID chromatogram of the base/ neutral extract of a duplicate effluent sample from Sauget, IL Treatment Plant, diluted ten timesbefore analysis . ..................... 16 9 Capillary GC/FID chromatogram of the acid extract of a duplicate effluent sample from Sauget, IL Treatment Plant, diluted ten times beforeanalysis....................................................... 17 10 Capillary GC/FID chromatogram of the extract of a 1.07 g sediment sample from Sauget, IL Treatment Plant, diluted ten times before analysis..................................................................................... IB iv HONS 022395 Huger U 12 13 H F1CURS (continued) ^3? Capillary CC/FIO chroaatoqran of tho extract of a 1.38 9 duplicate aedieent saaple froa Sau9et. IL Treatment Plant, diluted ten tiaee before analysie ..................................................................... 1* Analysis of 59 vq/mL Aroclor 12S standard. using (GCI'/HS-SIM analysis techniques. ... 20 Analysis of an oil sample, using (GC)*/MS--SIM analysis techniques ................................................................ Extraction procedure flowchart..................................... 21 22 v HONS 022396 Humber 1 2 3 4 5 6 7 6 9 10 11 12 TABUS Fiat Amount of Chronatographable Compounds Detected in the Base/Meutral Extract of the Influent Saaple. Diluted Ten Tinea Before Analyaia . . 23 Amount of Chronatographable Coepounda Detected in the Acid Extract of the Influent Sample, Diluted Ten Tines................................................................... 28 Amount of Chroeatographable Compounds in Detected in the Base/Neutral Extract of the Effluent Saaple. Diluted Ten Tines Before Analysis.................................................................................... Amount of Chronatographable Compounds in Detected in the Acid Extract of the Effluent Saaple. Diluted Ten Times Before Analysis . 30 33 Amount of Chronatographable Compounds in Detected in the Base/Neutral Extract of the Effluent Duplicate Sample, Diluted Ten Times Before Analysis ................................................................. 34 Amount of Chronatographable Compounds in Detected in the Acid Extract of the Effluent Duplicate Sample. Diluted Ten Times Before Analysis.................................................................................... 3~ Amount of Chronatographable Compounds Detected in the Methylene Chloride Extract of the Sedment Sample. Diluted Ten Tines Before Analysis.................................................................................... 38 Amount of Chronatographable Coaipounds Detected in the Methylene Chloride Extract of the Sediment Duplicate Sanple. Diluted Ten Tines Before Analysis .................................................................. 42 Total Concentrations of Extractable Compounds Present in Water and Sediment Extracts, Analyzed using Three Different Methods. ... 46 Priority Pollutant Screening Levels GC/MS ... 47 Screening Levels for Pesticides/PCB's Extract able Priority Pollutants................................................ 48 Analytical Results for Volatile Organic Priority Pollutants in Water Samples, pg/L (ppb)................................................................................ 48 vi HONS 022397 Humber 13 11 15 1" It :: 22 23 TABLES (continued) page Analytical Results for Extractable Organic Priority Pollutants in water samples, wg/L (ppb).................................................................................... 49 Analytical Results for Extractable Organic Priority Pollutants in Sediment Samples, ug/g (ppm).................................................................................... 50 Quality Control Data for Organic Priority Pollutant Analysis of Water Samples ........................ SO C-ality Data for Organic Priority Pollutant Analysis o: Sediment Sample .......................................... so N.-r.-Priority Pollutant Organic Compounds Detected in Three Volatile Samples Prom Sauget Treatment Plant........................................................ SI Identification of Major Extractable Organic Compounds in the Ease,Neutral Extract of the Method Plank..................................................... Identification of Kjaor Extractable Organic Compounds ir. the Acid Extract of the Method Plank....................... .... ......................................... . 53 Identification of Major Extractable Organic Compounds in the Bese/Neutral Extract of the Influent Sample. Diluted 1:10, Not Corrected for Background............................................. 54 Identification of Major Extractable Organic Compounds in the Acid Extract of the Influent Sample, Diluted 1:10. not Corrected for Background............................................................................... 57 Identification of Major Extractable Organic Compounds in the Base/Neutral Extract of the Effluent Sample, Diluted 1:10, not Corrected for Background............................................. SB Identification of Major Extractable Organic Compounds in the Acid Extract of the Effluent Sample, Diluted 1:10, not Corrected for Background............................................. 82 52 vii MON S 022398 Humber 24 25 24 27 26 29 30 31 32 33 34 34 36 37 TABLES (continued) Tag* Identification of Major Extractable organic Compounds in the Baac/Neutral Extract of the Effluent Duplicate Sanple, Diluted 1:10. not Corrected for Background............................. Identification of Major Extractable Organic Compounds in the Acid Extract of the Effluent Duplicate Saaple. Diluted 1:10. not Corrected for Background...................................... 44 47 Identification of Major Extractable Compounds in the Methylene Chloride Extract of the Sedieent Sample. Diluted 1:10. not Corrected for Background....................................................................... 69 Identification of Major Extractable Compounds in the Methylene Chloride Extract of the Sediment Duplicate Sample. Diluted 1:10. not Corrected for Background...................................... 73 Analysis of chlorinated Dibenzo-P-Dioxins in water Samples.................................................................. 76 Analysis of Chlorinated Dibenzo-P-Dioxins in Water Samples.................................................................. 77 Analysis of Chlorinated Dibenzo-P-Dioxins in Sludge Samples....................................................................... 78 Analysis of Chlorinated Dibenzofurans in Sludge Samples..................................................................................... 78 RCRA Metals in Sludge Leachate...................................... 79 Herbicide and Pesticide Concentration in Leachate..................................................................................... SO Cyanide and Phenol Analysis of Leachate .... B0 Total Metals Analysis of Sludge Sanple..................... 81 Analytical Results for Priority and Mon Priority Metal Pollutants in Water Samples. . B2 Quality Control Data for Metals Analyses of Water Samples ....................................................................... 83 viii HONS 022399 Muisber 38 39 40 TABLES (continued) Page LOQ Values for Metals by 1CP Analyses................... 84 Analytical Results for Total Cyanide and Total Fhenol in Water Saaples .................................................... 8S Analytical Results foi Non-Priority Pollutants in water Sasiples...................................................................... 85 ix MOMS 022400 1. INTRODUCTION wale: and sludge staples collected at the Sauget. Illinois Waste Treatment plant were submitted to the Dayton Laboratory for priority and non-priority screening analyses. All analyses were conducted m accordance with the U.S. Environmental Protection Agency's (EPA) approved procedures (1, 2, 3, 4, 5). 2 . SAMPLING Sar-jr 1 ing was performed at the Sauget. Illinois by Waste Treatment 1 : .1-1 Samples were received at the Dayton Laboratory and submitte to the various analysts. " SAMPLE EXTRACTION UO SCREENING FOR ORGANIC POLLUTANTS C:.v .r.fluent. one effluent and one sediment sample from the Sa-get. Illinois tieatment plant were received for priority po.Iutant and wide scan organic analyses. A method blank, consisting of a one liter Burdick and Jackson distilled in glass organic free water, a duplicate of the effluent and a d_: 1:cate .of the sediment sample were also analyzed for quality ccr.tiol purposes. Each water sample was spiked with 100 wg/L eic. rf phenol-d... Cl 2 -benzene-d4 . pyrene-d, ,, and chrysene-d,] liquid liquid extraction according to the EPA Method 825 a... sis protocol. The sediment sample and duplicate were s;iked with the same surrogate spiking compounds, but at levels ro::esponding to ie7 pg/g for the sediment and 145 ug/g for the seii.cent duplicate. Al. sample extracts were screened using capillary GC/FID analysis techniques. Figure 1 shows the chromatogram from the CC/FID analysis of the surogate compound spiking standard added to each sarple before extraction and Figures 2-11 show chromatograms from the analysis of the base/neutral and acid extracts from the water sa.-ples and methylene chloride extracts of the sediment and sedi ment duplicate. The method blank extracts were analyzed with no dilution of the extract, while the remaining water and sediment extracts required dilutions of 1:10 due to the very high levels of organic compounds present. The laboratory data system was used to generate a summary report of extracts analyzed in Figures 4-11. Tables 1-8 show these results. They contain a retention time, an area, and an estimated concentration for each peak observed in the capillary GC/FID chromatograam (Figures 2-11). Note that very high levels of phenol-d| and Clt-benzene-d< are reported in the water extracts, due to other co-eluting compounds. The identity of the nalor 1 HONS 022401 components shown in Tsbles 1-8 will be discussed in later sections on the analysis of priority pollutants and other organic compounds in these samples. The totsl aaounts of chromatographable coapounds axe summed at the end of each table. These totals are based upon the assump tion that the FID response of the coapounds are equal to the anthracene-d!,, internal standard. Table 9 summarizes these values found from the CC/FID analysis. This table shows that there it very little difference between the influent and effluent water samples and that very good agreement it observed for the water and sediment duplicate analyses. Table 9 also shows the total amount of compounds identified from GC/WS analyses, to be discussed in a later section. The following sections give detailed mass spectrometnc results concerning the levels of priority pollutants and other organic compounds in these samples. Due to the requirement of sample dilution before analysis, only approximately 40 mayor components are identified in the water and sediment extracts. Also note that it is not certain what extraction efficiencies these compounds exhibit, especially in water samples containing high concentration levels of organic compounds. Therefore the levels which are reported in the following sections present lower level concentrations of compounds which are present in these samples. Other more direct analyses, such as direct aqueous sample injection, were beyond the scope of the present study. 3.l Volatile Priority Pollutant Analyses One organic free water sample (used as a method blank) and three water samples labelled 9:19 a.m.. 10:23 p.m. and 11:19 a.m. were analyzed for the volatile priority pollutants listed in Table 10 using CPA Method 624 (1. 2). Table 12 gives the results of these analyses for those priority pollutants detected. 3 2 Extractable Organic Priority Pollutants A method blank, an influent sample, an effluent sample, a duplicate effluent sample, a sediment sample and a duplicate sediment sample were analyzed for base/neutral, pesticide and acid extractable priority pollutants listed in Tables 10 and 11 using CPA Method 629 (1. 2) analysis protocol. Tables 13 and 14 summarise the results for those priority pollutants detected. Before extraction began, the water and sedismnt samplea were each spiked with phenol-d*. Cl]-benxene-d4. pyrene-dt> and chrysene-d,, surrogate spiking compounds. Tables IS and 14 summarize recoveries of these compounds in the various extracts analysed. 2 HONS 022402 3.3 wide Scan Organic Analyses Large amounts of non-priority pollutant organic compounds were observed in the volatile and extractable organic priority pollut ant analyses, given above. Table 17 gives the tentative identi fication of compounds and estimated amounts of detected compounds in the volatiles analysis and Tables 18 through 27 give these data for extractable compounds. Appendix A gives detailed information on the methods used for identification of non-priority pollutant extiactable compounds. 3 4 Discussion of Priority Pollutant and wide Scan Analyses Table 9 summarises the total concentrations of extractable orgimc cor* ; cur.ds measuied in watei and sediment extracts from the Saujet. Illinois Watei Treatment Plant. The total amounts reported ir. thif tatle a:e calculated ty three different analytical methods The totals measured under "CC/F1D" assumes all chromatographab*e cor.;c.;r.ds have F: L responses equal to anthracene-d,(used as a:, internal standard). The totals measured under "CC/MS-Total" assures all cht or.atographab le compounds have mass spectrometz ic responses equal to a:\thracer.e-di < The totals measured usinq "GC KS-Ff ' ate totals of all priority pollutants measured using EFA Method tZl This latte: method uses authentic standards for each of the detected priority pollutants and thus are more accurate (for the priority pollutants) than either of the previous totals listed ir. the tac.e. However this last total does not contain the amounts o: r. j:-p: :oi it/ pollutants which are present in the various sarple extracts All three base Neutral extractable water analyses show that the major organic components are not priority pollutants and thus the CC FID and GC >:s-Total amounts are free 4 to 1? times larger than the GC/WS-PP totals. All three acid extractable water analyses show that the major organic components are the acid priunty pollutants and therefore the gc/ms-PP tota.s for these extracts are approximately the same as the totals measured using the other two methods of analysis. The fact that the latter acid extractable analysis actually produces total amounts approximately twice that measured from GC/FID and GC/WSTotal is due to the more accurate method of quantitation for the acid priority pollutants. 4. ANALYSES FOR CHLORINATED DIPENZO-P-DIOXINS AND DIBENZOFURANS Water samples were prepared by extracting one liter of water with 40 mL of petroleum ether by shaking for 15 minutes. The ether was removed and further cleaned up by extracting with two SO mt washes of IN KOH. This ether extract was dried over sodium sulfate, concentrated to 2 mL and then chromatographed on a column of siliea gel. silica gel plus H}SO. and silica gel plus KOH. The column was eluted with 4S mL of hexane which was again concentrated to 3 HONS 022403 2 kLs. The concentrate was then chromatographed on a 2.5 gm Woelm B aluauia column. This coluan was first eluted with 10 Ml of 21 CH,Cl,/Hexane and this fraction discarded. A second elution was carried out with IS aL of S0% CH,Cl,/Hexane; 300 pL of dodecanc was added as a keeper, the saaple was concentrated to 300 pL and submitted for CC/MS analysis. The sludge samples were prepared in a similar manner. One gram of sludge was spplied to the top of a four gram silica gel column. The sample was eluted with 30 at of CH,C1, and the collected fraction was concentrated to 2 sL and applied to the multi stage silica column as described for the water samples. The work up then proceded in a manner comparable to the water samples. Replicates, low and high level spiked and blanks were processed with all samples. The CC/MS analysis was carried out on a Hew.'ettFackard 59E5B CC/MS. A 30 meter SE-S4 capillary column was used fo: the separation of the PCDDs and PCDFs. The mass spectrometer was operated in the selected ion monitoring mode following ions characteristic of mono through octachloro dibenzo-p-dioxins and drbenzofurans. The results of the analyses are given in Tables 28 through 31. A pair of hexachlorodibenzo-p-dioxins (HCDDs) were found in the influent water samples (see table 28). The reproducibility of the analysis of these HCDDs was not good and no reasonable ex planation can be given especially in view of the reasonable quantitative agreement of the heptachloro- and octachlorodibenzop-dioxin results. In certain instances interferences in the influent samples significantly raised the detection limits and this is noted as a ME (LXX) meaning none detected with a detection limit of XX. The sludge samples were very difficult to analyze and therefore the method detection limits are quite high for both PCDDs and PCDFs. The low level spikes for several of the lower chlorinated PCDDs were not detected above the background interferences and have not been reported. S. ANALYSIS OF OIL SAMPLE FOR PCBS One oil sample was analyzed for low pg/mL levels of PCBs. Molecular ions of the mayor chlorinated biphenyl components of all Aroclor formulations were monitored using capillary GC/MS-SIM analysis techniques. Figure 12 shows the analysis of a Si wg/mL Aroclor 12S4 standard and Figure 13 shows the analysis of the oil sample. Both standard and oil were diluted 100 times before analysis. The response at 24.5 minutes is very likely due to cl,-blphenyl isomers. This level of Cl,-biphenyl corresponds to li pg/mL, using Aroclor 1254 for calibration of the mass spectrometer response. However, the signal/noise ia too low to verify what Aroclor formulation is present in this sample. 4 HONS 022404 6. STATIC DAPHNIA MAGMA BIOASSAY A static Daphnia --qna bioassay was performed on a grab effluent sample obtained from the Saugot Waste Treatment Facility on March 2. 1962. Procedures utilised for the Daphnia bioassay were based upon procedures outlined in "Methods for Measuring the Acute Toxicity of effluents to Aquatic Organisms" (EPA-600/4-76-012). Six effluent concentrations (100%, 56%, 32%, 16%. 10%. 5.6%) and a control were set-up in duplicate. Ten first instae Daphnia map?.* (^24 has old) were placed in each replicate concentration. Well water, which was used for dilution purposes, was adjusted to simulate the quality of the Mississippi River near Sauget. 1L. total hardness = 230; pH s 610). The results of the Sauget bioassay were as follows: Effluent concentration 100 S6 32 18 10 S. 6 Control Percent mortality 24 Hours 1 46 Houri 100 100 100 100 50 90 0 65 0 3C 0 3S 00 Statistical analysis of the Sauget test data by the Binomial. Moving Average, and Protit Test Methods resulted in 48-hour C*0 values (95% confidence limits) of 14% (0. 32), 14% (9, 16). and 11% (6. 14). respectively. Test concentration physical characteristics during the March 17-19. 1962 bioassay are presented below: Physical parameter Dissolved oxygen. ng/l Exposure period, hrs 0 24 46 8.3 3.7 3.5 8.1 5.6 4.8 7.8 6.7 7.6 7.4 7.3 7.7 Effluent concentration \ 100 56 32 18 10 5.6 Control (continued) S HONS 022^05 Phvsical parameter PH Conductivity, umbo* Ttir.pf rsture *C Alkalinity . 9'L CaCOj Hardness. ee/L s CaC03 looter* aeried. hri 0 24 40 0.3 7.0 7.6 0.1 0.1 7.0 -- *---- 01 02 01 0.0 0.0 7.9 7.200 4 69C - 1 ICO 400 7. ISO 4.6S0 - 11 SO 600 7.200 4.600 - 1.050 700 22 22 22 22 22 22 -- -22 22 22 21 22 22 no 3'2 - 224 196 >500 >500 - - 274 230 6/fluent coocenj \ 100 $6 32 10 10 56 Control 100 St 32 10 1C 56 Control 100 56 32 18 10 S6 Control 100 56 32 10 10 56 Control 100 56 32 10 10 5.6 Control 7. EF TOXICITY TESTINC OF SLUDGE The sludge saaple was extracted per the U.S. EFA RCRA procedure as shown in Figure 14. The resulting leachate was then analysed in accordance with approval EFA analytical procedures (3, 4 and S). Results of the aetals analyses are shown in Table 32 with the applicable quality control data. Table 33 shows the herbicides and pesticides concentration found in the leachate. While not a 6 HONS 022406 part of th RCRA requirements, tha results for requested analyala of the leachate for cyanide and phenol concentrations are shown in Table 34 with the applicable .quality control data. 6. ADDITIONAL ANALYSES OF SLUDCE SAMPLE Additional analyaes requested for the aludqe sample include pH. total cyanide and its total metal content. To obtain the pH a 10 q sample of the aludqe was mired with 20 mL of distilled water and slurried. The pH of this slurry was measured to be 11.07. The total cyanide content of the aludqe was determined to be <1.3 uq g (dry weight) using an EPA approved method (4). The total metal content was determined by atomic absorption (AA) spectroscopy ar.d ar Inductivity Coupled Plasma (1CP) excitation techr.Ague. The methods used are described in Reference 4. Results of these a:.al'.ses are snown in Table 35. 9 ANALYSES FOR PRIORITY AND NON-PRIORITY METAL POLLUTANTS IN WATER In addition to the organics the EPA-designated priority pollutants include 13 metals whici. are to analyzed for under the protocol |1). Four metals (arsenic, mercury, selenium and thallium) are analyzed by AA spectroscopy. All others are determined by ICP excitation tec!::;.gue. Results are shown in Table 36 with the applicable q.ility control data shown in Table 37. Table 36 lists the least observable quanties (LOS) for s>etals by ICP analytes. 10. ANALYSES FOR TOTAL CYANIDE AND TOTAL PHENOL IN WATER SAMPLES Total cyanide in the water samples was determined according to the conventional wet chemistry technique described in Reference 3. Independent standards were included with the water samples for quality assurance. Ir. addition to specific phenolic compounds and phenol measured by CC/MS. total phenol in the water samples were also measured by typical wet chemistry techniques |3,4J. Independent phenol standards were alto analyzed for quality assurance. The results for these analyses were shown in Table 39 with the applicable quality control data. 11. NON-PRIORITY POLLUTANT COMPOUNDS A number of pollutants as designated by the NPDES Consolidated Per mits (3) as Croup A and B pollutants wars analysed for. Tbs com pound was analyzed for in accordance with approved EPA methods (41. The results for these analyses era shown in Table 40. 7 M0NS 022407 12. MEFSUMCES 1. Draft Final Report: Stapling and Analysis Procedures for Screening of Industrial Effluents for(Priority Pollutants, u.s. Environaental Protection Agency, Cincinnati. Ohio, April 1977. 145 pp. 2. EfA Guidelines Establishing Test Procedures for the Analysis of Pollutants, Proposed Regulation, Federal Register. Monday. December 3. 1979. 3. U.S. Federal Register, Book 3, Vol. 45. No. 98. Monday. May 1. 1980. 4. Stands: d Methods for Exaaiination of Water and Wastewater. Fourteenth Edition. American Public Health Association. Was!.:r-9ton. D.C., 1976. 1193 pp. 5. Manual of Methods for Chemical Analysis of Water and Wastes. ErA-62S/6-76-003a (PB 259 973). U.S. Environmental Protec tion Agency, Cincinnati, Ohio. 319 pp. a HONS 022408 ISS'S*. * f* M IU IIM I - - - - - k ........ .......... * - * -- ----- - |,M 4.19 9.29 12.39 19.49 29.99 24.99 29.29 32.99 I. .trait.. unmet (llli IMT II IHJCCICt tit ttilSi.S HIM I, Ittt I.IMI MKH (Ml MIS. (rot t I.IS. Figure 1. Capillary GC/FID chioaatoqcaa of surrogate compound spikeing standard added to each sasple before extraction. HONS 022409 lu ji ? Iini|-I4M > I.M T li imilti smnci i#si-i''H injcctci it i7tii .*3 0* mm 9, test N(h4i IMMK VMI VRISS Free* |f|K Pigurt 2. Capillary CC/FID chronatogran of the base/neutral extact of the acthod blank (Burdick and Jackson Water, distilled in glass). MOHS 022410  4||.H I AM FIITU9 C .* w V -*#c# 4 * rigvn 3. Capillary CC/F1D chroaatofraa of the acid extract of tbe netbod blank (Bardick and Jackson Water, distilled in glass)- MONS 022bll M V U T U K a .S f *|V*H9N4 IC A lrf4 O .N I Fiqure 4. Capillary GC/FID chroeatoqran of the baee/neutral extract of influent aanple froe Sauget, 1L Treateent Plant, diluted ten tinea before analyaia. HONS 022412 I r ' MfUilsUO rigora S. Capillary GC/F1D chronatogran of tha acid aatract of th infloont saapla froa Saugat. 1L Traataant Plant, dilutad tan tinaa bafora analysis. i HONS 022413  t l4 r. < fH P lU O K *#**. ICM4. I2IM, MM. t T la Flour* 6. Capillary GC/F1D chroaetogran of the base/neutral extract of the effluent saaple froa Sauget. 1L Treatment riant, diluted ten tines before analysis. HONS 022414 R P LfTU K . * < <C*1 Figure 7. Capillary CC/FID chroaatograa of the acid extract of the effluent eauple Iron Sauget, 1L Treataent Plant, diluted ten tinea before analysis. HONS 022415 ! l S .m 4.i* i.n ir.se >** II In nlnutM lMM.Ii I0S4->'NI(II. INJCCTCS II MlI4i$l ON MW 1. I M2 n.tM, MHOS r..i NISO Prntl Milt rioure (. Capillary CC/FID chioaatoqrw of the baie/neutral extract of a duplicate effluent sauple frow Sauqet, IL Treatment Plant, diluted ten times before analysis. HONS 022416 M .M I - (C M *'9 * 4 uv-<n4c <Ut*llTU0C i . 2 l )4IM. I.H RT In ntnuUi f* 1.21 . I*.5# RlCl 1054-0I Oil INJCCH1 at I tl9tSI ON MR 10, 1902 imi iiio PrMi irio Figure 9 Capillary CC/FID chronatogran of the acid extract of a duplicate effluent saaple free Sauget. 1L Treatnent Plant, diluted ten tinea before analyais. HONS 022417 . Figure 10 Capillary OC/FID chronatograe of the extract of a 1.07 g eediaeat iMple froP Saugat. IL Treatpent Flant. dilated tan tinea before analysia. W.49 HONS 022418 M FlITVM V .2 t4 u V *fe c e *4 l C *l*' # * 4*.eo I I . 4<t**t. IMM I2M 41 H PI In timiUi - ----------------- 1----------------- * *.%* .ee n.w **.<* **.* 2r.ee samiCt sc3t52ipvr hoick* t inMtie ew *** i*. iw N*Ko4i **l 1*144 Pro<: t*!44 Figure 11. Capillary GC/FID chroeatograe of the extract of a 1.31 9 duplicate tediaent sanple fro* Sau9t. 11 Treatment Plant, diluted ten tines before analysis. H.m 1 HONS 022419 * $pcct*uw ois^i>v/CDir s* 1 Ut S9 UC^m. 4H0CL09 1SS4 (Dlt HIM) 3s23s*a 9m SI4)-3NII) 9TLI13 014939 014939 1^ 1. "* 881 row 14939 1ST SC/991 449 * .99 V* 1.99 CVB M _____________________ 199.1 .... ...........,----^ TI __________ &--------------- t!i--------------- ik---------- ___ M Figure 12. Analytic of 59 i>q/mL Aroclor 1254 ituxUrd, using (GCI'/HS-SIH analytic techniques. HONS 022420  SPCCTPiSt DlSPtPV^CDIT t I Ui ICIWWICH on. <OIL 1UN) 3/22^92 >nN **<4>-3**t*> Tl* 014*34 014*34 row 14*34 1ST SCsPQl 43$ X* .$ V* 1 .* I--aA _ M* - -~L Figure 13. Analysis of an oil sanple, using (GCI'/MS-SIH analysis techniques. HONS 022421 (inn U. Extraction procedure flowchart. 22 HONS 022422 TABLE 1. ANOUirT OT CNBOHATOGBATBABU OOMNUMDS DETECTED IN INK BASE/NEUTBAL EXTBACT or TNE IMrUIENT BANTU. DILUTED TEN TIIKS BEFOBE ANALYSIS T BM Wt\. MM 3.44 *TU W 404.14* 3.4* W 137.072 4.07 ?.<w 234) VO 912.315 31*^* 00 5l. !'* 5.74 131334 OV 1025.07 <.i* w 3:4.331 w i3*3.:. 4..*' 7.:.b 7.4.' 4.'- t.ti ^ :v 4.7< | OV 44*.404 i;rj vt 55. 1027 00 14.415 2**1 Ov 37.V* ITj VO .Jli 7133 Ov %7.i7i i.4; 0.54 4;.o w 55.414 *;7 w 131.053 v.TT 7<4 w 102 5.54 0.7: USoi W *.2: 7.'7 302 7;* W 4047.* U*OZ V 504.074 . 12740 vv 177.:*; ' .i* 1215 VO 14.037 r::i4 ov 44<.oo? I. .. i: lo.tr 371.7 W 517.4M I7I72-4 w 2307.54 10.4* 2I0532' W 2724.93 10.5; 207(7 w 3)7.905 1C.41 10.44 217444 vv 3051.13 30144 W 200.362 10.71 4>*4 W 0-l.*7 II. 01 11.14 52*3 W 74.55** 1401 W 203.132 11.34 *790 W 00.495 11.4? * OV 7.7IC* 11.40 15155 W 210.472 11.04 1*>:;4 W 344.451 11.73 13.07 IV-2 W 20.095 13445 W 107.447 12.14 12.27 12.34 2310 W 32.331 io4l W IS.030 )5*4 W 21.470 12.44 13.54 12.47 21354 w 277.273 47f W *4.7*0 107* W 24.125 12.74 25)40 W 94*.7*2 237.504. 0*N04*05 CL2-K*ZCNC*I> 23 HONS 022A23 TABLE X (continued) ss*m :.? 12.0* 12.94 IS. *i;-.i: I : . IT li.rs l*.3f li.4 i:.r li. 7* iMt *. vv .i: >t : i*.:.' 14.44 I 4. 4 14.*. t*.t* u. rt |4.*r i. it .< IT. C' it. i it.:-4 It-4 It.i; it.lt.5' it.**: k . i: it. 17 it.;. l .3: i<.: - U. u. 7> it.c: 17.**. I7.lv 17.| 17.24 |7.>4 17.47 |7.VI 17.71 10.41 10.71 /(. mih w n.t*3 irt9> w ii.?io hi? w n.ts? 34'.-. w 47.399 1374 w 34.0?-* 431 v W M.MI I54?i W 314.923 4*7/7 W 112. If' :?*1 w 3S.II2 i r:t* v. i*..7v. I It-' W 15.47j I li I w It.4| vv 74i.Ul 4;*7 wv lit.*37 hit;: v. it.?, it w y:.m ;?*: w 35.1:4 ?-; T4 W 74.4J ' *'. V. IS.044 :?v it 1.1<4 3.445 :m* tv 4t>.3c* it;: v. :i:.tr : -< vv as. it.: I'O v. |4.2(v ;; : i v. t>;4.11 i3*tm v. iirt.tt v. *r>.Zl*. it: V. t: : v. 7:.7ti 47. t.v.i tt:r f. 7*.fi 3: t: 4t. o* t it"it vv m.s<t < ::* vv 07.?ti 34*37 w SO.397 :<i; v. at. si* ::*! w 31.934 |0>><-4 7 w 1399.23 4 *4<> w 43.47; 2517 w 32.309 1974 w 34.094 2293 W 31.901 3010 W 4|.M2 2740 W 39.347 21 It- W 29.409 10313 vv (43.373 243 vv 3.493 0341 W 119.940 104431 W 1492.13 14022 W 222.744 >vf'24 W 9004.34 7*41 W 104.039 3703 W 30.444 >990 VV 34.009 944 W 13.390 DM 2 HONS 022424 TABLE 1 (continued) ftt 10.3* it.; i. or IV I* -. i.:s 1 *. 94 r*.i *.; If*. |M i :o. :* JO. >. JO. 44 r: :t' 2: . * * jv-.s: :*.' i IS . IT . si.s* 11. <* 11 . T : ;. i ...L. ... 1: I. !; ::.* ?.. . > .. -1 11.19 I.. IT< V. i.r. n.c :?.7i 2?.7% 2M J3.n 24.07 24.14 24.24 24.22 2.I 24.** 24.00 IS. 02 23.23 23.42 23.32 23.01 23.30 29.00 MICA I3M Iv 24.100 700 w 7J| U*> vv 47.57> n;i w 13.141 11120 W 194.734 cist w 144.0.4 Uil v 0.447 14**0 Ov 201.44* 0<4 W 11.07; II W .u<: ;? vo 9.97,, 47: ov i:.iit 4?; vo 4.27C r . s < - JO w 7?r- v. **..J4? :.. r v. :.07 4-7' VV *7. 774 ? ' 1 VV 4\.. T 7' w 1* H W 499J VV no v 31. ov. 29.J4V 41.31* 4I.447 19.i. VV N . 0l ic::: w 1*3.7l J4{ I W 94.4* m w iirj.t; 1141 W (7. r : o. (.vl ;o* w 3 i . I ... 4 ;; vo 4.C-J: 447- . i r: * v . i:: wo 4i.;-v9 - m: It.47* 4'i: >V *..;3; 4 1'-? V, OC .114 i i:: ? w 131.It: i ::w 247.474 ICW? 1 w I3C.04I ?4;j w 73.200 K>)2 vv 1*1.000 J4I VV 23.441 2c MI W 2'3.74* ?<.? w 134.491 7934 W los.o:v 4* 71 W 43.347 20* VO 4.202 494.2 *v 49.:j 4K.7I W 403.214 340| W 74.294 2103 W 30.4*0 7l*"t W MNTMUCM-OIO 12-. VO 17.237 4*J >0 4.421 1100 OV 14.407 342 30 204 OV MM W 20M 03 Oil 30 202 V3 7.940 2.033 19.019 00.493 12.047 0.344 2S MOWS 022*25 1 TABLE 1 (continued) fit . i; ;t.; a.n it. j; ;6.u :i. i it . Tt 2*.C'. ;i.t. *6 r* 27.*4 IMf 1.0. ri.: : *. i i *. i* 2- .4 v r\ .p*. 1 ' 1. . ; I . *T ? -i: \i >. : i .i 3-v. 7? jK . > jO. *Si .01 ^ : lr . v 11.*: St. ft* SI.** *:.o! :;: j;.<i U.H s:.** .; 9J.lt 33.3* 33.U H.M x.:; M.S x.tt 59.40 95.3 an* #/l 1*55 tv 93.004 ftftft vt IS.40? 5*3 tv 7.02* x: W 7.953 t*i* *V 34.440 Vt w 4v 5.3*4 7.774 j?:: w ?** V4 15V tv 137* vt 4. *; V* 91.74* 5*.7G> 3i.*: I*.132 is.t: I3.7> : 1* lv : V* 4. 2T-4 3. 7;< 2T-T tt 3. 54 * :i ft* 251 44 4.01 1 4.9*4 I' 4 t. 17. 7|t ?? vv 4.014 io;a VV 14.141 17V w 40.477 vv 50.*75 * w is;.7? i*-' V . 20.217 2c W 3. *73 11 . W S.< 11 Jt* I'.T, 1* *;' 4. Vv V. 1 *. * 1 * 2*. 4* It.f . ?*? 7*t tv II.0< 7 in'. V. ; ; .< ; ; 1 ',i- vt |7.rv; ::: vt 1: . M 5 : t- 7.* 4t 1 tt 4.405 5 Vt ;n.> >v *.0l 1. < 1 73* vt 10. so?. ic*; tv 14.402 I2'*v* tv 1*9*'. * 1459 tt 20.2*1 ;i:< tt 2. *5* sit 94 7.309 tt 79.944 so: tt 94* 94 ft* tv 2 922 4.004 IS.704 17*7 w 34.979 4*4* w 107.304 547 tt 7.000 1441 tv 22.431 : vt 7.9*0 *42 tt *U 99 4.14* 4.757 394 9* 9.595 951 Vt 4*7 9 9.4*4 0.009 444 99 0.509 1719 99 99.000 MM FY*ENf-MO o*nu-: 26 HONS 022426 TABLE 1 (continued) it m.*: :i.y. tm l TO m> *Z2 Of \++: *> Si M .?? n.j* . 1*1 *.#? 4.70 TpflC API* 0**fr7 al:<csud (t riwii miu TOTAL w'l LAW DAT* r H.1 *k|** (,, /r ;t I W*Tf i Tt. ( - > * l II Irt* TK* ( I > I > , t # Mm Mt' >>' It A* lU | * I *!. I * I l# C <><*. IrilU'.t I ,, / <. > II >>! l-t'.i ) 114*.44' I* W. *l | * . J. .* I'.. S. . - . *<,*. i ! t> # i M I . Pt'.f* lll*fIH (A#|#K| |4*ll*l* '< < Id' 111*4 t* IM Ml*' .! (< III*.* ll*gl.* 41*4 to *.' , *!*.# i * ' ' w 4# lit (M IMll*'l>bl| {<.> 4l I* . I.I.. .. *. *4.000 I ** | < * cirl.'.4t .#' C . * r . . t*- *r* C . t * : t i* ***>. ? * 4#' 111 * '-*i'*il I. l# *.. * I'. I* .< '' ; H )#<*> *nUr .*. ?. t i. <*>. ) * II. I M ' . t. t I* ***.' *#C I . . *,* I*. *!.. t. ll*llr.|* 27 MOMS 022427 EXTftACl or THE INTUJQIT MW. 01LORD RM TIMES IT 4.7? lf . I II. J.,4- K. -1 15.24 KM It. l< I*.*4 17. 1C >7. 2t 17.U 1 7.* U.If c.:* 14.45 ll.it K'.i-Z ;(*.7i : i. i7 M/l ?o7 m :.m lit! OP 15.447 7Jt N 0.0*1 Mi 00 7.34* 0)0 00 II.ISO 17*7?. Ov 105.455 V# I44.4AC 1510 01 ZO.l*', i" i o. 4^.:..' * :i v. SMlI 7. ?:*. VO 4*4.54 : o t.7*> .T 00 4.?4? t; o t.*r* 00 44i:.r4 204 00 s.757 t>' Ov os. 42V :i~3: v 34.9*4 *C 00 13.205 3< 774 0v 530. *24 4-;t vo o;.i*5 43* 00 5.7|r. 4133 Pv 03.341 3051 W 3C. 13) ?!?* VO 31.31* 00 *.34 377<. 00 90.01* 344 Of 4.013 1)41 00 14.241 :-J7 bJ S3*.551 Sc > VO 7S.4H 05* Pv 0.050 3<t3<> VO 44I.0C5 041 44 11.3*2 SIS3 00 30.015 374 *. 3.474 042 * w 114.005 21* VO 3.04* 7504 00 100.040 771 00 10.372 120*42 00 1034.03 575 00 7.047 2244 00 90.14* 104* OV 14.0*0 C42-MN7fC-(.4 28 MONS 022428 TABLE 2 r*o? r; joj i:u ;u,4 .ex i. .0*4 i.t:i 0ANt*AC<-rtr s?>* n j*. 7: 4 -:t ;ct iATi rut: Ni>i T0I*w w*/L - 10.14. TTt- AM DATA rui> *!.! 4| t l.t It l-t > 4 t I !#*.' ! ** (Ui|4i #rw , *1 (i I t>4 wMtt f m lll.ul.t. I 4 II. Cv**..**'.! ' c4 * || *w I tf . CM!.** *u>4t*l |* !*. him c4vumJ mi Kk> */t. < . Tl.v 'tt-4l4 lt cA* 4*l kill. I ! ii ji<* t*if. ?.<K *><! 34.0r0 U'-k'i I. . ' I l. (J M-rMl >#* V44 I 41*4 4*iU*' C" !* l>4i:t*'l kill.* tl. Rtlw4 4?* I.t*t;tl44 ?t . 1t.f l4'<tlt "* I <*r I t I 44lltlM (l444Mht4 4 I* M *>**M If. Ih* (.* r.1*4l < ItMll <.** } ill L C>. 14 MtllMJ % ** |M|f*Utl44 * IM MI4 H *** >* 11* (|4|1l|l C</nS IMlflll l*f ll*lMI> 4llCw44t If. 4 Utn 4<tllh. 21 HONS 022429 TAMX 3. AHOOIT OT CBBOMKICUraULl CCWMM IB DETECTED I* THE 8ASE/MEUTXAL EXTKACT OF TBE BFFUIDfT SAHFLE. DILUTED TEH TINES BEFOU ANALYSIS 1 MC* */(. MV >.4 *1 >*4 *V 1*03.M i.i w s**.*?* .oc 9**: v t.f- *?? m n.*ia t.?> I7|5 frv 2*3<..45 4.tI . r c.: 4J47 V 45.24? vi - i. ??< if :i? v. !>;.v. <. *.;; >* i* vv ;. ic; v4 i;-- 44 . M' (.1? :>4 44 ;.t;( 5*V 4v 4?. |i ir?% r w :?i.fji i; iov. w it;.4* <. ?? k :* v iv-4.:i t. u< ; w . 754 3i7ir; w 4t '*.44 r : v4 7.7ti * .? . ? !.<: 41411 4v .5< . 1?? ?!< w . ;o; *::? *.?>?. i.. i: 54:?; w 4::. *: 10.34 '."* Vv |f..4i I 34' 71 WV i0<t.47 u.:. <: w 3'i.u.i 3%~i: w?4:.:? ic. 1? '.*; w 317.*4v ;?; w 42.(77 i:.o? 1?t: w 11.1* 11.94 ;;* w *2.?03 2*1* W 44.437 U.4-S lit W* 3.477 11.3* 1445 v ;i.sn 11.43 *10 W 13. *f 11.7* SlVv W 74.400 II.tt 12.i: 20121 W 304.1*4 703 M 10.(75 12.27 t-O* v* *.* 11.34 11.44 |07| WV 14.440 21*4* WV 334.303 12.SS 11.74 243* WV 45.047 4*7C VV 1533.37 12.04 177*3 VV272.40? cl7*k*i](ne-[< 30 HONS 022430 ***U 1 (continued) i>.i> i).n . d.i: ll.H II.M .oo 14.13 14.j4 14. )7 14.5* 14.70 4.*i IS.21 It.i* 15. M is.ri *? M.M 14.:: 14.* 14.11 14-*? 7.'-' I7.I: |7.;;. 17.41 |7.t: li.i*.* u.: I*. 4.. If.4? i*.:: I*.:*.?7 K>.l 20.;* 2v.45 20.44 so.4 ai.3t. n.K 21.40 21.74 22*I* 32.37 32.4 22.00 35.04 33.14 33.35 33.32 33.44 33.42 33.44 33.04 34.13 MU M tna w n.it; tni w i.m m* w h.i ojoi w m.i*) *?o* w to.113 17*2 W |,n IMI VI }4.}0 MM| *v .}o 7002 W II*.Ml 22*04: w :*.o4 :*>: w 4ot.4<>: > V* 44.;*; 404 04 4.2^ t?i3z *v i*. 4333*0 W 4*5?. f 7 :i73:i V* 3234. 1011 tv 31.004 573 - 5.7:-. :>* w 52*: W *1.314 1414 V4 24.4/4 2*11 V* 57.64* 2015*4 tv 50*7.70 ISM w 134.JIT v* 4.c:. :*<4 44 4J.?4-. vi 4.c;V.i-, |.< 51.17: u;is. w iT7.o:-: 7: -zi v. 11:4.41 tvs w t >7. 40445: W t;|.4T 2354 V* 3'-.277 t-ci i/ 23o.:oi 2:472 W 343.3(1 Mil V* 17.*54 3030 *V 44.401 ;*4 >* 4.514 4417 tv 70.444 547 Vi 0.405 j:,.i *1 3*. 1* 3.047 314 00 4.0*0 101473 OV 3*14.53 4%.>* VO 4*. 201 424 00 12.440 *37 04 14.713 |$27 00 2*.741 210 44 3.337 13553 Ov 204.250 5054 W 00.044 I04| w 14.1*2 444 VO 4.047 5270 OV 51.741 3331 vv Sl.lOl 4453 W 00.103 522 VO 4.044 102* 00 30.000 MM 31 HONS 022431 TABLE 3 (COBtiflMd) NT w*/i ;4.ti ;t.R ii.j? Mi i u.n* I4TI 9* 75.3*4 7*i m *.*?: *5? H 14.470 70-? 04 447 44 7. 44* It?* H iri.isi i' iV 44 *OU. |41 *A4.. H lli. Si* ' k *n*. 41 *4:11 **.-,;cvc: U'* tut' 4* IT? tmm fMM-lie c**?scm>-di: 10TN. *4/1 42744.JOS MM 0474 mil 4*157 *4 T{: It.* ttkM r*l | HimUM tf*4 th C41t*'. C'.Tt: 4 **.!*. (*14*14* *t*4Ct 4* 4 l44IC w*t*t *). i m- . t I . .* lo*. *' .( *r *i.wtt. tt> *r* W(. I H 4*4 I 144* (CU<'|| 4*4 144 CUUMM C *M **t * 411 ** (kt/ll* . t- will* 4vl4Mtt If IK* 444* > *4444. , I 4 % tv* i *.4 It-* *>.... (44*k| *4444*44 14 *4w*1 V* I *4 l*l****t M4>-l< * 0tl.l 44*14*41*4 <4*4***4 I44*tll*4 * cMVttn4* *** 4*4 444*4 t* * **t*r ***! ...... *.!. C*c>. 4*lk|A* C4*4**4 *4* 444*4 I. 4>*4*c* )* . < i *'. of tOO **/L. !<. !>.! .| Il.(l4l *11 Ct>* **!** *44*4 * <o*4|*i.J* nNUM <**#. 7.W* h4 V4.000 (*! <! Oor.d 1. ( 7 ff.. (Ji ...**: t.. 4' :** I 4*4 u*1 4* 1r *C I *4 I'., ftm ntt.(-4 :* C.t4ctt4* 4r4l*<*t. f., | 4. '.tit- ft.*.**' **ltl4*T (44**MI I* 4 | >. |l. ** * l*1 *'4t4 1t4*> 5 w*/k C4* 4* I 1.1 . J l t. ti. ! 4 *4*4 4*%1 44 *H . 6.<. <:.! #4* *f |WIf *4l)lnU. 4l<*4 t. * . * ' 32 HONS 022*32 TABLE U. AMOUNTS OP CHROMATDGRAimtt OOKPOUWS OCJBfS) IN THE ACID EXTRACT OP THE tmUENT SAMPLE, DILUTED TEN TIMES BEFORE ANALYSIS IT M4 */(. T.i* *.;; t.li |f-.T7 Ii. I> u. : j. 7: it. it. ! 1! . :* 3:vn.* t^t j.m 14.. *4 0, l-I.T-44 17407 V* i31.47> S>- 4.4^ IT*: tt fM.OM rt- ooi to m *T *. C.ai vi- 4 4 u:;.4 i{*,<* vt- i4:.:.v III- to l. 4- 00 to *; o < .* S'.7 to 7 , 7* j h.; to t*CNQL-05 a2*KM2CC-D4 ;o.& :7.* 2*. 17 32.4: < t v M.4*T :4.4:1 4-:.- vi t: oo t.44 i i4i to n.r:; iT4 to 74 4 :**. vi :.<7: to i >7 00 1i.OV 17;.-. x.3I r-7* f>t. 3i.7vr- :4: 1.1 4.*.?* 74:77 to 00 7..,J UMTtftLCtK'DlO :><; > . 10: T074L 44(4 -71 TOTAL w*/L 10077.071 FftOCilOCO D*l* fU.lt ** >: MM DATA TlLO 0*142 9C*t\t NC>TC< Tk* !* r*rt t* MM'lt*! *14* (i1lii* * * Mlktl4 *Tr*<t < r> * Mtt* 1IMI4 (4M < 3). Tim -** tla* *! kiMu. Tim Ml| ** <** |M Ik* (4444Mnl i4-l> < 1< ItktMklM tl4 l4kMM (M444i ! II I44l (# (It* |M****I Illf>4i4- #! *<#*m*4I0. Otb*t MtlfltH C--v*n* *r* * ill** UM4t *0*40 r* *44*4 I* lk *** ***! ! Ulilitt. **. lid lit** C4MM44 Ml *44*4 I* *f *4*4* mUi Mi<4trUk # 140 **/l. TO* ***** IMliltl lKl4| 4ll (MlMtllMVMIIl **!4 ill **( ii4i* IImk 7,000 MO 04,000 lIUh *>***# tv C7 tM*4* CW MIMl lnOMIlllMi 4*0 AC* C44 04 4atl*<lT Min Tit* VO IMk4 429 IttfMllM Tr(Mil TO* |0**T|T *4 M, |*||* **tl*t**t cimimMI III-- t* 0* --I I* TO* !, k4lilll *1 l*v*1* **** 10*4 S */L COO 0* *4T*l**4 0 4*rt0*r dtifirittllM *4 TO* Mil MKtrl Oot* *0t*l**4 li--TO* **11** OC/MO --lltili #* iriirlTt **tlT*oT, IIM1WM4 40 O tot** 0*411*0. 39 HQNS 022433 BASI/NEUTRAL EfflMCT OT SCrtOBfl DUTUCAJt SAHT1X DIURED TO TIMES BETOftE MALTSIf m * . *4 1 I . <7 It. > 11.34 n.so ii. 5* 11.4* 11.7* ij.fi i:.ir ** a t*ii* 12*4.5; itioi v. ;**. mi 5U*4 VO 755.042 u .:c jrvtr-' :*u*. i; SKii w TN.SIS :*:4-. v; 1471* Vf ;5.7S* .i t *.i;i >1- frr 4.44, 145* t 27. It.7 iTTi- tv 257.41? ( T( W 44.445 |f>>T<s>- W |4?f.44 liit-7 V* 1^4.OS'* 3S:-44> V. 4*>4.4I tr:*' w 22.404 44103 vv 44V.57? ;;?s w >4. fir 4;?J7 W 4*7.t-44 554*7 vv 514.21? 4*::: .. t>>4.*... Mr ;; vv ;iio.*i 1 405' V. i<>. 42<- 377. I f. vv ;: ;f.r w 3: *-.4S.. v.- u.tn 1*12 vv 11.04*. 5*4* VV ilvl w 45.ST** 2w vf 5.o;i ;;t * j.3i* ov 3.4i4 4.4 w 73.:;: ii175 W 311.074 v*v v ts.ru it; w 4.301 W |.f4* 1145 W 17.|0* :3( '; w 534.354 3C14 W 44.272 105214 w IU>,7) 1710} W 2.S54 Nine ftCMOk-DS U.2-MOSCNC-54 34 HONS 022434 B tiapS B K ti ZABLE) S (egptlnM t M/li n.|7 D.rr i:.l* II.t: ?.? 13. CT 14.1? 14.24 14. J7 )*.-* 14.74 14.4: 15.21 !.17 15.3.. 15.71 IT.S if..*? U. 1: i.: It.4* t<.t i*..- 17.. . 17.5it.; 17.1. ' U.t-i li.io U.4; 11.41 l i . 71 I -.:: I'-.:- |4.*7 l-.i Ii.4! :v.4! 20. *1 21. :? 21.3! 21.20 21.2* K W 49.9BI *;! W fl.fl) w M.on 25*2 W 110.920 5**7 v *4.0*4 * W 0.441 l01 V* 20.40* 4IVot tv 415.404 r?-41 W |J5.4** :j-;w j?.;*.?* I - I - I W 4i.?'-l 3?.;; w 3i.*t>: * VO 11.775 ov 4715?* W 4*?7.05 ?:417> W 147|.{il 54; VO 7.* r?4l 00 3:.*:'' 4.5 v. t.iiT- w 137.07: W W 05.432 ;?4 w 33.03* 2771 VO 40.710 ::: * 3414.45 |.4?; w. 1:4.54: *i ; VO 4. it7 :w.: 44 4< .34. 1;;' 4V iv.li; .;*-* w *1.171 117-r. w i7i.:ii i4:i. v. nv.57 *7* W 141.474 *i;ii v. 4747.1: :-V. VO 4.24* 14.0? 44 21.335 l7w*% 4V 25-..757 w 3? 1.*45 1707 W 25.071 7i7 V4 10.445 1373 90 20. tot 4/>? o 5.**s 37 Ov 77. *45 ?43 VO 11.211 23*7 90 34.12* M 99 9.92* 3*3 90 5.229 3122*0 9V 31*3.12 3213 VO 24.414 043 >V >2.320 554 00 0.1*4 252490 32.113 214 90 3.147 1942* Ov 224.9*4 400* W 100.034 |4|* W 20.047 004 W 12.404 23.43 23.41 4409 W 09.90* 9221 W 94.021 rm 39 HONS 022*35 tabLX S (ContlOMd) is 24. r 4.*; 24.91 2:.o* :.r : -. 4* Ml* 9/v V4 97.t* kmt m .n 4'*>7l *v 4104 V4 41.79*5 244 M 4.949 j: l> 9.3)7 11*: 44 :7.n* 4w: 94 e*- 494* 9.9* 3.o:t 13 17V.*41 97| 44 14.24* 1. ;7i 44 *4.*r* 4i:--i 4* 40. . :70 44 t.4J7 ^rt 44 i57.j; 10T*w 44(4 4443T2* vfttM-OtO 0*v2X*C-Dl2 TOT**. **/L - 44T74.4*! PM<()!tt 0474 ricli AM E*4TA riLfl 44124 l T(: T>.* l-t-v* IB **'> Pr<4. I f<* ( c* /7i:> *.*: i <* Mt*-.t*o* *# **< I III. Tl. t *>< | 1 *.. I IB* Bf'lll (i *| (.(*. t W>.|t t't tBwMt *'* t* (Ba*BBAl C**<*M'4tl iii :<>** 1 *!'* ivI'imk itmiB'ii. 1* to# ... **-,>* l'- *****. <<..>*'.* IB . I B V A1 !* > *''*.*>*-41 . Cl**' 4**t*'t*<l <***b*'.J >. . *.*>* *1. |l *1* * * U, Ml I,*.', *-l>*ttl>' b*B.. ('. Bll'-* (B**B)"J MB ** *' C"0**0* *t B ** ICw wB.'l. Tl.* **' '*!.BtB *11 (BfB*4lB9> **!> * * (|.vhB Will * ,.*t* I'.JiUI |.*lw*. ?.0>>v '-J 94.000 <*"*B*vf. l.. C" !**.*' C ; 4 WMl o->.<'*f*B > * wtlCO <4- * .*i*<**j iii.* to* fWti>*4 423 I.I'BCtiB'. f*!< I. T*.* |4'tlt. *4 ***.-* !< | **tl*t*M (BABBAtBlB |B*'. t* V* >**BM * I*.* ***** **.* BIB *t ** 9*Mlt' !*> Z *'l <*' 4* wt t*.l-.} 1*. w't*.*r t'-t*'* Bt*t 1*0 * m MM t**C I ' I 4Bt* BbUlMt I'BB to* (*l<Ul QC/fU BMl'IIB 4** MIB'lt' Bllwt|l>tB' lltOMtH I* * t%t*r *<tl*'-. 3* HONS 02243* mu *. unm or chrchatocxa'hablx comfoukk detected IN IBB ACID EXTRACT or THE EFFLUETC DUPLICATE SAMPLE. DILUTED TEN TIMS BEFORE ANALYSIS >1 3.*' <M */t 341 b> . as* )7i; 14 90.790 14447 |V 144.060 HWl`B 1 ... 7- i*. > .:u.t v.K .< ' K:t..;.i i?.<: 17.<" i:.: i 27.7 11. ! 34.41 4lM* M 441.302 :i|4.>7 1 3107.33 flf* >V 13.041 .-I vl 7t.%ti ti i.' uti.ri |.>7f*l VI 143.437 *77 14 13.04. 1*7, U 35.174 u< ii t.n: 5<I2 11 73.30 K7> 11 11.411 91333 IV 704.*11 7*. I- Vl 104.7<r 42-.11 11 37?.34o t:..- 11 43 11 47 11 7. IIS 1Z.4SV l|.41c 7144 11 Bb.443 #3-rr ii is**.ss (14 11 10.114 11 ;i.:io ;ii ii 34.?**- 370 11 4.1*4, 74117 11 30 11 442 11 4.344 4.303 CL2*KNtM'ft( 14MlOIKCtt-01O 301 11 4.434 1014^ M4L- 413134 TOt41. w/L 0034.311 OKOCCMCl (<474 Blk(l !> KM* OKI* MLll 04143 MJT|1 H* *** rr| U MNFtt** IM 62/010 IMllltl # 4 blBM4s ntPSIt *1 SA StlStt Ml*' MS*I Ip* < 2* 74* rtUMIM 114* BRItl 4*4 *!**(* IN r*4 Mils 4* IRltOtUl 4M4 SM IM CIBMRIRl (SHMlfll I*** 4'V (lUpIStl* * MIM IStMllt ltlMirn< I* IN P*M I* ASM*- * 1, lllcSIM 14* mARMfk CIRPIMA* B4B*MB* IB l*Sl V* IA mlt'Nl IMs<*M*tB. BIImp 4stPFSl4 iiipipMi 14**1i* i*4 4*4 IRlbIM M*MR* nM(B MS 40040 I* IM Mlr MRPlt M*MS .UBItl*A MMA. K%C4 IPIkllf tlSPIl MB *44*4 I* PrS4( MS** (MilPAirSIISA * IW Bb. * * ** TM *M *Ml*ll imIMbs I1 (hPMsIsBPSPMklp ti--Runts Mil Ml# IMll*l MImSR 7.000 M0 14.000 IstKB f#PPBPM4l C7 IMBB C34 pml MOBtVMBBl 4*4 0>l(k 4 M p|p(| SIM SM (OK HIM 4S3 IllPMIISB BpbImsI. Tlo l4*Bllfi #7 >* l#llf B*I1IbaS OSPPASSll B4*m s 1* oootoKt to tlo oIom SMlnls ot 1#sH bpbbIbi IMB 9 M/L UR b* MttlMO 1* lP|M IRIHHIUIIM S* IM MSB BMttfKl MU IStSIRSl ook tlo **bIII#py 0C/IO bmItbii #or rpibtIIt bbIMbbUi oibcbb*o to 0 totoo IMI1B*. 37 HONS 022*37 TABLE 7 ambit or cboutocutmu eoroBM wwap m THE METHYLOfC CBL08I08 iHSMCS 08 TK HDtMVT ' SAMPLE* DILUTED TDI T1KS BEfOBS ANALYSIS M 5.4* . .* .. *. : .<.. .1 . ... : . ' .; *. ' .4 . t"! .* .T :.-.44 ..: . -- 1.4 ,1.'; ,1.-7 ;.;i , ..4l.M 12.(-4 2.74 i,,...; IA.V >2. i* *M MM ;no v M.oao :* v* i3.IT) * n.4*o *: n .jr. :*'* n> .w&; t:r h *.*k 5*44 ftv 4., 7 w ;* w. il.IV. 04.047 *0.7C4 <- i'.4* it........ 0*.*-; !' A 4* . 'M : a*:' ov no.MMd-i-r -** , . i>i.; w ili l W Si*. 3l V. VO 7.4i*7 " 141 (*rf | >. t4i : :s' w *<.. 74: 4KSI W 0*1.21" *iw 97^.07; w 211.74; T vt 5*. 30? cl.-7cn;em*-i / 34.31* ;*.> 4i. *. 54.7<4. ;r v. 1; .v.47 r :-.7v* ' .. 111.4; 7 tin w or.*;.: 4*:; w t'.siv :: 1 t ?.t<r :: ov ;.;4 irvr w 21.447 1175 V* 17.004 .V 44 3.441 ;i? tv lt> V7> 333 >4 s.oto 3.4*4 4.737 St? V 0.319 :v ov 30.71: 4*-: VO 7.074 Ti: Ov 7.300 74.K W in.03* 38 HONS 022438 TAIU 7 (ecatiMD D.i) XK 14.1; 14.*; 14. 7* 14.>1 19.11 11.24 19.40 I*. *4 I<I. u 17.20 17.3. 17.*; l*.*v l.4c I 7. *, I*. I' i*.;: I 7. T'I .( I. i I . ! I .. 70.' 11.14 31.11 .1.4.4 11. v 31.4* it. 11 23.42 as.si 11.44 32.74 12.14 22.43 23.47 21.11 23.33 29.49 23.'.' il,v im H.4 9034 Of 91.410 974 *V 13.000 1441 w 34.044 *3 W 103.770 4440 W 440 0 >004 09 24W 00 313 0V l*-7 V4 44.113 4.944 14.304 33.3M 4.404 1.303 421 44 314 04 IV. | 4.030 7. j>4 3.0.1 411 44 2`X V9 737 04 0444 Ov I7;| y 447 00 3.441 2.044 lv.41* 132.974 34.470 4.920 1* VO ?--7 00 ; r oo 3.344 3.477 3. <*4 VO M7 >0 i~ss- io 00 l.444 71.342 :*.;ri 4.9M IK* 00 410 00 4.4I.C 3.371 M5 OV lo. to; I'ti vo 04 S.0S9 412 0* 2?; v. 4.704 3.93* 023 W 13.133 5041 W 412 VO "*i OV 217| W 7}.74. 1.992 43.194 32.302 222 VW 304 00 4*3 00 >42.1 M 4T1 00 3.143 4.390 >.315 2v.20O I.VM 494 00 34*0 00 10*0 ^ 7.4*4 49.490 19.074 1447 WW I Owl W 2444 VW 1007 VW 1910 Ml 450 OV 313* WW IV34 Ml 009 WW 23.431 27.097 41.907 27. IB 14.349 37.013 73.000 27.913 14.19B 1300 Ml 10.0*4 (US WV 24.999 044 WV ti.3 st HONS 02**3' XASU 7 (GSiIWMl rz 30.00 ft* n> .u i2t',..4*77 25.*.. 2t.: ;<. r, ;*.3i *.. . r. t : .* . .. *.74 >....4 1 *...7; . ..Vi :1.47 i Mum **, ai* w . 400 40 ate teat w im v xt as WN >515 9.179 33.205 14.517 17.470 10.774 N 2Or- ** jm a* r* h 4i r 5.434 a. 54a 13. 7w 4.204 i+ aw 23.451 w 1340 V* 14.341 7J44 Bt 3).34* 4i.t 54 a* 2>77 0v H: w 11.f%i j.r- :.35 J,.72* JKv wv ;.** 4<. v4 24> 4w 34. Ml Tv.- v. r. 't: l'l T s. 114.gt 7*; w 11.27; ',74 4V I 1*7 4V i;t7 4w 4.Tt4 14.3' 7 17.444 4-- vi ;j4 :7v. 4* i-.:?4 I *V 17.045 744 WV 10.411 7*> V5 n.344 45 lo.**'. 44 27v*.74 107* 44 15.350 14*4 40 34.447 7t 45 i).0* 4.^ 45 5*.t;7 241 H 4.0m4 mu 44 30.214 PV>.C*-blo mvwc^ii T014w M(* * <4<0*3 ;r- 5414 14.1s 1*10:1 TOT*. M/t 0540.514 MM 041* 7011 MI4) 00711 74# 44w r##tet 14 MtMnlH f*M Ik* uillrt OC/710 4441-414 *4 4 MtliUte (hlMtte *4 4 44041*. 7*0 **#*ti#* Ilk* **||| tv 010*144. 14# 4**4 (tklll 4*4 10144*414* (44014 4o0 14# (400(4441 (40(401*411404 144/4* 4*4 C4Uw>4l*4 4* 44104 4*10401I( 41*004004. 14 10# *44* 14 04004. ** ( 44440104 104 *040*40 (4004400 *4404*44 14 40*4* t* 14* 14004*4. 4014*4(404-010. 014*0 0**1#*4l40 (4004*004 l0*Ottl*0 - k*o*4( 401(104 voO**../( 0k|(h 404 40040 to 1*4 440* 1* 4**4* 1*4t1* 04040. 10(4 4014100 (4000400 004 00040 1* OO*04(* 44010*01 (40(401*41140 4# 300 40/0. Tfa* 40**4 40*1*414 10*1*0*4 *11 (0**041*4* 4*4401-- * >*4 .1. ** kt.H fiO.1 o*0 04.000 t*k|k k**o*o*o4. 40 HONS 0224(0 TABLE 7 (con II C7 04 MfiUl >xr>W>--> *M Mtii * l *t<4 VIIM MlkUa * M MtrMttM tM # MD'WlMlI* **>UUM >>M < 4* ftMAt | tM 4lull mu 9 > !** ##*# v* l(. CC/N) * lb* Ml* *! 4*U '* *l It* I*. | l|tl' * t lK. 41 HONS 022*4*1 TAIL* ANOUK OP CSROflAXOGftAFHABLE COHFOUIOS DClfcLIED IK IS NenmjjiE chloride extract of the sediment* duplicate SV^LE. DILUTED TEH TINES BEFORE ANALYSIS s.:3.47 t o 4.u * .. ;. i. * *.*' 5.W '. I* ".*> * 7' : -'" iv.u i< !.** ".t: 10. 'i !'.?> .*' M . 1t : * 11.4; 11. ^i II-7 1.W 13. II u.:i I2.4t i..r >: li.v; 13.01 13.10 " I' l * 13.11 13.IT stsi v ti v nos m tv mi v 1453 so 2*4.4 ss 47 v> tv 27.474 14.474 I4.ll) 75.154 34.V7*. 14.5*. 30. |t(i ?. 14 wv wv 24.SPT- 231* wv 74. 34) >?n vv 5*27 v 75.707 K7iS IV 114.*t? K<4?*. |V is:.?;./. a. to; (4: vt . 75; pv 132. 5T: 5 w 44. ( V "* w *94.4*.7 *c;-s<ww3*2. 0V5 v. 2I0.417 i.lV4 *. i. i ?M',pv 34.234 21.; w 4k.< * W 24. ?V> * . *'/'> . !',.WV *" vt 15.113 I*. /<* . i * St 4. 1U P*ii sv I 13. *44 yjc'i w 95.04; 54-1 VS *4.?54 T-* St 7.40* 3. 1 * IMO sv 2?.4r7 it> wv 10.910 jo* OS : PS i w* 2. T-44 3.17 * 4.774 24S5 pv 34.1*4 7-3 w 10.122 75| w 9.53 7f<-4 vv| 01.713 I v VP 7.77. 4*57 Sv 43. 30'. 51 VS 95.SSS P4X-D5 Cl.7-4N7ENC-04 42 HONS 022442 TABLE (continued) HI I4.II .*r I4.* 14.4? 14.7* 14.t; i*.. n* ;.: ? i ". - * 19.41 I*. 14 u.;o 1. . M 74 U.l i:. <' u.. i 7. :o : 7.; i it.:: i r. 4,: 1 V*1 it.;*. 1*.*? . i.. ; i; ; .. >. > ;.t: !*.* i^.f-T . ( . It .(. 34 aw. u 20. 4v ;o. v. :o.Ti iu.K* i 21. K 21.21 21.Sa21.45 21. VI 21.** 22.12 22.42 22. SS 22.49 22.27 22.07 22.* 3l.M *2.21 22.22 MCA 1202 IV |1W 209 VO 2.422 m ao 3.902 TOT* *V 34.771 10447 W 193.400 4094 W 2*4 VO 995 00 I24-* 00 2223 N 299 OV oi.m 3.022 7.0*1 19.*54 41.193 9.29* il* VO 317 00 M 2.003 4.100 :.57 ;i, tv 5.474 2 VO 5.440 9!* 00 4.09* 770 >0 9.02* 1*5 00 5.394 ox vo 4-391 3* 1 00 4.**4 OV 11.231 in., t w 175.901 2X; VV 94) 00 31F 00 15.4*4 4.*41 4.040 1' 73 00 97 79 Ov l*.l 00 13.747 73. 74<> :4.0.3m *;> oo vo 7T 00 9.430 3.*4I 4.047 1*349 07 r: i w 49.: vo 17.251 5. or.: 7*9 ov 20'. VO tr>?3 Ov 10.10* 3.4*9 13.004 9249 W 40.91 T3' W *.397 Sl.4 w 49.*40 r?-; * w : jo vo 5l OV 32.059 4.221 2.951 099 VO 2C2 00 1940 0* 10.*70 2.004 1*.470 443 M si4 m 2424 30 1113 OV 17*4 V* 2024 OV 330* W 1*47 W 10*4 W 9.496 4.9*9 44.920 14.217 22.700 29.092 39.440 24.047 19.04* 27*1 OV 9347 W 2030 W 39.440 40.999 24.031 43 Oil**3 HO**5 r; n.ii * .14 >.73 30.34* 30.41 30.73 3u.7> 3i.:: 31.75 31.47 33.1* 33.34 U.6, 31.77 TABLE 8 (continaad) n: w 1)74 VO t*33 N 73 W 7433 vy ^44 VV U7 V Ml M 740 tv (to w ic*ft w d: v* ir m M/t 3.5*4 w.s: 8.41) 14.19* 33.094 33.4*4 7.14* 3.335 I4.03S i4. *: i.Ttn Mff I4NT4W4CPC-OIO :-r- *4 4.*34 Ic- k4 3.43* Sul W 4.9*4 337 V* 4.303 444 M 3.*3C |440 W 10.474 717 V? *. IV? ::i * 4.337 itit ftv j: .3?7 : ? w 33.111 l >44 W 17.477 3S44 9v 31.744 ft* i.Vf it* *4 ?t: vft 7.374 ft* 3.;i4 *. 4t.i44 .v ;>47 w 7i 47- .ft ft.4*7 314 ftft 4.3 3644 V 3: . 7v:. 3f>4; W 34.044 10717 V.- 107.70* II4: A* I4.9V4 ::o ft* 3.79 is* ft- 40* yy 4.313 :.* 3.003 ir 8 3.443 140* ft. J*.tu 970CK-0I0 4141 ftft S3.174 JV ftft 3.305 3*4 00 3.43* 947 10 7.014 43 PV S.304 003 VO IO.797 31407* OV 3770.03 148 VO 30.735 Ui 00 7.777 1774 9V 35.310 15*3 Oft 17.95) 013* VO tOO.*00 3*0 BO 3.333 MO NS 022444 TABLE t (continued) j:.u k.u *. on n o.oio 3ox> oo J N 0.010 lom M* 7*0l IMtlUD 0*1 riu> U1M wot rw.iTi MU 8010 MIS' 01(4 NTVTti IN# (* ffMfl |( to* I. .. ,r|;. V* *(( tH (M(f IN (aUKl ( M4IMM Ha f (>>( #> Iim mmU or* OlMwVo*. (M ' wr.il* |>IM(1.' . *.< I i '. IN aaMM (*t(lMr(tll !'> r (|U*UU( ,i t. (t llri < >**>< t(H(4i(l- I* IN (t I* M*(> I>I > . -II-.. M If****** II MiKl t* ( I . > 4w'r**t* I|||M (imii'iIi *** M4( I* ( Mft.li 4) !-'.. ((! 1'iltal <.>..< mi 4(4 la *r MCia.i-1 (*** t < kCO tl. (|.a *(< >114 ll*v**4 Oil (kfMl4*'4Nl<* (M. v 4> ill btM4- 7.000 4*4 04.000 t ... I. (HPiia.Nl (7 f `,4 AMMl t.K <.*M-wli* * 1*4 Vr. (a * l.* l.i 4ll*4 O'llMil 41 4* *.l*<tl*.* Tl. a -l t 1.4 **( I..' |1> |.. < |. , > wit !.. !--. r.*l.4ia ( 1 * I * *!' III'. " <>. I. . Ill i.4 l N' 1'*' |M.*'I41|.'' ** IN Mil |aiil'4i 4al| '*l.*i>* > i v. M>. \ 4| 11 > .*< IT > 4 1 ' 411 4 v ' Il< .Itvt4'<tl' 111 .>< . II. l I 111'. 4S HONS 022^*5 TAEL 9. TOTAL CONCENTRATIONS OF EXTRACTABLE COMPOUNDS PRESENT IN WATER AND SEDIMENT EXTRACTS. ANALYZED USING THREE DIFFERENT METHODS Extract identification Influent base/neutal extract Influent acid extract Effluent base/neutal extract Effluent acid extract Effluent (duplicate) base/neutal extract Effluent (duplicate) acid extract Sediment extract Sediment (duplicate) extract Total concentrations (p<j/L for water sampler and ,9/9 for sediment samples) CC/FID CC/MS-Total CC/HS-PP 54.000 20,000 6.200 10,000 5,500 12,000 63,000 34,000 3,700 10,000 6,800 11,200 65,000 36,000 3.900 10,000 6,000 10,600 8,500 9,700 7,810 8, S00 8,900 7.360 HONS 022++* TAILS XO. PKIOftlTV rOLLUTAITT SCUEMIMC LSVXU CC/MS tinw<n tml. M/l MVUBHbp 1ml. wan. ACldS: {CklMIpiMMl MitripkiMl rMiwi 2.4*0ichlerephenel 2.4. t-Trichlerephenel 4.i-Dlnitr**fcrMl 2,4-Otnitrephenol D*CMor*a*crMl Pentechlorophenol 4-NllrOphMOl Chloronethene OichlorediUonrene thane IroMMthaw Vinyl chloride Chleroethane Methylene chloride I r i chlorof loorM thone 1.1'Dichloroclhylene 1 l'DiehlorooYhone Trent* 1.2-dicMoroe thy lent Chloroform 1.2-Dichloroethono 1.1.l*Trichloroethono Carbon tetrachloride BronedlcMarenothono u(chleranethyl) ether 1.2-Oichleropropene Irene* 1.3*dichlerorenene Trichloroethylene bLbrnoochlocenotheM Ciz*1.3-dichloropropene l.l.2>Trichloroetheno benzene 2-Chlereetbyl vinyl ether rmlon TetrechXoroethylene 1.1.2.2-Tetreehlornethene Toluene Chi orMontane Blrt lmi.ct+1,. Icnlito Acrylonitrile 2$ 2$ 25 25 2S 25 250 250 25 2S 25 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 200 100 tMszataisk: 1.1'Dlcfclerebemene 1.4-Dlchlerebenzeno Manochlereethane 1.2-Olchlorehentene Bie(2~chlerleprepyl) ether Nenechlorebutediene 1.2.4-Trlchlorohiiuene Nephthelene lie<2*chloroethyl) ether Keuchlorocyclopentediene Nitrobenzene lie(2~chleroetho*y) nethene 2*Chloronephtheltne Acenaphthylene Acenephthene Iaephorene Fluorene 2.t*0inltroteluene 1.2*Diphenylhydrezine 2,4-Dinitrotoluene N-nitrosodiphenylenine Heeechlorobeiuene 4`Bronophenyl phenyl ether Phenenthrene/enthreccne 0Inethyl phtbelete Diethyl phtholete riuorenthene Pyrene Di-a-butyl phtholete Benzidine Butyl benzyl phtholete Chrysene Bie{2~ethylhexyl) phtholete Benz(e)anthrecene Bente(b)fluerenthene enze(k)Fluoronthen# Benzo(e)pyrene lndmn<1.2.3*cd)pyrene Pibenzo(e.h)eathrecene Benzn<f.h. i)perylene iMHtrueedimthylmine M-nitroeodi-n-prepyloulno 4~Chlorophenyl phenyl ether 1.1*-Bichlnrebenzidlne Di-a-actyl pktbltu it 10 10 u 10 to 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 25 25 2S 10 10 10 10 10 47 HONS 022447 nui 11. aamamt uvsu rat rmiciea/vo1* EXTRACTABLE PRIORITY POLLUTANTS Aldrin a-BDC R-BHC Y*BHC (lindini) 6-BHC Chlordene 4.4*-DOT 4.4*-DDE 4.4'-ODD Dieldnn Endotulfan I Endoaulfin II Endosulfin aulfatc Endrin Aroclor 1248 Aroclor 1260 Aroclor 1016 Toxaphene Hcthoxychlor KSS6 'W 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 10 1 TABLE 12. ANALYTICAL RESULTS TOR VOLATILE ORGANIC PRIORITY POLLUTANTS IN WATER SAMPLES. vg/L (ppb) Analyte Methylene chloride 1 .l-trana-dlchloroethrlene 1.1-oichlordethane Chlareforn Bicblorobreaoaathane 1.1,1-Triehloroethane Carbon tetrachloride Trichloroethylene lenxene ChlorodlbroaMaethane Tetrachloroethylene Toluene Ithylbeaaem ehlorobanaane (link HD* <*10Kb ND ND ND ND ND <10 ND <10 <10 <10 <10 Swale id 9:15 a.a. 10:21 a.a. 20 <10 <10 090 30 10 <10 <10 5,350 <10 <10 530 430 2,540 BO <10 <10 440 20 20 ND <10 6.020 <10 <10 710 400 2.660 11:15 a.a. 150 <10 <10 430 20 20 ND <10 5.900 <10 <10 1,000 300 2,560 - ea^owd not, detected. k`<` - caapeond iNiwt, bat veebelcw icreening 1ml. 48 HONS 022448 TABU 13. ANALYTICAL RESULTS FOR EXTRACTABLE ORGANIC FR10R1TY POLLUTANTS IN WATER SAMPLES. pg/L (ppb) An*Ivte Sample ID Effluent Blank Influent Effluent duplicate Bese 'neutral 1.3-Dichlorobenxer.e 1.4-DichIorobenzene 1.2-Dichlorobenzene Kapthtler.e Diethyl phthalate Di-n-butyl phthalate Butylbenryl phthalate Eisl2-ethylhexyl) phthalate Di-n-octvl phthalate Phenanthrene Anthracene fluoranthene fyrene HD* HD HD ND <10 <10 HD <10 HD <10 <10 <10 <10 60 720 700 sao HD 10 2.990 80 70 ND HD HD HD 70 970 1,290 3S0 <10 <10 1,040 <10 HD <10 <10 HD HD 70 1,000 1.350 380 <10 <10 1.070 <10 ND <10 <10 ND HD Acid 2-Chlorophenol 2-Nitropnncl Phenol 2.4-Dichlorophenol 2,4,6-7richlorophenol pnt*chloropheno1 4-Nitrophenol HD 160 HD 2.790 <25 175 HD 390 HD 960 HD 30 HD 4,380 290 4.760 130 1,200 1.250 <25 3.580 260 4.470 110 1.090 1.110 <25 3.540 *ND - compound not detected. b"<" - compound observed, but wes below screening level. 49 HONS 022449 7ABU 14. ANALYTICAL RESULTS TON PTBACTABU ORGANIC VU0N1TY POLLUTANTS IN SDIMR SANKSS. U9/9 (ppa) Analyte 1.3-Dichlorobenxen* 1,4-Dichlorobenxene 1.2-Dichlorob*nzcn Napthalcn* Di-n-butyl phtlialat* Butylbenzyl phthalate Di-n-cctyl phthalate SaaDla ID Sludoa Sludo* duDHeat* 20 240 330 70 30 7,100 20 10 100 240 60 20 6.020 30 TABLE 15. QUALITY CONTROL DATA FOR ORGANIC PRIORITY POLLUTANT ANALYSIS OF WATER SAMPLES Spike* Dichlcrobenzene-d. Phenol-ds Pyrene-dio Chrytene-d|, Sample ID. percent recovery Effluent Blank Influent Effluent duplicate 66 56 88 80 39 28 30 26 117 29 20 21 64 31 73 82 *SfA - 100 w9/L. TABLE 16. QUALITY CONTROL DATA FOR ORGANIC PRIORITY POLLUTANT ANALYSIS OF SEDIMENT SAMPLE Spike* Dichlorobenzene-d. Phenol-d. Pyrene-d,, Chryaen*-d,s Sample ip, percent recovery Sediaient Sediment duplicate 53 50 S3 39 S3 64 49 63 *Spike level StdiMRt - 1B7 M9/9 Sedinant duplicate - 14S P9/9. SO MONS 022450 TABLE 17. NON-PRIORITY POLLUTANT ORCANIC COMPOUNDS DETECTED IN THREE VOLATILE SAMPLES FROM SAUGET TREATMENT PLANT BT (ain) 9.9 13 4 15. S 17 1 2C 8 22,0 III 33 4 34 6 3( 0 39 5 b Tentative identification0 Unknown (44. 43. 42. 41)C Unknown (56. 43. 41. 39) Acetone Unknown (4b. 43. 59) Hethvl ethvl ketone Unknown (43. 42. 41) Hethvl isebutyl ketone Unknown (43. 58. 57. 59) Unknown (61. 43. 154. 108) Benzaldehyde Xylene*isomer Concentration (pq/L) Semple identification 9 1S a.m. 10:33 p.m. 11:15 a.m. 31 ND 4 17 13 29 70 14 8 29 66 170 17 18 22 44 55 81 690 650 ,,N_Od ND 24 35 8 10 98 47 21 33 670 "Estimated concentration based on tht trta of the major ion of the identified compound to the major ion area of benaena*d. internal standard. ^Tentative identification, not confirmed with authentic standards. cnajar masses of unknown compounds are listed in parentheses according to decreasing intensitives. * detection limit is 1 pg/L. 51 HONS 022451 TABLE 18. IDENTIFICATION OF NAJOR EXTRACTABLE ORCANIC COMPOUNDS IN THE BASE/NETURAL EXTRACT OF THE METHOD BLANK*1 detention Peak tine. m. nin Compound {najor nesses) Internal standard 2 21.28 Anthracene-dl0 taount Anaunt Feat area. detected. spiked. Ftrctwt total counts uq/t. vq/l recovery 304007 100 . Recovery standard0'^ 1 7.83 1,2-Dichlorobentene-d4 3 25.42 Pyrene*d|0 4 28.27 Chrysene-d|j 279S84 42S30I 197053 64 100 66 0 117 100 117.0 64 100 64 0 Organics dmcttd Mont detected TOTAL CONCENTRATION ^Include* all nAitune that ware found at or above a 5% threshold on the feATOI peek identification pragran in the Hewlett-Packard systen, corresponding to a detection of lioit of 2 pg/L. klMferKtM*4|| internal standard added ftanediately prior to analysis. 50 ng/i injected egniealant to m p^L in original aanple. Hintseated recovery standard (spihe). added to original saople before extraction. ^Quantitated relative to area of najor ion for authentic standard. HONS 022452 TABLE 19. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC CONFOUNDS IN THE ACID EXTRACT OF THE METHOD BLANK*1 Retention Hal tine. Bo._____ oin Compound (Major mikm) Internal standard^ 2 21.20 Anthracene`d|,, Amount Area. detected. _fotaI counts pg/t Aswunt spikd. pq/L Percent recovery 370013 100 Recovery standardC`d I 4.70 Phenol-d* 37178 39 100 39JJ Organics detected None detected TOTAL CONCENTRATION *IkMh all aahotances that were found at or above a S\ threshold on the BATCH peak identification progran in the Hewlett-Packard systan. corresponding to a detection of linit of 2 pg/l. Snthracened<# internal standard added ianediately prior to analysis: SO og/L injected egoivalent ta 100 pgfl In ariginal sanple. cBantaratad recavery standard <spike), added to original sanple before eatraction. ^Quantitated relative to area of nsjor ion for authentic standard. HONS Q22h*3 TABLE 20. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE BASE/NEUTRAL , EXTRACT OF THE INFLUENT SAMPLE. DILUTED 1:10. NOT CORRECTED FOR BACKGROUND*' detention Nik m. tiae. in Compound (oaior oasses) Internal standard0 n 21.27 Anthracene-d|,, Recovery standard**'* 1.2*Dichlorobentene*d4 ryrene-d,0 Chryiim*d|{ Peak area, total counts Aoount detected, im/L Aaount spiked, PR/1 Percent, recovery 3S3040 1000 54 29 31 -- ` 140 54.0 100 29.0 100 31.0 Organics detected*^'*1' 1 3.22 Chlorobenzene 2 3.73 Xylene (isooer) 3 *.32 Xylene (leaser) 4 (U ensaldehyde and C)-bnMM <iso*er) i *.S* Aniline 4 4.90 Cj'benzene (isener) 7 7.33 Dichlorotoeniene (leaser) 141147 149044 71447 171244 411004 113040 1344S3 5.1 a 10* 4.2 x 10* 2.0 l 10* 4.0 I01 1.2 10> 3.2 a 10* 3.0 X 101 (continued) MOWS 022454 TABLE 20 (continued) Oetention reek time. Ho. min Compound (naior masses) Organic! detected (continued) 7.47 Unknown (U1.12S.1S4. 71) 9 7. SO Cj-benzene (isomer) 10 7 70 C<-benzene (isomer) 11 7.87 Dichlorobenzene (isomer) 12 0.02 Benzyl alcohol 13 9.13 Unknown (119.121.117,93.91) 14 10.10 Chlorooni1ine (isomer) IS 11.23 naphthalene and/or azulene and/or isomer 14 11.S7 Unknown (91.140,143.92) IT 11.40 Chloroaniline (isomer) It 12.20 Chloronitrofcenzene (isomer) 19 12.4? Chloronitrobenzcne (isomer) 20o 12.40 Chloronitrobenzene (isomer) 20* 14.1 N-phenyl formamide 21 IS.10 Diehloronitrobenzene (isomer) 22 IS.30 Dichloronltrobenzene (isomer) 23 1S.SS Nitroaniline (isomer) 24 1S.S? Nitroaniline (isomer) 2S IS.40 Nitroaniline (isomer) 24 10.43 C|*alkone or cycloalkane Peak area. total counts Amount detected, pq/L Jleovnt spiked, Ptmot Mtt___ recovers 43rs2 17707 588111 411639 262696 36927 145425 114324 255942 42047 41779 99SOOO 477200 1650S8 434779 101930 774109 1229S 21936 66006 III 10' 50 17 * 101 1.2 * 101 74 x 10* 1.0 X I0J 4.1 x 10J 3.2 x 10* 7.2 x 10* 1.2 X 10* 1.2 X 10* 24 x 10* 14 x 10J 4.7 X 10* 1.2 x 10J 2.4 x 10* 2.2 x 101 33 42 1.4 X 10* (contimxd) HONS 022*55 TABLE 20 (continued) tent ion Pea time. N. min Comoound (motor mosses) Orqonics detected (continued) 27 IS.73 Nitrooniline JO. 2d C*-phenol n 24.52 Sulfur (SR) 11 21. IS Butyl bonsyl ptitholote TOTAL COHCCHTMTIOM1 Peak ore*. tot.il count*? Amount detected. ij't Amount Spiked. imyt Percent recovery 172253 68944 104131 577042 M 10' 2 0 10' !.l a 10* 1 t X I03 20 0 I I03 *Fer background. tee Method blank analysis. Table IS. klncladee all substances that sin found at or above a 51 threshold on the BATCH peak identification 4> pray in the Hewlett-Packard aysteai. corresponding to a detection of linit of too pg/L. Cknthracene-d|e internal standard added inaediately prior to analysis; SO eq/L injected equivalent to MM pg/L in oriqinal sanple. Sewterated recovery standard (spike), added to oriqinal sanple before extraction. *gnsntitated relative to area ef najor ion for authentic atandard. ^tatinoted concentration based on area of total ion relative to that of anthracene-dm. internal standard. ^Tentative identification, not confirned with authentic standards. *W)er oaaaes of mihnewn co^oonds are listed in parentheses accordinq to decreasinq intenaities. . .. Pooslble aolecslar lens are underlined. ^tanetisa of concentrations of detected ceapounds. eacludinq standards. HONS 022*5* TABLE 21. IDENTIFICATION OF MAJOR FXTRACTARLF ORGANIC COMPOUNDS IN THE ACID EXTRACT OF THE INFLUENT SAMPLE, DILUTED t: 10, NOT CORRECTED FOR BACKGROUND*'0 Relent ion Hal line. Be. an Compound (aaior Masses) Intern*! stand*rdc 10 21.28 Anthr*cene-d|,i Recovery standard**'* Phenol-d., Ai"*mt Peak area. detected. total counts ___ 1'9/L Aaount spiked. i>q/L Percent recovery 4jio;s 1000 * * 28 100 28 0 Oroanics detected*'**'*1 1 1.00 Oenteneac thano 1 M 10.2S Nitroptienol isoaer 4 10.82 Dichlorophenol isoaer s 11.u Nleture of 25% dichlorophenol isoaer and 75% chloropAenol isoaer 4 14.02 Cl*coatainin9 wnfcwoim (121,83,44,173) 7 14.SO Trichlorophenol isoaer 154148 1125466 100080 133682 128535 357472 3 6 x 10* 2 6 x 10' 2.3 x 10* 3 1 x 102 3 0 x 101 8 3 X 10* (continaed) HONS 022*57 TABLE 21 (continued) detention feok tine. Mo. nin Compound (maior masses) Organics detected (continued) 14.02 Cl3*Containing unknown (207.2Q0.97.133) 9 17 43 Nttrophenol isomer TOTAL CONCENTRATION' Pe-ik area. tot.il counts Amount detected. I'O/L Amount spiked. VO/L Percent recovery 44427 317844 1 1 x 102 7 4 * 102 55 x 10' *for background, see method blank analysis, Table 19. ^Includes all substances that were found at or above a 5% threshold on the MTCH peak identification program lit the Hewlett-Packard system. corresponding to a detection of liait of 80 pg/L. cAntbracetie*dip internal standard added ianediately prior to analysis,- SO g/L injected eguivalent to ItOf pg/L in original sample. Seaterated recovery standard (spike), added to original sample before extraction. *QMntitattd relative to area of major ion for authentic standard. *ISttaatod concentration based on area of total ion relative to that of anthracene-d}*, iaternal standard. ^Tentative identification, not confined with authentic standards. Shjer naaaea of unknown cognnda ore listed in parentheses according to decreasing Intensities. Pnonible nalecular iono are underlined. ^tHBMtlon of concentrations of detocted cabounds, excluding standards HONS TABLE 22. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE BASE/NEUTRAL EXTRACT OF THE EFFLUENT SAMPLE. DILUTED 1:10. NOT CORRECTED FOR BACKGROUND * Retention Nik tine. Re. in Condound (naior mosses) Internal standardc 29 21.28 Anthrocene*d|0 Peak area, total counts Amount detected. 1*9/ L Amount spiked. 1*9/1 Percent recovery J75998 1000 - - Recovery standard**'* 1,2-Dichlorobenzen*d4 Pyreiw-d,. Chrysefte-dtj 88 100 88.0 20 100 20.0 73 100 73.0 Oroanics detected*',,h 1 3.25 Chlorobenzene 2 3.77 Xylene <isomer) i 4.37 tylm (luatr) 4 4.12 Riatwri of 9S% benaaldeNyde and S\ Cj-bensene (isomer) S 4.43 Aniline 4 4.92 C3-benzene (iaoner) 423801 230111 125049 294079 577450 170110 I I K I0J 11 10' J 3 x 10* 7.9 x 70* 15 x 101 45 > 10' (COfttlMWd) HONS 022*59 TABLE 22 (continued) Retention Nak tine. N. in Compound (meior messes) Orqenics detected (continued) 7 7.33 Oichlorobenseoe (isomer) 7.50 Unknown (111,125.154.71) 9 7.70 C<'benzene (isomer) 10 7.06 OicMorobenzene (isomer) . II 0.06 Benzyl elcobol 12 10.12 50% Propyl benzene *nd 50% chloroent)ine (isomer) 13 11.23 Nepbthelene end/or ezulene end/or isomer 14 11.40 Unknown (91.146.143.92) 15 11.46 Mixture of 47% chloroeniline (isomer) end 33% cbloropfcenol (isomer) 14 12.20 Chloronitreftensene ft17 12.46 CTiloronitrabenzenc (isomer) 1ft If 12.45 Cftloronitrobenzene (isomer) 20 14.12 Mixture of 60% X-phenyl formemide end 20% unknown (151.153) 21 15.10 Dichloronitraftenzene (isomer) 22 15.37 DicMoronitrobeiuene (isomer) 23- 25 15.55 Mitrooniline (isomer) Amount Peek ere*, detected. total counts ua/L Amount spiked. Percent retmtrr 387403 14406) 493965 047)73 719824 357095 121496 025794 142507 124640 22)0107 1107879 577294 562488 40923 1340059 10 X 10* 3 8 X 10* 13 X 10* 2 3 X 10* 1 9 r. 10* 9 5 X 10* 3 2 X 10* 2.2 X 10* 3 0 X 10* 3 3 X 10* 5.9 X 10* 2 9 X 10* IS X 10* 1.5 X 10* 1.8 10* 3.4 X 10* (coU--<) HONS 022460 TAPLE 22 {continued) Peak No. Be tent ion tine. nin Compound {nejcr masses) Organics detected (cunttnurd^ 24 14.as Chloromtroam 1 ine (isomer) 27 14.S7 Ithoxymt roben.rene (isomer) 21 IB 71 Nitroamline (isomer) 30 2B 13 Butyl benzyl phthalate TOTAL CONCENTRATION1 Pe>k ir#i, tohl counts Amount detected. Amount spiked. Percent recovenr 6*0 S3 91 187626 323S/2 1 8 x 10* 2 4 x 10J 1 1 X I01 8 6 x 10* 34 0 x I03 *Por bKkyowd, see method blank analysis. Table 18 ^Includes all substances that were found at or above a S\ threshold on the BATCH peak identification program in the Hewlett-Packard systea. corresponding tc a detection of limit of 200 pg/L. CA*threcene-dl0 internal standard added imedutfly prior to analysis. SO oq/L injected equivalent to 10M pg/L in original sample. Seuterated recovery standard (spike), added to original sample before extraction. *gnantitated relative to area of M)or ion for authentic standard *ftstiMted concentration based on area of total ion relative to that of anthracene-d|0. internal standard. tentative identification, not confined with authentic standards. *W)sr nasses nf wkwnun compounds are listed in parentheses according to decreasing intensities. NNillt molecular ions are underlined. Ibnntfjae Jf AmnatrsUfM of detected cn^imairtx. eacludinc standards HONS 0224*1 TABLE 23. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE ACID EXTRACT OF THE EFFLUENT SAMPLE. DILUTED 1:10. NOT CORRECTED FOR BACKGROUND*''1 Peak Wo, Rtttntion tine. mn?2**',*Jt ot_ * l Internal standard*" 10 2128 AAthricnc>d| d.e Recovery standard Phenol-d* P*k Ano\mt Ae*ount *. spiked. Percent Min* s__ _ jig/Lpq/L recovery 415039 1000 30 100 30.0 Organics detected*,q,h 1 4.77 CMorophenol isoner 2 8 00 Oeneenenethono1 3 10.25 Nitropfeenol isoner 4 10.92 Oichlorophenol isoner 5 lit* Hiature of 25% dichlorophenoliscner and 75% chlorophenol isoner 4 14.03 Cl-containinq unknown (121,93.44.173) 7 14.52 Trichlorophenol itoner euai 174088 920424 370139 353570 192132 470451 2.0. 10* 4.2 10* 2.2 10* 1.1 * 10* 15 10* 4 4 > 10* 1.1 I 10* (continued) HONS 022462 TABLE 23 (continued) Retention Peak tine. MO. mn Compound (major masses) Oroanics detected (continued) lb.02 Cli-containing unknown (207.97.209.133) 9 17.02 Nitrophenol isomer TOTkL roNCCNTRATION1 at** . t o t ri l counts Amount detected. IKI/L imunt spiked. M/t Percent recovery 42090 23V.M 1 0 10' S 7 * 101 1 I < I01 Voe background. see method blank iMlytii, T<bl< 19 ^laclvdti all instances that war* four.d at or above a 5\ threshold on the BATCH peak identification prayaa in th* Hewlett-Packard aysten. corresponding to a detection of limt of 70 pg/l. > CAmthracen-dl0 internal standard added isnediately prior to analysis; SO nq/L injected equivalent to w IMO pg/L in original sanple. ^Bewterated recovery standard (spike), added to original sanple before extraction ^Quantitated relative to area of najor ion for authentic standard. ^tat lasted concentration based on area of total ion relative to that of anthracene-dls. internal standard. ^Tentative identification, not confirmed with authentic standards. Stejor asset of unknown ceopounds arc listed in parentheses according to decreasing intensities. Pwaibla nolecular ions are underlined. ^Suautim of concentrations of detected compounds, excluding standards. HONS QlZ1*** TABLE 24. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE BASE/NEUTRAL EXTRACT OF THE EFFLUENT DUPLICATE SAMPLE, DILUTED 1:10. NOT CORRECTKU FOR BACKGROUND 'D Retention Nik tine. Ho. in Compound (major masses) Internal standard*" 28 21 28 Anthrecene-d,0 Peak area, tot.41 counts Amount detected. 1*1/L Amount spiked, i*q/L Percent recovery 361259 1000 - - Recovery standard*1'* 1, 2-DUMorobenxene-d, Pyrene'd|Q Chrysene*d|3 Oroanics detected*' 1 3.23 Chlorebensene 2 3.78 Xylene (luwr) 3 4.33 Xylra Umrl 4 4.18 Mixture of 95% bensaldrhyde and 5% Cj-benaene (isomer) S 4.83 Aniline 80 100 80 0 21 100 21.0 82 100 82.0 344454 228741 1S3266 235243 803042 i ti i* t 1 1 10* 2 * 1* i S > It* 1 7 X 101 (coat limed) HONS 022464 TABLE 24 (continued) Rftcntion Peek time, No. in Compound (maior Masses) Organics detected (continued) $ 7 8 4 10 II 12 13 14 IS 18 17 8 lio l 19 20 21* 24 8.92 7,35 7 72 7 88 8 10 10.12 11 23 11 58 11.70 12.22 12.S3 12. 14.1 IS.20 IS.37 1S.SS C-rbenzene (isoioer) Uichloroftenzene (isomer) C4-benzene (isomer) Otchlorobenzene (isomer) Benzyl alcohol Mixture of 70\ chloroeni1ine (isomer) and 30\ unknown {91.120.133,n4) Naphthalene end/or eiulene and/or isomer Unknown (91.148.183.92) Mixture of 70\ chlorooniline (isomer) and 30\ chlorophenol (isomer) Chloronitrobentene (isomer) Chloronitrobenzene (isomer) CHleronitrobenxene (isomer) N-phenyl fomemide Dlcfcloronitrefeenzene (isomer) Dichloronitrobenxene (isomer) llitroeniline Amount Peak ara, det*ct*d. total counts MQ/t Amount spiked. tj/t Percent recovery 211513 14)036 501962 824287 748664 355415 126080 815700 134788 I3IS56 2317024 1189099 591344 548057 72487 1347402 5 4 X I0; 9 5 X I0Z 1 4 X I01 7 3 X to' 2 1 X I01 4 4 X to? J 5 X IP* 2 3 X 10* 3 7 X 10* 3 6 X 10* 6 4 X 10* 3 2 X I01 1.6 X 10* 17 X 10* 2.0 X 10* 3.4 X 10* (continued) moms 022465 TABLE 2* (continued) Aetention Peak tine, He. nin Compound (Mior masses) Orqanics detected (continued) 25 IMS Chloronitroaniline 21 18.57 tthoxynit robenzene 27 18.80 Nitroaniline and chloronitroani1 in* 2* 28.13 Butyl benzyl phthaUte Peak area total count ' Amount detected. l"J/L Amount spiked. W/t Percent recovery 67294 90437 48019S 3244S6 1 * a 10* 2 5 a 10* 1 3 a 10* H a 10* TOTAL COHCtHTtATlOU1 15.7 x 10J *Fr background, tec nethod blank analysis, Tabic 18. ^Includes all aubatanccs that were found at or above a S\ threshold on the 8ATCM peak identification progr in the Hewlett-Packard sytten, corresponding to a detection of lioit of 200 pg/L. CAnthraceM-d|0 internal standard added ionediately prior to analysis; SO xg/L injected equivalent to 1000 pg/L in original sa^le. Sewterated recovery standard- (spike), added to original sauple before extraction. *Q*aititated relative to area of najor ion for authentic standard. *tSthMted concentration baaed an area of total ion relative to that of anthracene-df9. internal standard. ^Tentative identification, not confined with authentic standard*. Nttjor nooaeo of anknown caopoiMdi are listed in parentheses according to decreasing intensities. Peaoible nolecwlar ions are underlined. Swnntlen of concentratiana of detected cagouids, excluding standards HONS 022466 TABLE 25. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE ACID EXTRACT OF THE EFFLUENT DUPLICATE SAMPLE. DILUTED 1:10. NOT CORRECTED FOR BACKGROUND ' Mitntion Ptik tine. No. in Conpound (fMior masses) Internal standard0 10 21 28 Anthracene-dl0 Peak ar*a. total counts Amount detected. l'Q/1 Amount spiked. Mq/L Percent recovery 425158 I000 - Recovery standard11'e Phenol-d* 1,2'Dichlorobcn*ene-d Pyrene-dto Chrysene-di2 26 100 26 0 Orosnlcs detected*,q,h 1 6.77 Chlorophenol iieacr 2 7.00 Bemen--ethanol 2 10.23 Nitrophenol isaner 4 10.02 Dlchloraphenol leaner 5 11.05 Mixture of 25% dlchlorophenol isoner and 75% chlorophenol isoner 60426 130238 861552 331313 324850 1.4 * 10* 31 > 10* 20 x 101 7.0 * 101 7.6 x 10* (continued) HONS 042+67 TABLE 25 (continued) ftetention Peak tine. No. nin Coupound (najor nasses) Oroanics detected (continued) t 14 05 Cl-containinq unknown (121.73.66.173) 7 M 52 Trirhlorophenol isomer B It 0? Cli'Contaimnq unknown (207.97 133.209) 9 17 62 Mitrophenol isomer Torn comcektiution1 Peak ares, total counts Amount detected, I*Q/L Amount spiked. Percent recovorv 193047 41659$ 34361 24IS21 4 S 10' 6 S > 10' 81 5 7 a 10' 6 0 a 101 *for bKltyoMwd, see method blank analysis. Table 19. ^Includes ill lubtlancts that were found at or above a S\ threshold on the BATCH peak identification profraa in the Hewlett-Packard tyitca. corresponding to a detection of Unit of 70 M9/L. CAHthracene-d,0 internal standard added immediately prior to analysis; SO mq/L injected equivalent to 1M0 Mp/l in original sanple. Souterated recovery standerd (spike), added to original sanple before estraction. *Quantitated relative to area of najor ion for authentic standard. *tatlnated concentration based on area of total ion relative to that of anthracene-dt*. internal standard. ^tentative identification, not confirmed with authentic standards Staler naaaes of unknown compounds are listed in parentheses accordinq to decreasing intensities. Peesible nolecular ions aro miderlined. Swatln of concentrations of detected coopounds. eacludinq standards. 022*6 TABLE 26. IDENTIFICATION OF MAJOR EXTRACTABLE COMPOUNDS IN THE METHYLENE CHLORIDE EXTRACT OF THE SEDIMENT SAMPLE. DILUTED 1:10, NOT CORRECTED FOR BACKGROUND flk NO. Recention t if*. in Compound (tor masses) Internal standard** Peak area, tot a1 counts Amount dM*eted. i>q/q Amount spiked, MO/O Percent recovery 24 21 15 Anthrtcene-dH, 158690 93$ - - Recovery standardc ' d 4 6. SO Phenol-ds m 7.7 1,2*01chlorobenzene-d4 JO 25 25 Pyrene'd|0 40 29.10 Chryn-d|, 9476 35670 16900 11207 99 IR7 53.0 99 187 53 0 99 187 92 107 49.0 Orqamct detected9 1 3.42 1. 4-Dimethy lbeiuene (isomer) 13S62 2 5 53 Bicycle!2.2.1)heptene. 2.2-dimethyl* 3- MtkyltM * or BicycU|3.1.1)lwpt'2-M.2.6,i`truttthyt' cyclotettn*.S`rthyl'3-(l-Mtthylcthenyl)-. trM'(-) 11247 BO 66 ozi`*b`> *ONS TARLF 26 (continued) Rlttntion Had tine, m. nin Compound (nojor me**a*j_ Amount Amount Pa,ik *rM, detected. spiled. Percent tot* l_counM_____i<g/_gpq/q recovery Orqamcs detected (continued) 1 5.95 Cj-benxene (isomer) or 1.J-cyclopentediene.5-<1-methylpropy1idene) 1J927 02 ftS ft. 73 Cj-bensene (isomer) 7.20 Dichlorobensene (isomer) 24032 31070 1 5 I01 1 8 n 10* 7 7.57 C<-benzene (isomer) 24969) 1 5 I01 7.53 00% C4-benzene (isomer) end 20% unknown (93,107.121,136) 71340 2 101 7.7 30%. Cl;-benzene (isomer) end 70% Cl]*bcnzenc-d spiking standard 35670 2 1 I01 9 9.00 50% C4-benzene (isomer) end 50% unknown (109.93,107.136) e 10.62 Unknown (lS2.ft7.ftft.l54) 12172 9322 7! 55 11.10 fticyclo|4.4.IJundece-l,3,5.7.9-pentoen- 11-one end/or nophthelene 9101 54 12.27 Chloronitro-bemzene (isomer) 25310 1 5 l 10* 12.42 Cbloronitro-bcnzene (isomer) 0710 SI IS.03 Oichloronitrobenxene (isomer) 21225 1.1 < 10' 1ft.47 Unknown (97.ft9.ft3.70.139) 3677 22 1ft. 07 Unknown (ft3.97.69.111.70) 6360 37 1ft. 30 19.57 Unknown (97,03,111.69) Unknown (97.03.111,69) 7763 4591 46 27 {continued) HONS 022*70 TAP.LE 26 (continued) Retention Nik tine. N. in Compound (iMjor masses) Oroanics detected (continued) 10 20 02 Phenol.4-(1.1.3.3-tet ranethytbutyl) 20 20.13 Nonyl phenol (isoner) 2! 20 27 Wonyl phenol (isoner) 22 20.4 Unknown (135.107.121.134) 22b 20.50 Unknown (31.210.121.05.107) 22c 20 5 Unknown (149.107.31.121) 23 20.07 Unknown (135.107.130.91) 25 23 57 Unknown (91.119.134.10:) 20 23 00 Unknown (134.97.03.91) 27 24.04 Unknown alkyl benicnc(l05.106,134) 2i 24.35 Sulfur, Molecular <S) 24.50 Unknown (150.97.03.104) 31 25.37 Unknown (9I.105.1S0) 32 20.50 Unknown alkyl bonsene (105.100.91) 33 20.00 Oewoen--in.4-nltre-W`phnyl- 34 27.03 Unknown (91.115.149.119.133) 35 27.00 Unknown (91.149.147) 34- 37 20.03 Unknown phthaUte (149.91.204150) Pe*k totn1 counts Mount *cted. ).g/g Mount spiked, n>9 Percent recowenr 0152 0204 quo 3 '7 <,n R2?9 2760 5109 3857 4411 10945 0845 4077 4704 0037 6017 3013 3534 900420 37 49 54 16 49 16 31 23 20 65 52 29 20 30 39 21 21 57 a I0J (continued) HONS 022^,x TABLE 26 (continued) detent ten Peek time, Ho. min P**k area. Compound (major masses)toj. 1 counts pq/q Organics detected (continued) 39 29 32 Unknown (41.114,105.133) 39 29.73 Unknown alkyl benzene (105.104,41) 41 32.09 Unknown phthalate (144.107.41.207) TOTM. CmCOfnUTI0Nh 2844 444 J 5794 Amount detected, Amount spiked. pq/q Percent recover? 17 59 34 4.7 x 103 ^Includes a!) ndatineet that were found at or above a 0 S\ threshold on the BATCH peak identification program in the Hewlett-Packard system, corresponding to a detection of limit of IB pg/g. ^hnthraeene-d|9 internal standard added ixnediately prior to analysis.- $0 ag/L injected egsivalent to 93$ pg/g in original sample. 'beuterated recovery standard (spike), added to original sample before extraction. Quantitated relative to area of major ion for authentic standard. vtitlMtod concentration based on area of total ion relative to that of anthracene-d,0> internal ttwdKd. ^Tentative identification, not confirmed with authentic standards. \ajar mosses of wdoiown expounds are listed in parentheses according to decreasing intensities. Possible molecular ions are underlined. Svmotien of concentrations of detected coopounds, excluding standards HONS 022472 TABLE 27, lPENTI FI CAT ION OF MAJOR EXTRACTABLE CfiMPoUNDS IN THE METHYLENE CHLORIDE EXTRACT OF THE SEDIMENT DUPLICATL SAMPLE. DILUTED 1:10. NOT CORRECTED FoM BACKNOUNL> Retrnt ton Peak tine. No. in CoMpound (Major nesses) Internal standard** 2t 21.13 Anthrecene-d,,* Peat ar*e. total counts AjftOllit detected. M/9 Anount spiked. W/9 Percent recovery 171907 725 - - Recovery standard* 4 t.sa Phenoi-d* 7.S7 1.2-Dich)oro6enzene-d4 JS JS Pyrene-djo 44a 29.10 Chrysen-d)7 1 3.42 2 s.ss 3 5.4$ S 4.75 4 7. IB 7 7.53 9 0.30 lit 9.40 ION 5.1 11 11.43 12 11.00 Oroanict detected*** 9 (See previous table for cwpound identifications) 8575 887 36 29681 16423 73 145 50 0 57 145 39 0 93 145 64.0 9! 145 63 0 10472 8609 10659 28990 42636 26621S 7364 19498 19494 13516 8593 44 36 45 l.l * 10* 1 a a 10* II 1 II1 31 84 84 57 36 (CMtiMH) HONS 022*73 Retent ion Peofc Um, >0. nin S 8 S 3 V X 8 8 S **:S *S :X & I) 12.25 14 12.40 15 11.02 IS IS.4S 17 10.07 10 10.30 19 10.42 20 19.57 21 19.00 22 20.02 20.12 20 27 20.50 20.07 21.02 22.97 23.57 21.00 20.05 24.33 24.00 25.30 25.55 25.73 20.50 20.00 41 27.05 TABLE 27 (continued) PeAk Are* Compound (major nesses)totaI counts Amount Amount detect'd, spiked. pq/q|tq/g Percent ntovtn Organics detected (continued) (See previous table for compound identil cations) 2454* 9775 32066 6439 6966 9267 4116 7727 2701 8040 16710 11119 5277 6192 1593 6090 6759 2297 14737 5107 15369 9231 5030 3311 9505 1200 10200 l 2 n 10* 41 14 N 1 27 30 39 17 33 16 34 79 4? 22 26 7 20 29 10 02 22 05 39 21 14 40 5 43 (continued) HONS 022*TM TABLE 27 (continued) Betention Peak tine, Me. nin Compound (naior nasses) Organic* detected (corninvrd) 42 4) A 44 4$ 44 4? 4m 4k 49 27 90 26.0524.04 26 32 28 53 26.73 29 2 29 2 32.07 (See previous table for compound identifications) TOTAL CQNCEimun0Nh Arnnunt Peak area. detected, total counts trq.'-** Amount spiked. ua/a Percent recovery 2018 1406794 4897 4338 14553 2053 2053 9124 9 5 9 x lO* 25 18 61 9 9 38 8.9 x 10' Includes all substances that vara found at or above 4 0.5% threshold on the BATCH peak identificatton peogran in the Nevlett-Packard SjSten. corresponding to a detection of linit of 10 ug/g. ^Anthracene-dt9 internal standard added innediately prior to analysis; SO g/L injected equivalent to 725 pg/g in original sanple. cDaterat*d recovery standard (spike), added to oriqinal sanple before extraction. ^Quantitated relative to area of najor ion for authentic standard. *BstlMted concentration based on area of total ion relative to that of anthracene-dj*. internal standard. ^Tentative identification, not confined with authentic standards. %ajsi naaess of unAnoun compounds are listed in parentheses according to decreasing intensities. Passible oolectalor ions are underlined. Staaetisn of concentratIona of detected expounds, excluding standards. HONS 022473 TABLE 28. ANALYSIS OF CHLORINATED DI BENilO-r-n I OX I NS IN WATER SAMPLES Stmclt Effluent Influent Influent (rep) Blenk Method detection Unit Spike level KfflMent (spiked) Becovery percent Spike level Influent (epiked) Recovery percent Cl, TO* < 14 nq pibenzofui.in/i ttf t (pot) ______________Incimeia ____________ Cl, Cl, Cl. Cl, Cl. NO HD ND ND ND nd (<nib ND ('7) NU ( < 6 ) 6 61 < 14 ND ('16) Nt> (<8> ND (<5) 12 140 ND ND ND ND ND ND t0 3 2 54 13 12 9 11 69 92 14 10 12 12 14 12 12 9 100 120 100 75 130 120 97 no 75 92 140 99 120 120 120 99 130 220 86 100 101 100 Cl, "Hi ND ND 17 100 20 no ND ND s4 13 10 12 14 92 140 130 100 120 120 7i 65 *M> - dom detected. Nd (<u) - none detected (detection Unit). HONS 022476 TABU 29. ANALYSIS OF CHLORINATED DlBFNZO-P-DtOX I NS IN WATFR SAMPLES S*jaole Effluent Influent Influent (rep) Blank Method detection linit Spike level Effluent (upiked) Recovery percent Spike level Influent (tpiked) Recovery percent Cl. NDa HD (<U)b ND (<14) ND 2 4 4 100 36 39 10S mj Dibonzofur*ry 111'<i (ppt) ___________ I sow*'i s_____________ Cl, Cl, Cl. CK sir cl. T17 ND ND ND ND ND ND ND ND (< 90) ND ND (<4) ND ND 4 11 ND ('110) ND ND (< 4 ) ND ND 6 11 ND ND ND ND ND ND ND 3 4 3 7436 6 7 4 10 18 4 11 4 e 4 11 14 5 It 67 114 100 110 78 12S 100 64 69 45 104 176 38 no 70 70 31 SI 131 33 no 109 101 69 70 74 74 90 *MD - non* detected. ^1 (<**) - none detected (detection liait). HONS 022477 TAILS 30, ANALYSIS OF CHLORINATED D1BOOO-P-D103UNS IN SLUDGE SAMPLES Siaole ng PiNniop*dlMin/a Hndw tppfcT _ Iwtri - Cl. cl, T-nr ti, -nr (1| Sludge ND* ND ND ND ND 11 s 620 Sludge (rep) ND ND ND ND ND 17 SI 030 BUnk ND ND ND ND ND ND ND ND Method detection limit 20 20 IS IS 10 10 10 10 Spike level Sludge (spiked) Recovery percent 13 12 14 10 12 12 13 10 ND ND ND ND 18 34 93 700 - - - " ISO 167 1S4 - Spike level Sludge (spiked) Recovery percent 130 120 140 100 120 120 130 100 69 120 87 120 ISO 1S3 220 060 S3 100 62 120 12S 116 113 55 *WD * none detected. TABLE 31. ANALYSIS OF CHLORINATED DIBENZOFVRANS IN SLUDGE SAMPLES Semple Sludge sludge (rep) Cl. HD* ND nq DiDenrt.!uren/g sludge (ppb) Isomers cl. Cl, Cl. CK Cl. Cl ND ND ND ND ND 33 ND ND ND NO ND 25 CU 39 73 llenk ND ND ND ND ND ND ND ND Method detection limit 10 20 25 10 30 45 20 20 Spike level Sludge (spiked) Recovery percent no 200 220 140 310 S20 no 370 27 110 130 no 290 500 130 410 25 ss 59 6$ 94 112 92 69 Spike level Sludge (spiked) Recovery percent 1.100 300 3S 2.000 2.000 100 2.200 2.700 123 1.400 1.300 93 3.100 3.100 100 5.200 5.300 102 l.no 3.700 940 3.400 03 90 %D - mm detected. 78 HONS 02247 TABLX 32. RCRA METALS IN SLUCCC LEACHATE1 Analyte Arsenic Barium Cadmium Chromium Lead Mercury Selenium Silver uq/L (ppb) <3 1.75 x 103 1.68 x 10* 348 514 2 6.2 96 Reference standard Quality Control Data True Observed value. value, ud/L yq 'L Arsene TN-7 Barium ERA 2767 Cadmium TM-NR Chromium ERA-1120 Lead EnA-1120 Mercury TK-Cl Selenium SRMA Silver SPEX-A 35.7 429 313.5 16S.3 278 IS. 5 10.2 111 35 460 300 160 265 20 10 100 Percent recovery 102 93 105 133 105 93 102 111 Analyte Arsenic Spikeb Concentration added. ______________ nq/L________________ 50 Percent recovery 102 *Ai* analyses by AA. bS0 pg/L of standard solution is added to leachate and amount recovered is determined. 79 HONS 02*479 TAfttf 33. HEM 1C IOC AM) PESTICIDE CQMCOmiATlOII XH LEACHATE Analyte Lindane Endnn Hethoaychlor Toaapgene 2,1.5-TF Sjlvexb Concentration. U9/L (ppb) HD* ND ND ND ND ND Lower detection licit. na/L 1.000 400 SO 1 x 104 10 10 Quality Control Data A known amount of 2.4*0 and 2.4.S-TF Silvex were spiked into the slud?e sample. The percent recovery was: Analyte 2.4-D 2.4.5-TP Silvex Percent recovery 120 105 *ND * not detected above lower detection limit. ^Duplicate analyses performed. TABLE 34 CYANIDE AND PHENOL ANALYSIS OF LEACHATE Analyte Cyanide Phenol Concentra tion. ___________ usZL______________________________ 10 1.297 Analvte Cyanide Phenol Quality Control Data Observed value, True value. uo/L P<J/L 60 SO 116 125 Percent recovery 75 94 0 HONS Q224B0 TABLE 35. TOTAL METALS ANALYSIS OF SLUDCE SAMPLE Analyte Arsenic1 Mercury* Selenium* Aluminum Antimony Barium Beryllium Boron Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Silver Sodium Tin Titanium Vanadium Zinc ua/q ippeT 16.9 <0.2 5.7 2.6 x 103 <73.0 96.6 <23.0 78.8 45.0 4.5 x 104 156.0 15.0 995.0 1.1 x 10* 361.0 2.5 X 103 230.0 64.0 820.0 <2.4 a 101 23.7 1.2 x 104 <519.0 105.0 <14.6 3.0 x 103 'Analyses by AA. all others by ICF. 61 HONS 022461 TABLE 36. ANALYTICAL RESULTS FOR PRIORITY AND NON-PRIODITT METAL POLLUTANTS IN HATER SAMPLES Priority metals Arsenic? Hercuryb Selenium. Thallium0 Antimony Beryllium Cadmium Cnromium Copper Lead Nickel Silver lire Non-cnoritv metals Aluminum Barium Boron Calcium Cobalt I ron Mageslum Manganese Molybdenum Potassium Sodium Tin Titanium Vanadium SANPlR ID. iig/L tpplfl Influent__________ tfflunt* 31 .7 <0. 0 14.. 3 <63 <830 7 71 227 1.7 x 103 777 esi <250 3.9 x 103 4 <0 9 <63 <830 12 <18 91 <35 <460 303 <250 133 890 187 388 2.6 x 10s <70 6.8 y. 103 3.6 x 10 457 562 1.6 x 10s 6.4 x 10s <2.2 x 103 54 <150 <450 77 674 <210 <70 253 <70 186 849 1.1 X <1.5 * <2.2 x <43 <150 `Average of duplicate analytes. ^Analyses by AA; all others by ICP. 82 HONS 022482 TAM 37. QUALITY COWTIKX. DATA POR METALS ANALYSES Of WATER SAMPLES Analyte Areenic* Mercury* Selenium* Thellium* Aluminum Antimony Barium Beryllium Cadmium Calcium Chromium Cobalt Ccpper Iron Lead Hanganese Nickel Titanium Vanadium Zinc Reference standard TH-7 TM-Cl SRMA SPEX-A ICP rep ICP ICP ICP ICF ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP Observed value, P9/L 31.7 18.5 12.2 91.3 410 1,010 831 173 51 1,180 153 123 602 1,100 254 1,090 1,160 1,100 114 157 True value, yq/t 35.0 20.0 11.0 100 515 1.000 920 165 50 1,000 160 115 615 1,000 265 1,000 1,000 1,000 110 16S Percent recovery 106 93 111 91 80 101 90 105 103 118 96 107 98 110 96 109 116 110 104 95 *Anely(es by AA; *11 others by I CP. 83 HONS 022*83 TABU 31. LOQ* VALUES YOU IBTALS BY ICF ANALYSES Analvte Aluminum Antimony Binun Beryllium Boron Cadmium Calcium Chromium Cobalt Copper I ron Lead Magnesium Manganese Molybdenum Nickel Potassium Silver Sodium Tin Titaniua Vanadium Zinc ua/L 450 25 23 6 230 18 210 33 70 35 56 460 70 3 65 60 4.3 x 10* 250 1.4 X 10* 2.2 x 103 43 150 26 *L*aat observable quality. 84 HONS 022484 TABLE 39. ANALYTICAL RESULTS FOR TOTAL CYANIDE AND TOTAL PHENOL IN WATER SAMPLES -- lp. P9A-lPP*>) AnalyteInfluent Effluent Cyanide Phenol NR* 1364 10 1698 Ouality Control Data Observed value. Reference standard __________ US/l True value. yq/L Cyanide Phenol 110 160 222 250 *NR - analysis not requested. Percent recovery 69 89 TAELE 40. ANALYTICAL RESULTS FOR NCN-PPIORITY POLLUTANTS IN WATER SAMPLES AnalvteInfluent Sample ID Effluent Biological Oxygen Demand (BCD) Total Suspended Solids (Tssi pH Total Organic Carbon (TOC) Fluoride C:i and grease NR4 117 mg.<L NR 19 mg't NR 8.54 NR 184 mg/L NR 1.56 mg/L NR 16 mg L Analvte TSS Oil and grease TOC Fluoride Quality Control Data Observed Reference value. standard q/L Hardness 3253 PCS PCS ERA 3253 34 24.9 48.6 3.3 *KR - analysis not requested. True value. mq/L 34 26 48 3.4 Percent recovery 100 96 101 97 65 HONS 022485 APPENDIX A CC/MS ANALYSES OF EXTRACTABLE ORGANICS A-l HONS 022486 GC/MS ANALYSES OF KXTftACTABLE 0RCAN1CS Introduction All GC/MS analyses were performed using the protocol developed (or the EFA-sponeored Chesapeake Bay analysis program. These analyte* were performed by eutomated capillary column chromatography using a Hewlett-Packard 59SS-A CC/MS with a 5934 data system, which used Revision C Software and inluded a 7920 multi-drive disc unit. Method The relevant GC/MS parameters used for the present analyses are summarized below: - 3C m fused silica SE-54 WCOT column - Column head pressure, 7-9 psi - MS operating pressure, 1 x 10s to 4 x 104' torr - Septem purge on at 0.5 min - initial temperature, 50C - Initial temperature held for 4 minutes - Heating rate, 8*C/m:n - Final temperature, 300*c - Total analysis time. 40 min - injector, splitless mode, temperature, 2S0*C - Transfer line temperature. 2S0*C (fused silica column through this zone, directly to the MS source) - Electron energy. 70eV - Source temperature, 200*C - A/D rate. 1 measurement/0.125 amu; scan rate, approximately 0.6 s/scan - Mass spectrometer scan delay, 3.0 min The routine procedure used for GC/MS analysis was to transfer 150 pL of the sample extract into 1.5 mL sample vials along with 150 pL of a 100 pg/mL anthracene-d,0 in methylene chloride inter nal standard. The vial was capped and placed in the autosampler, which injected approximately 1 pL into the GC, operating in the splitless mode. A-2 HONS 0224** Infrpretation of Hass Iwctri The following protocol woo followed in interpreting the mass spectral date obtained froa analysis of water and sediment extracts: 1) Spectra of compounds detected ae peaks in the HewlettPackard BATCH program with a 0.5% or 5X threshold (depending upon the complexity of the saiaple) were autoaatically coo pered with standard apectra in the computerized EPA/MIH ass spectral data base using the Probability Baaed Search (PBS) software supplied by Hewlett-Packard. A goodness of fit paraaieter was generated (1.0 being a perfect natch) for the ten Batches closest to 1.0. 21 The results from these searches were reviewed by an exper ienced aass spectroscopist using the Hewlett-Packard sup plied spectral comparison software. SPOIF. to compare the sample spectra with the standard spectra identified by the SEARCH prograa. 3) In cases where the spectral agreement was judged to be ade quate. compound identities were assigned. When compound isomers produced similar spectra, no specific isomer could be identified based solely upon mass spectral data.4 4) In cases where the agreement was not adequate, identifica tions were made on the basis of manual interpretation (when obvious), or compounds were listed as unknown with their major masses given in parentheses. If a high even mass was present after which followed isotope peaks in the proper ratio, the underlined to indicate a possible molecular ion. A-3 HONS 022*88 The approach outlined Above wot odoptod to tinititi the eoot and tine required for the onolytet of larqe amounts of copillory ehro* matoqraphie mass opectro by maximisinq the uoe of computerised doto interpretotion techniques. Fiqures A-l ond A-2 show tpectrol couponton plots which were qeneroted from those "best fit" condiote compounds identified in the o computerised scorch of some typical GC/TI5 doto. These fiqures show cor.pontons of two different trichlorobenzene isomers with the unknown spectrum. From the difference of each of the two spectra plotted in these fiqures. it can be seen that less than 30% devia tions with the two standard spectra were measured. Since the two standard spectra of trichlorobenzene isomers are very similar, the identification of the peak at 11.0 minutes would be listed m the effluent table for as "Benzene, tnchloro-(isomer )." These ccrparative mass spectral plots were reviewed by an expert ra$ spectroscopist who based cn experience in mass spectrometry and mass spectral interpretation, accepted or rejected the cc.-puter-ger.erated identification. In the example, trichlorober.zene (isomer) was determined to be the proper identification for the compound in question. It should be emphasized that this identification is considered to be tentative until confirmed by the measurement of its relative retention time of an authentic standard of isomers of the identified compound using similar analytical conditions as those used for the original sample extract analysis. Some considerations that qo into makinq decisions on the identity of components in effluent and sediment extracts include: 1) The unknown spectrum must contain all peaks with intensities greater than 10% of the base peak in the standard spectrum. A-4 HONS 022489 rnw 3t4 9*crmjn 4cn nw- im c6mx i 3 Figure A-l. Comparison of the mss spectrum of the highest matching compound with that of an unknown compound eluting at 11.0 minutes. 022'*' HONS K" 3*< S*CCTmjn SCSO HO- 1 lacioci)snaana. I.J.t-irlckUrc CSH3CI3 in n H_2. Comparison of tht mama epactrua of the third highest a*tching coapoend with that of an unknown compound eluting at 11.0 nimitaa. HONS 022491 2) All mi intcnsitiM of aultipltti present In the standard epectrua auit also b* praaant in the unknown epectrua with similar ralativa intensities. 3) Since the DFTPP spectrum in the low eats region is lower than that given in the EPA criterion for this compound quantitative agreement of ion intensities was not required for masses below /e 60. 4) if peaks are present additional to those in the standard spec* trur. of a compound, then it is assumed that the additional peaks are due to the presence of an unknown co-eluting compound. In obvious cases of mixed spectra, the PBS SEARCH program identified the presence of a mixture of spectra with a in the column following the match factor. Where mixed spectra ate cc;.firmed using the spectral comparison program, tne major identified compound was listed along with an estimate of the percent of the unknown compound present in the mixed spectrum Atterpts were made to give additional information such as the major masses found in the unknown, the molecular weight if the spectrum appears to contain a molecular ion. and the presence of nonhydro* carbon ator.s. However, the identification of the presence of chlorine, sulfur, or silicon ir. unknown compounds is based solely upon the occurrence of multiplet ion patterns which are consistent with the naturally-occurring abundances of isotopes for these species, and is used only to give more information about the unknown compound's spectrum. Quantitation of GC/HS Data The calculations used for determining the concentration of or ganics in sample extracts were performed in two ways. All levels of deuterated spiking compounds were determined using the response A-7 HONS 022*92 of tlio molecular ion of oach of the compounds. relative to tha anthracene-d,, molecular ioa. Tharofora. all recovery data vara calculated using authentic etandarde. The amounts of all other compounds were determined assuming the total ion response of each compound to be equal to the response of the anthracene-d,, internal standard. This latter calculation was aade using the following relationship: Cor-.tniration of X Total ion ares I in untnown concentration Anthracne-di0 Total ioa ores anthreecne-d,n a (saaple concentration factor) The saaple concentration factor takes into account the extraction and concentration of the 1-liter sample to a 1-mL extract or the extraction of approximately 30 g sediaent and final volume of 1 nL in the sediment extract. PA:PC for Extractable Organics MR: uses a routine procedure for assessing the condition of the mass spectroaeter and the capillary column in the gas chromatograph. The nass spectrometer is tuned approximately daily using perfluorotnbutylamine (PFTBA) which is the basis for the Hewlett-Packard AUTOTUNE program. The output from an average tune is shown in Figure A-3. Samples weis run in the autoaiated BATCH AQUIRE mode overnight, and with each batch of samples a system performance standard was analyzed. This included the compound decafluorotriphenylphosphine fDFTPP) which was analyzed by the Bewlett-Fackard program: DFTPP EPA Criterion Verifier. The output from a typical analysis by this program is shown in Figure A-4. A-8 HOMS 022493 MTC ren 1N M |/M, l ut KtUC*iyMM< m MOLT*OC<U |rw< rocustui*)* 4TU C*|NMt$ orrscT-m th UN5<nu^)i33 rMSS AXIS ClN*|.MI$? ~AAVU>*1S r*SS MIS 0rrs(T--.lM401 C^I5SION<UA*3M IONS! POSITIVC IttCT. CHCCVItW >?# ACTUAL $OU*CC Ttw ## LOC aha orrjcr.j A. f LIN-IKM T) ACTUAL AH ness AMS# AM/MO i f (IS; UNMH tt) 4tt UwtO) ACTUAL ISO ACTUAL trw iso rrs AMMO ISO AaTIO VIOTM it. M II4H see eit.pt test tt.it set.tt cat t.ts .S4 .tt .St tt to tlt.tt 4)9 tt) tt 1.14 t.tl t.tl wo to tot ooticwt see Figure A-3. A typical result froa tuning the Hewlett-FacfcerO S9IS mss spectrometer with FFTBA. MGNS 022494 OT-V l^TPP EPA CRITERION VERIFIED DRNi 22M2 ?PECTRuni 2*u Haaa Pal. afaund. ** SI 68 69 79 187 197 198 199 875 3C5 41 48 443 9.95298 9 29.7239 9 33.4849 9 199 8.69813 22.8732 1.79278 14.7949 73.8397 18.8387 WTEi '**' MlnlM n\ of range! Criterion 38-899 FMSS 199 < 29 rMSS 69 < 29 mSS 89 49-899 mss 198 < 19 FMSS 190 9*SE PCMC 6-99 mss 198 18-399 mSS 190 > 19 mss 199 < mss 443 > 489 moo 198 17-839 mos 442 PRESS tfOWD TO RERUN... Figure A-4. Computer analyaia of am apectrua of DFTPP. HONS 022495 Typically, the SI and 127 on our instrument fall to--what below tha normal range specified by the program. This fact was taken into account in interpreting Bata apactra. if othar paaka fall outside tha ranges, tha tunin9 of the warns spectrometer was re-examined. Tha substances present in the system perfomace standard were: (1) 2,6-dimethylphenol. (2) 2,6-dimethylaniline, (3) decanol. (4) pentachlorophenol. (5) anthracene-d(0 added prior to analy sis. (6) octadecene. (7) octadecane. () DFTPF. (9) eicosane. UO) heneicosane. (11) pyrene. (12) methyl stearate, and (13) chry sane. Figure A-5 shows a typical chromatogram obtained from the standard. By examining the resolution of the peaks '20.7 min and '24.7 min, and by looking at the tailing of certain peaks such as decanol and pentachlorophenol. we visually determined the condition of tha column, when the resolution and tailing were substantially worse than in a new column, the injection port in sert was replaced ar.d the front end of the column was broken off or the column replaced. In order to assess the accuracy of GC/XS quantitation, two stand ards were compared with each other. A Supelco phenols standard was analyzed on 6 February 1981, end a freshly prepared MRC standard containing many of the seme phenols was analyzed on 4 April 1981. In both standards the concentrations of the com ponents were close to 100 mg/L. Taking the concentrations in the K8C standard to be correct, the concentrations of the com ponents in the Supelco standard were calculated and compared with their stated values. The substances analyzed included 2-mtrophenol, 2,4-dmitrophenol, 2,4-dichlorophenol, 4-chlorom-cresol, 2,4,6-trichlorophenol, 2,4-dmitrophenol. 4-nitrophenol. 4,6-dinitro-o-cresol, and pentachlorophenol. A-U HONS 022496 A -1 J Figure A-S. Chroaatograa of the coluan perforaance standard with the GC coluan in average condition. The nuabered peaks are identified in the tent. HONS 022497 HONS 022498 A-14 HONS 0224" Based on me standards tha average percent deviation of the values found froa the stated values was 28X. excluding 4-nitrophenol. where 7 ag/l was found vs. the stated 100 ag/L. The quantitation of 4-nitrophenol has been a source of difficulty previously, as it appears to diainish in concentration with stor age tiae of the standard. The indication froa the coaparison of standards is that except for a particularly troublesoaie coapound such as the 4-nitrophenol, the average uncertainty in the quan titation of clean saaples in which the unknown coaiponcnt is of comparable concentration to the standard, is approxiaately 130V A-15 HONS 022500 Monsanto 11036 COPY I MONSANTO AtSEARCH CORPORATION / DAYTON LABORATORY / OAVTON. OHIO 4S407 EASC - DAYTOX_____________ (D^/SICTCNt ANALYTICAL nwomi TYU ot l|POT a w* PP o. s J. -- . a. sc n* 7< a. S'/S R(OATNO.: MPA303 JOR^ROJCCT NO 3;i'.:i';o and -*8;.::io OATS: Mty ;s, i?s: PERIOD COVERED: TITLS: ANALYSIS OF TEXAS CITY SOIL SAMPLLS FOR POLY CHLORINATED DIBENZO-P-DIOXINS (PCPPs) and POLY CHLORINATED BIPHENYLS (PCBs) TredericL D. Hileman B. Mason Hughes o in -3UO tiMM fc. > Z ARSTRACT: Three soil samples were received from Monsanto Texas City for the analysis of polychlorinated diben:o*p-dioxins (PCDDsj and polychlorinateJ biphenyls (PCBs). The result? of these analyses are discussed in thi> reoort. RECEIVED Approved by: jun l Robert F. Ivory OATTOH Environmental Analytical SciefiBNTWai rare Center Service Project Manager Approval date: i\n ii ii RESTRICTED DIST1 C O M R A N iY . C HONS 022501 ' . rio\ COTVNUMBEH 1 C. Rinaldi J F. D. Hiltain J B. M. H-jjhe* 4 R. F. I v o r v S Central Files b Tech. Reports 1S90 1:50 i:so i:so 12 50 R3C abstract omit R. K. FIitcraft-12S0 R. M. Scott-)2SA J. D. Wjl$on-C3fcG NOTH: Distribution of this report is rest ricted. Requests for additional copies shoulJ be made through the principal contact at the Monsanto location involved or the Manager, Knvironnental Analytical Sciences Center (fASC), Dayton Laboratory, Dayton, Ohio. ACKAOMLPGLMPw The contributions of the following Dayton Laboratory employes are gratefullv acknowledged: Sample Preparation: 'J. kirk Ms report to Control Filoo. Dayton. HONS 022502 Three sell saaplOs labeled TP-1 (Saaple A)| TP-S (Saaple I), aad TP-S;SK (Saaple C) were received for the analysis of polychlori nated dibeazo-p-dioxins (PCDDs) and polychlorinated biphenyls (PCBs). These saaples were assiined NIC Log nuaber 1-B2-0S-O701. Table 1 shews the results of the dioxin analyses, while Table 2 shows the results of the analyses for PCBs. SAMPLE PREPARATION The saaples were prepared for analyses by weighing S graas of soil into a 230 aL bottle. Forty al of petroleua ether was added to the bottle which was then sealed and shaken for IS ainutes. The petroleua ether was decanted out of the bottle into a centri fuge tube. Fifteen aL of aethylene chloride was added to the bottle and then shaken for S ainutes. The aethylene chloride was also decanted into the centrifuge tube with the petroleua ether and these extracts were concentrated to 2 aL. The extract was applied to a coluan containing * graas of silica gel which had been preeluted with IS aL of hexane. This extract was then eluted through the coluan with 4S aL of aethvlene chloride and the eluant solvent exchanged to hexane concentrate and this concentrate was then placed onto a coabination coluan containing silica gel, silica gel plus HsSO. and silica gel plus KOH. This coluan was eluted with 4S aL of hexane and this eluant was concen trated to InL. The final chroaatographic separation was carried out on a 2.S graas coluan of Koala B aluaina. The first elution consisted of 10 aL of 21 aethylene chloride/hexane (v/v) which was concen trated to 1 aL and subaitted for PCB analysis. A second elution of this coluan was aade using IS aL of SOI aethylene chloride/hexane (v/v) to which was added 300 uL of dodecane keeper and the eluant was then concentrated to 300 uL and subaitted for CC/MS analysis for PCDDs. Quality control was carried out by spiking Saaple B with both PCBs and PCDDs. This saaple was selected for spiking since it appeared to be the aost contaainated and would thus give a worst case situation for the recovery studies. A replicate and a nethod blank were also prepared and analyzed. DISCUSSION OF PCDD ANALYSIS The CC/MS analyses for PCDDs were carried out on a Hewlett Packard 59BSB CC/MS systea using a 30 aeter SE-S4 capillary coliaa for the separation prior to aass spectral detection. The boss spectroaeter was operated in the selected ion aonitoring node following a/s values characteristic of aonochloro through octachlorodibeaxop-dioxin. 1 MOMS 022503 No PCDDs were detected in any of tho saaples at tho detectloa lialta given in Tabla 1. Results froa the quality control samples aro also (Ivan. Nota that tho dctoction linlt for dichlorodibeazo-p-dioxia wore hither than tho spike levels in both the low level and even the high level spike. Therefore no recovery infornation could be given for these dlchlorodibento-p-dloxins. For the other PCDOS the recoveries are not particularly good but in light of how contaainated the saaples were and the short tine constraints, these results were considered adequate. DISCUSSION OF PCR ANALYSIS Three saaple extracts, one replicate and two spiked saaples were analyted for Aroclor formulations. Eight PCS itoners were quanti fied and froa these levels of Aroclors 1248, 1254, and 1262 were deterained. The low Aroclor 1248 and 1254 concentrations reported for Saaple A nay be due to instrument contaaination froa the the higher concentrations of these Aroclor formulations present in Saaples B and C. The Saaple B plus 0.16 ug/g can be treated as a rep licate of Sample B, since the spiking level is ten tiaes less the aaount of Aroclor 1248 present in Saaple B. Recovery of Aroclor 1248, added to 5aaple B at a concentration of 1.6 ug/g, was measured to be 751. The levels of Aroclor 12S4 and 1262 are only order of aagnitude estiaates, due to the large number of inter fering coapounds present. 2 HONS 022504 TABLE 1. ANALYSIS OF SOIL SAMPLES FOR CHLORINATED DIBENZO-P-DOXINS Sample ID .....ki i Sample A ND* Sample E ND Sample B (rep) ND Sample t ND Blank ND Method Detection Liai t 2 Spike Level B (spiked) Recovery 1 4 3 75 Spike Level B (spiked) Recovery \ 35 22 63 ns Dioxin/ea Soil (PPM Cl* cr. Cl. ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 50 2 2 2 2 34 333 ND 2 3 2 2 - 50 100 67 67 34 38 21 33 32 ND IS 20 15 20 " 39 71 45 63 Cl, ND ND ND ND ND ? 4 3 75 35 23 66 cr; ND ND ND ND ND 2 i 2 67 21 12 43 ND non* detected at the method detection Halt A HONS 022505 TABLE 2. LEVELS OF A ROC LOR FORMULATIONS Ml. ASUREP IN SAMPLE EXTRACTS Simple ID Sample A Concentrations fuc/c) Aroclor l*4g Aroclor l.aJ Aroclor i:6; 0.053 h 0.n;gh <o.o: Sample B Sample B (rep) y * 0. P69 0.047 ft. 0" 5 0.04S B * 0.16 ug/g Aroclor 1243 T1 0.06' 0.061 Saaple C 1.6 0.1S 0.37 B 1.6 Lg/g Aroclor 1248 3.4C 0.10 n.po *tg Aroclor foraulation/g sample. Eight PCB isoaers were used to identify the Aroclor formulation and estiaate the relative aaounts. ''Possible instruaent contaaination froa analysis of Saaples B t C. cThis value for Aroclor 124S concentration represents a recovery of ?Sl of Aroclor 124B added to Saaple B. % HONS 022506