Document bdORbNGpKvkEjwqa485grw80

-- Monsanto 11052 COPY/ Environmental Services Report 0 4 - 72- job/project HO.: 482.2070 DATE: 23 April 1982 TITLE: ANALYSIS or WATER AND S-DIMENT SAMPLES FROM THE SAUGET, ILLINOIS WASTE TREATMENT PLANT AUTHOR: Robert F. Ivory ABSTRACT: Water and sediment samples Cron the Sauget. Illinois Waste Treatment Plant were analyzed for the US. Environmental Protection Agency's for the priority and non-priority pollutants The results of this analyses are presented in this report. F n\/ir ii ;i r\ r\ > ii RECEIVED APR 2 MONSANTO-DAYTON CENTRAL FILES Monsanto Rsrch Corporation, Station B. Bo* 8 o Dayton. Ohio 45407 (513) 268.3411 MOMS 220610 COTV NUMBER 1 carl Marciante 2-3 Steven Scith 4 R. F. Ivory $ Central File* Saugat, IL Saugat, IL Dayton Dayton ABSTRACT ONtV R. K. Flitcraft/Dayton R. M. Scott/Dayton acknowledgement contribution* of the following Dayton Laboratory personnel to this project are gratefully arkntvledged: Analyses: S. A. Barksdale A. Ford D. R. Grothe F. D. Hileman B. M. Hughes P. Hughes S. J. Johnson J, T. Miller S . Mitrosky T. Morrow D. E. Sharp H. M. Strickland C. Thomas T. E. Wcosley MOMS 220*11 CONTENTS 1. INTRODUCTION............................................................................. 2. SAMPLING.................................................................................................... 3. SAMPLE EXTRACTION AND SCREENING FOR ORGANIC POLLUTANTS........................................................................................... 3.1 Volatile Priority Pollutant Analyses ........................ 3.2 Extractable Organic PriorityPollutants..................... 3.3 wide Scan Organic Analyses..................................... 3 .Discussion of Priority Pollutant and Wide Scan Analyses .................................................................................. 4. ANALYSES FOR CHLORINATED DIBENZO-P-DIOXINS AND DIBENZOFURANS .................................................................................. 5. ANALYSIS CF OIL SAMPLE FOR PCBs . ..................................... 6. STATIC DAPHNIA MAGNA BIOASSAY .................................................. 7. EP TOXICITY TESTING OF SLUDGE................................. 6 ADDITIONAL ANALYSES OF SLUDCE SAMPLE ................................. 9. ANALYSES FOR PRIORITY AND NON-PRIORITY METAL POLLUTANTS IN WATER.................................................................... 1C ANALYSES FOR TOTAL CYANIDE AND TOTAL PHENOL IN WATER SAMPLES................................................................................................ 11. NON-PRIORITY POLLUTANT COMPOUNDS ..................................... 12. REFERENCES........................................................................................... APPENDIX A. GC/MS analytes of extractable organics ........................... 1 i 1 2 2 3 3 3 4 $ 6 7 7 7 7 8 A-l 01B3/A-D iii MOMS 220612 Number FIGURES Page 1 Capillary GC/FID chromatogram of surrogate compound spiking standard added to each sample before extraction............................................. 9 2 capillary CC/FID chromatogram of the base/ neutral extact of the method blank (Burdick and Jackson water, distilled in glass). .... lo 3 Capillary CC/FID chromatogram of the acid extract of the method blank (Burdick and Jackson water, distilled in glass)....................... ll 4 Capillary CC/FID chromatogram of the base/ neutral extract of influent sample from Sauget. IL Treatment Plant, diluted ten times before analysis.................................................. 12 5 Capillary CC/FID chromatogram of the acid extract of the influent sample from Sauget, It, Treatment Plant, diluted ten times before analysis.................................................................................. 13 6 Capillary CC/FID chromatogram of the base/ neutral extract of the effluent sample from Sauget, IL Treatment Plant, diluted ten times before analysis ................................................................ 14 7 Capillary CC/FID chromatogram of the acid extract of the effluent sample from Sauget, IL Treatment Plant, diluted ten times before analysis.................................................................................. IS 9 Capillary CC/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.................................... 16 iv MOMS 220613 F1GUWE5 (continued) P*5L* 11 Capillary GC/FID chromatogram of the extract of a 1.38 9 duplicate sediment sample from Sauget, 1L Treatment Plant, diluted ten times before analysis............................................................... 1'* 12 Analysis of 59 ug/L Aroclor 1254 standard. using (CC)1/WS-SIM analysis techniques. ... 20 13 Analysis of an oil sample, using (CC ) */MS -- SIM analysis techniques . . .................................... 21 14 Extraction procedure flowchart.................................... 22 v 0*IS 220614 Number 1 2 3 4 5 6 7 9 9 10 11 12 TABLES page Amount of Chromatographahle Compound* Detected in the Btte/Neutrl Extract of the Influent Semple, Diluted Ten Timet Before Analysis . . 23 Amount of Chromatographable Compound* Detected in the Acid Extract of the Influent Sample, Diluted Ten Times................................................................. 26 Amount of Chromatographable Compounds in Detected in the Base/Meutral Extract of the Effluent Sample, Diluted Ten Times Before Analysis.................................................................................. Amount of Chromatographahle Compounds in Detected in the Acid Extract of the Effluent Sample, Diluted Ten Times Before Analysis . 30 33 Amount of Chromatographable Compounds in Detected in the Base/Neutral Extract of the effluent Duplicate Sample, Diluted Ten Times Before Analysis ................................................................ 34 A-cunt of Chromatographahle Compounds in Detected in the Acid Extract of the Effluent Duplicate Sample. Diluted Ten Times Before Analysis. .............................................................................. 3" Amount of Chromatographahle Compounds Detected in the Methylene Chloride Extract of the Sediment Sample, Diluted Ten Times Before Analysis............................................................................. 38 Amount of Chromatographahle Compounds Detected in the Methylene Chloride Extract of the Sediment Duplicate Sample, Diluted Ten Times Before Analysis ................................................................ 42 Total Concentrations of Extractable Compounds Present in water end Sediment Extracts, Analyzed using Three Different Methods. ... 46 Priority Pollutant Screening Levels CC/M5 ... 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).............................................................................. as vi HOMS 220615 Humber 13 14 IS1` 1' It ,- 11 Cl 23 TABLES (continued) p<0e Analytical Results for Extractable Organic Priority Pollutants in water Samples, ug/L (ppb)................................................................................ 49 Analytical Results for Extractable Organic Priority Pollutants in Sediment Samples, wg/g (ppm) Quality Control Data for Organic Priority Pollutant Analysis of Water Samples ....................... SO C-ality Data for Organic Priority Pollutant Analysis 0: Sediment Sample...................... .. SO N::-.-Frionty Pollutant Organic Compounds Detected in Three Volatile Samples Prom Sauget Treatment Plant.................................................. $1 Identification of ftajor Extractable Organic Confounds in the Ease^Neutral Extract of the Method Blank............................................................... 52 identification of Kjaor Extractable Organic Compounds ir. the Acid Extract of the Method Plank...................................................................................... 53 Identification of Ma;or Extractable Organic Compounds in the Base/Neutral Extract of the Influent Sample, Diluted 1:10. Not Corrected for Background............................... $4 identification of Major Extractable Organic Compounds i-n 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, ............................ 59 Identification of Major Extractable Organic Cowounds in the Acid Extract of the Effluent Sample, Diluted 1:10, not Corrected for Background, 42 vii MOMS 220616 50 Number 24 25 2 21 26 29 30 31 32' 33 34 35 36 37 TABLES (continued) p<qe Identification of Major Extractable Organic Compounds in the Base/Neutral Extract of the Effluent Duplicate Sample, Diluted 1:10, not Corrected for Background............................ 64 Identification of Major Extractable Organic Compounds in the Acid Extract of the Effluent Duplicate Sample. Diluted 1:10, not Corrected for Background.......................................... 67 Identification of Major Extractable Compounds in the Methylene Chloride Extract of the Sediment 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-F-Dioxins in water Samples................................................................ 76 Analysis of Chlorinated Dibenzo-P-Dioxins in water Samples................................................................. H Analysis of Chlorinated Dibenzo-P-Dioxins in sludge Samples..................................................................... 7g Analysis of Chlorinated Dibenzofurans in Sludge Samples................................................................................... is RCRA Metals in Sludge Letchtte...................................... 79 Herbicide and Pesticide concentration in Laachate................................................................................... B0 Cyanide and Phenol Analysis of Leachate .... 80 Total Metals Analysis of Sludge Semple................... 81 Analytical Results for Priority and Mon Priority Metal Pollutants in Veter Samples. . 82 Quality Control Date for Metals Analyses of Vater Samples..................................................................... 83 viii MONS 22061? Number 38 39 40 TABLES (continued) page LOQ Values for Metals by ICP Analyses.................. 84 Analytical Results for Total Cyanide and Total Fhenol in Water Samples .................................................. 0$ Analytical Results foi Non-Priority Pollutants in water Samples..................................................................... es ix MONS 220618 1. INTRODUCTION Wile: and sludge sanples 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 in accordance with the U.S. Environmental Protection Agmcy-s (EPA) approved procedures (1, 2, 3, 4, S). 2. SAMPLING Skiing was performed at the Sauget, Illinois by Waste Treatment fi.i-- samples were received at the Dayton Laboratory and submitte to tie various analysts. I SAMTLE EXTRACTION AND SCREENING FOR ORGANIC POLLUTANTS C:.i- . r.fluent. one effluent and one sediment sample from the Sa-d-.*t. Illinois tieatment plant were received for priority pr.lutant and wide scan organic analyses. A method blank, cc:.s;sting of a one liter Burdick and Jackson distilled in glass organic free water, a duplicate of the effluent and a d-:I:cate of the sediment sample were alto analyzed for quality ci.v.:cl purposes. Each water sample was spiked with 100 pg/L et:'. :f phenol-d.,, cl - -benzene-d, pyrene-d, 0 and ehrysene-d,3 tliquid liquid extraction according to the EPA Method 62$ a.u.ysis protocol. The sediment sample and duplicate were sp.Ked with the sane surrogate spiking compounds, but at levels c:::esponding to 167 ug/g for the sediment and 145 ug/g for the seiment duplicate. Al. sample extracts were screened using capillary cc/FID analysis techniques. Figure 1 shows the chromatogram from the CC/FID analysis of the surogate compound spiking standard added to each sa.-p:e before extraction and Figures 2-11 show chromatograms from the analysis of the base/neutral and acid extracts from the water samples 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. x* The laboratory data system was used to generate a summary report of extracts analyzed in Figures 4-11. Tables 1-6 show these results. They contain a retention time, an area, and an estimated concentration for each peak observed in the capillary CC/FID chromatograms (Figures 2-11). Note that very high levels of phenol-d| and Clf-benzene-d4 are reported in the water extracts, due to other co-eluting compounds. The identity of the major 1 MOMS 220619 component* shown in Tables 1-6 will be discussed in l*ter sections on the analysis of priority pollutants and other organic compounds in these samples. The totel amounts of chromatographable compounds are summed at the end of each table. These totals are based upon the assump tion that the FID response of the compounds are equal to the anthracene-d,D internal standard. Table 9 summarises these values found from the CC/FID analysis. This table shows that there is very little difference between the influent and effluent water samples and that very good agreement is observed for the water and sediment duplicate analyses. Table 9 also shows the total amount of compounds identified from GC/MS analyses, to be discussed in a later section. The following sections give detailed mass spectrometric 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 major components are identified m 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 sar.ples. Other more direct analyses, such as direct aqueous sample injection, were beyond the scope of the present study. 3.1 Volatile Priority Pollutant Analyses One organic free water sample (used as a method blank) and three water samples labelled 9:1S a.m.. 10:23 p.m. and 11;1S a.m. were analysed 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 sedioent sample and a duplicate sedimant sample were analysed for base/neutral, pesticide and acid extractable priority pollutant* listad in Tables 10 and 11 using CPA Method 62S (1, 2) analysis protocol. Tables 13 and 14 summarise the results for those priority pollutant* detected. Before extraction began, the water and sediment samples ware each spiked with phenol-d, Clt-benxene-d<. pyrene-d10 and chrysano-du surrogate spiking compounds. Tables IS and 16 summarise recoveries of thoso compounds in the various extracts analysed. 2 MOMS 220620 Large amounts of non-pnonty 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 titimated 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 exiiactable compounds. 3 ! Discussion of Priority Pollutant and Wide Scan Analyses Table 9 summailies the total concentrations of extractable organic co* ; cur-.ds measured in watei and sediment extracts from the Sauj-tt. Illinois watei Treatment Plant. The total amounts reported ir. it.: table a:e calculated by three different analytical method! The totals rreasuiei under "CC/F1D" assumes all chromatographab1c com;; unds have F: L respondes equal to anthracene-d,,. (used as a:, internal standard). The totals measured under "GC/MS-Total" assures all chi or.atographab le Compounds have mass spectrometr ic responses equal to anthracene-d,,,. The totals measured using `GC Ms-Pf" aie totals of all priority pollutants measured using EFA Method 61S Tins 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 title However this last total does not contain the amounts o: r, j:.-p: ior ity pollutants which are present in ti e varices sample extracts. All three base'neutral extractable water analyses show that the major organic components are not priority pollutants ar.d thus the CC FID and CC-'MS-Total amounts are free 4 to 10 times larger than the CC/MS-PP totals. All three acid extractable water analyses show that the major organic components are the acid priority pollutants and therefore the CC/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 CC/MSTotal is due to the more accurate method of quantitation for the acid priority pollutants. 4. ANALYSES FOR CHLORINATED DIRENZO-P-DIOXINS AND DlBENZOFURANS water samples were prepared by extracting one liter of water with 40 aiL of petroleum ether by shaking for IS minutes. The ether was removed and further cleaned up by extracting with two SO mL washes of m 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 H3SO, and silica gel plus KOH. The column was eluted with 4$ mL of hexane which was again concentrated to 3 HONS 220621 2 aLs. The concentrate wee then chromatographed on a 2.5 gm woelm B alumuit column. This column wae first eluted with 10 HI of 2* CHjCl,/Hexane and this fraction discarded. A second elution was carried out with IS aL of SOX CHtCl2/Hexane; 300 wL of dodecane was added as a keeper, the sample was concentrated to 300 uL and submitted for CC/MS analysis. The sludge samples were prepared in a similar manner. One gram of *ludge was applied to the top of a four gram ailica gel column. The sample was eluted with 30 mL of CHjClj and the collected fraction was concentrated to 2 mL 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 5?5B CC/MS. A 30 meter SE-54 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 d:benzo furans. The results of the analyses are given m Tables 28 through 31. A pair of hexachlorodibenzo-p-dioxms (HCDDs) were found in the influent water samples (see table 28). The reproducibility of the analysis of these HCDDs was net 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 is a ND (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. 5. ANALYSIS OF OIL SAMPLE FOR PCBs One oil sample wet analyzed for low pg/mL levels of PCBs. Molecular ions of the major chlorinated biphenyl components of all Aroclor formulations were monitored using capillary CC/MS-SIM anelyeie techniques. Figure 12 shows the analysis of a SB *g/mL Aroclor 1254 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,-biphenyl isomers. This level of Cl,-biphenyl corresponds to 19 pg/mL, using Aroclor 1254 for calibration of the mess spectrometer'response. However, thm signal/noise is too low to verify what Aroclor formulation is present in this sample. 4 MONS 220622 6. STATIC DAPHNIA MAGNA BIOASSAY A static Daphnia magna bioassay was performed on a grab effluent sample obtained from the Sauget Waste Treatment Facility on March 2, 1962. Procedures utilized for the Daphnia bioassay were based upon procedures outlined in "Methods for Measuring the Acute Toxicity of Effluents to Aquatic Organisms'* (EPA-600/4-78-012). Six effluent concentrations (100%, 56%, 32%, 16%. 10%. 5.6%) and a control were set-up in duplicate. Ten first instae Daphnia magna l>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. <;-e. total hardness = 230; pH * 610). The results of the Sauget hioassay were as follows: Ef fluent concentration (%) Percent mortality 24 Hours 46 Hours ioc 56 32 18 10 5.6 Control 100 100 100 100 50 90 0 65 0 3C 0 35 00 Statistical analysis of the Sauget test data by the Binomial. Moving Average, and Protit Test Methods resulted in 43-hour EC10 values (95% confidence Units) of 14% (0, 32), 14% (9, 16), and 11% (3. 14), respectively. Test concentration physical characteristics during the March 17-19, 1932 bioassay are presented below: Physical parameter Dissolved oxygen. mg/L Exposure period, hr* 0 24 48 8.3 3.7 3.5 8.1 5.6 4.6 ----* - -* 7.8 6.7 7.3 7.6 7.4 7.7 Effluent concentration. % too 56 32 18 10 5.6 Control (continued) S MOMS 220623 yhviieil Birwttf P Conductivity. i*ho Trfrpr rtu> * . *C AUtliruty *<ja t c*co3 Htrdntt*. q/L I CtCOj tPOur period. hM t/flucnt CMKint'.ition 0 24 48_J 1.3 7.8 7.4 B.l 8.1 7.8 ----- --8.1 8.2 8.1 e.o a.o 7.9 7.200 4 60r. I . lOv 6v0 7.150 M s: . 1.150 too 7.200 4.600 * 1.PS0 700 100 56 32 18 10 56 Control 100 5t 12 18 10 56 Control 22 22 22 22 -- 22 22 21 22 22 22 - 22 ` 22 100 56 12 ie 10 56 Control 51C 100 3 ' 56 - 12 - 18 - 10 224 5.6 m Control >500 >500 - - 274 236 100 56 32 14 10 5.6 Control 7. EP TOXICITY TESTING Of SLUDGE TIm sludge sanple wt extracted par the U.S. EPA RCRA procedure , hewn in Figure 14. The resulting leachate was then analyzed in accordance with approve1 EPA analytical procedures (3, 4 and S). Beeults of the netals 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 MOMS 220624 part of the RCRA requirements, the results for requested analysis of the leachate for cyanide and phenol concentrations are shown in Table 34 with the applicable quality control data. 8. ADDITIONAL ANALYSES OP SLUDCE SAMPLE Additional analyses requested for the sludge sample include pH, total cyanide and its total metal eontent. To obtain the pH a 10 g sample.of the sludge was mixed with 20 nL of distilled water and slurried. The pH of this slurry was measured to be 11.07. The total cyanide content of the sludge was determined to be <1.3 wg g (dry weight) using an EPA approved method [4]. The total metal content was determined by atomic absorption (AA) spectroscopy ar.d 4!- Inductivity Coupled Plasma (1CP) excitation technique. The methods used are described in Reference 4. Results of these are snovn in Table 3$. 9 ANALYSES FOR PRIORITY AND NON-PRIORITY METAL POLLUTANTS IN WATER ir. addition to the orgmics the EPA-designated priority pollutants include 13 metals whiCi. are to analyzed for under the protocol jl], Fou; metals (arsenic, mercury, selenium and thallium) are analyzed by AA spectroscopy. All others are determined by 1CP excitation tech.:., qua. Results are shown in Table 36 with the applicable q..illtv control data shown in Table 37. Table 36 lists the least observable quantief (LOO) for metals by 1CP analyses. 10. ANALYSES FOR TOTAL CYANIDE AND TOTAL PHENOL IN WATER SAMPLES Total cyanide in the water samples waa determined according to the conventional wet chemistry technique described m Reference 3. Independent standards were included with the water samples for quality assurance. Ir. addition to specific phenolic compounds and phenol measured by CT/MS. total phenol in the water samples were also measured by typical wet cheeistry techniques (3,4]. Independent phenol standards were also analyzed for quality assurance. The results for these analyses were shown :n Table 39 with the applicable quality control data. 11. NON-PRIORITY POLLUTANT COMPOUNDS A number of pollutants as dasignated by the NPDE5 Consolidated Per mits (3) as Group A and B pollutants were analyzed for. The com pound was analyzed for in accordance with approved EPA methods {4). The results for thesa analysts art shown in Tabla 40. 7 MOMS 220625 12. REFERENCES 1. Draft Final Report: Stapling and Analysis Procedures for Screening of Industrial Effluents fonPriority Pollutants. U.s. Environmental Protection Agency, Cincinnati, Ohio, April 1977. 14S pp. 2. EFA Guidelines Establishing Test Procedures for the Analysis of Pollutants, Proposed Regulation, Federal Register. Monday. December 3, 1979. 3 US. Federal Register. Book 3, Vol. 45, No. 98, Monday. May 1. 1980. 4. $tanda:d Methods for Examination of water and wastewater. Fourteenth Edition. American Public Health Association, wasi.ir.gton. D C., 1976. 1 193 pp. 5. Manual of Methods for chemical Analysis of Water and wastes. EfA-62S,'6-76-003a (PB 2S9 973 ). U.S. Environmental Protec tion. Agency, Cincinnati, Ohio. 319 pp. 8 MOMS 220626 A tfl I rule ii. lt u V -M to n d l IC n U rfid * .* > KftMi imli iwi MU* Pfci IPiSf Figure 1. Capillary GC/F1D chromatogram of aurrogate compound apikeing tandard added to each sample before extraction. NOUS 220627 AnPLtTUDC .2S u V -|*t9 n J i iC n lft'ffd * 499 J4 ) II In sinwlft jmw>tct IKM'N INJCCtCI IT |7)lllS9MMMI S, |*S> Nllhodi IWK *I ri$S lr*4l HIS* Figure 2. capillary CC/FID chrooatograc of the bate/neutral extact of the othod blink (Burdick and Jackson Water, distilled in glass). MOMS 220628 A im ir u tt a . j| u V < i (o n d l iC 'ila rg v d *4 4 .4 1 ) 74444. ISS44. - 17444. (M. 1 I.N If In tnl*4 4.1* s.l* tUHTLCi IHI-* 17. It.4* 2l.tl 74.4* IHJCCTCa 77tltt4T 0*5 MM 4, 1447 tt.n it Figure 3. Capillary CC/F1D ehroaatogra* of the acid extract of the Method blank (Burdick and Jackson water, diatilled in glass). MOMS 220629 anPLITUDC . } ( u V * n t o n d i < C n | r ^ 4 . 31 . I t !. Figure 4. Capillary CC/FID chroaatograa of the baaa/nautral extract of influent saaple froa Sauget, It. Treat ment Plant, diluted ten tiaec before analyaia. MOHS 220630 AM PLITU D E 2 $ w V -'M (O A 4 l < (n l rQ t4 m 4 | | . | | | Figure 5. Capillary CC/F10 chronetogran of tha acid extract of the influent sacple Iron Sauget, it Traatnent Plant, diluted ten tinea before analyeio. NONS 220631 ftaPLITUSC n.iS g v-M (cn i ( O lt '? * * * T In kluglH swotc. mItai-lMMt imimtikxcPttcmsl sSStIf??>f*<cl KiW ' Figure 6. Capillary GC/FID chronatogran of the baae/neutral extract of the effluent saa^lo froo seugat, 1L Treatment Plant, diluted ten tinea before .analysis. MOHS 220632 U 4 M .M I nPLlTUDC a .2 1 Figure 7. Capillary CC/FIO chronatogrtr of the acid extract of the effluont sanple fro? Sauget, It Treatment Plant, diluted ten tlaai before analysis. I HOMS 220633 IW L IT u tC .2S u V -M to n d l 'C x ltr g id 4 M .> I299e. 999*. I.M 4.1* 9.29 12*39 19.49 29-99 24.99 29.29 (T In ainut** SM9LC1 l9*4-/mm INXCTtl T 29l4Ct 04 M 4, 1992 IHUK r.*i Mica ltar> Mica 32.99 Figure 0. Capillary GC/FID chroaatogras of the baaa/neutral extract of a duplicate effluent aaople froo Sauget, IL treatment Plant, diluted ten tinea before analyeia. HOMS 220634 anPLITU D E k ,IS u V - tt( o n t i[ n | r g ( 4 I.M tT In ntnules 4.11 *.* . 11.30 U.lt II.M I4.M JONH. Cl lSH-(Stl 1NXCTII ST tllt'tl ON tMUt 10, I fSI nvinoot ihmh *>> mo fri trio Il.n 91. Figure 9. Capillary CC/F10 chroaatogras of th* acid extract of a duplicate effluent saaple fro* Sauget, 1L Treatment Plant, diluted ten tines before analysis.. MOMS 220635 j i C * *- r * I **' 0f - 24>rn . | 60O> 4.ft f .OO II.SO *.# 12.** 3* .** taunt inxcu> at iirtrin o " i, i*: n*lh4i t*ml H4) frotl IFlO Figure 10. Capillary GC/F1D chroeatogra* of tha extract of a 1.07 9 eminent eanple fro Sauget, 1L Treatment riant, diluted tan tinea before analyaia. A n P lIT u llC / MOMS 220636 e n O L li'- ' SC v . 2 * S iV - * c o r t ) i i >c> n .it l (toon. IZSSO. IMS. 0.0* M (n ainulff 4. SO }.* It.00 .M SOBOLti SdllMHH* IHJCOO ! IJtfStl* OH MO 14, l*SI HW0J *i t(44 1:0(44 Ji.M Figure 11. Capillary GC/FID chroaatograa of the extract of a 1.3B 9 duplicate sediaent saaple froa Sauget. Ii. Treataent Plant, diluted ten tiaea before analysis. MOWS 220637  SPCT*un OWLAV'EDIT ca I UL 59 UC-'flL MOCLO* (354 COIL HIM) 3-'23-'93 9f%i 59C 41-3MII) STLS13 014939 0(4939 row 1439-------($T SC/^CI 445 k. . v. (,*e vwWVa^X iM.fl AiJ l\_ TI a 94 Figure 12. Analysis of 59 pq/aL Aroclor 1254 standard, using (CC)*/KS-SIM analysis techniques. MOMS 220638 * s^ccTPun oisPLAv-'Cctr it I UL KWimiCM OR <DtL 1>1H) Jsaa/fS r-H SS<4>-300<> TLt 014134 014134 re* M834 1*T SCsPC' 435 *- .5* v- 1 Figure 13. Analysis of n oil staple, using (GC)*/HS-S 1H milym techniques MONS 220639 figure 1,4. Extraction procedure flowchart. 22 HONS 220640 TABLE 1. AMOUNT Of CHROMATOGRAPHABLE COMPOUNDS DETECTED IN THE BASE/NEUTRAL EXTRACT OF THE INFLUENT SAMPLE, DILUTED TEN TIMES BEFORE ANALYSIS 7 J.44 4,0 7 f . (Vi ?.?i <. i' M 4 +i t.*'? 7 . %* 7.4,' fc.'(.14 J. 1> k .4^ l/,4 i. ?T i.'.: V. * 7 ` f '. i*.. i; 1 v. 1* to. 4* io.T : 10*41 to.%4 10.*1 1 t.O* 11.14 t*.4 11.4? 11.40 11 .ti lt. 44 12.1*4 1Z.lt i;.i7 i:.i4 12.44 12.34 12.47 12.74 MI* a*/L 44*U tv Mi. 1(4U w iii.oj; 22443 V* 912.213 3I"< >1 ii.-r*'1' UDH tv itn.r . #. w w imi.:* 4.7| | tv i.-7 V4 i;.*.r- io;? tfr 1.... 7* 244; tv v>* 47 + v* tv V.. |Tl 6,.C| w ST..I* ;7 vv Ul .011 TSM-4 vv t031.lt It!*** w t:.90 302 ?i*4 w 40*?.** 4+402 tv VM. 07 V 12700 v IZlS Vt :: i4< tv i7; .7 w 1(7.* M7: w 2I03:.2 w 2T2..*J 20717 w 214444 w 9031.1) 20144 w jfc.Ji; 4 w 4.... 1s4tu| :| w w 7*.13<> roi. u: -Tig w *).*3 t'* tv *.?:;. l?l w i'*:;4 w 2U..1I IV-2 w TO.Ml l)l& w 1*7.*% 2211 w 32.111 JOtt vv 11.090 1344 w 2I..VO : t ? *4 w 2*7.2*9 444f w M.7M itit w 2*..23 23140 w **.7*2 MM MMQL-DS CLI-K>:C*f If* 23 MONS 220641 TABLE 1 (continued) MT :,?? 1.99 2 . ** i.o* i. i: :. i t i. rt> 3t i. 4* ; ,r 2, ?4 it: 4 . vs. 4. i; *.: 4. :* 4. < 4. 4 4 . *. *. 6' 4, ? 4.t: 4. ' ' .( . * *1' *.4^ 5 *. 5 * . tJ w 1: 1* <.:. <. r. t.; 4., 4,7> 4*: ?,<*.; ?. iw 7r k T.i4 7. J* 7,4? T.ftJ T.l 7.90 9.00 9*70 9*9* 9*99 t-ftS 9*91 9*11 M4 W9/L *4l?4 w 473.143 w 43.110 i*i* w jo.ost 34f.*. w *T.Jo 17?4 w i*.ori 4 ^ w 40.*44 w tr>yr> w ui. ir' ;?*i w js. ir. t Tt' \ , .Tn It*-* w 13.*i t 1 t w it.i' w Tt_.tfc,l 4:* * W t l*.*3T X > IT/.?. It * ?*.-* W iii.Ttj ;?-: w 3i. t; 1 ;'4 vv Tt.;'. 4r. V* li.Ot* :*; Vl 15* 74 }.: kv 40.30* ir:; V : vv 33. v.: l'C f Vx tt.rti' ; 11 : 1 V- *>:*. 11 V iirt.t:. 4`!V v it:- vv f' ' V. tf'.TsI Z . tH * Tit 6 ? , 77 * * 7. \n: . * t. v. 1 Tt .ft* 4i.O*.', II"**? vv Tit 1 it t c: :-4 w ST.rt-. 3*7? w S0.33T u 1; V- 3*. 11 * V V 31.*5* 10* .44 7 Vv ITH.K 4640 w tt.tTI ;:i? vv 1t?4 w w 3(00 w 1790 w 31.305 It. 0*4 31.001 ll.MI 3*.3tT 2117. w 30. too 1071 2 w I43.3T1 247 w 3.453 741 w 115.040 104491 w 1431.13 14022 w JSS.T4* w 5004.34 2M1 w 104. *35 2U3 w 29*0 w 044 w 35.404 34.001 13.300 NM 24 MONS 220642 TABLE 1 (continued) HI 14.4u.t. 1*4 1*. t 1 . ii 1*. :< l*.?4 ii.i> i*.i; 1` 1 t*. * If*. c. 1* if', r~ >. ;o. <4 it -r: ;*. t* . ;!. ?* i A'. f; -1 ;i it ;i 11.34 : i. * il. ? IP. ` 1 II 4 l*i :.tii i;. ;i. t* *;i; 44* > li.B. IS.ti is. t: 13.31 33.34 21.4* IS. 44 24.0? 14.14 14.1* 1*.U 14. 4i 14.4* 34.00 IS. 03 . 38.41 38.92 38.41 28.04 39.00 Mtt */4 1044 *v I*. IU TC* M 0.3)4 4U" W *7.97!. mi wv is.j 111)0 w 194.72* w i*t.o;* t/ji v 4.*4? 14A4Q v 101 .** K*f4 w tt.oi; II * wv U'l VI* J.f.j n: ' t:. tt i 4?; yl *.J7f t: (4 ! . J "t ?cj w i:. 17' Vs t n . J 4 T V . :-t. O'! 4*t- w 4 7. TT ?'* 1 ' vv 4,'.T rr ;r;4 VV is.o*-. l * 1 < vv :.:4t *3M vv si* 4" 10 v :: vv 4'j r 4 t to::; Vv 142.31* 7441 w S4.4* , it; ^ vv tsr i.t: i;r. vv IT. 4: ; 4. t..l* 0 >>4 V.S 3 . t . . 4 ; v> 447 * 4. . in;. it: * V* : i. >-; 1:: Vt li .4T4 4T-i . 4v c p *T V* 4<.114 it;:* vv 1 w 247.*t* tc*r 1 w 1TO. *4; i*ij wv ?5. US 1CJ 4i vv 141 . (Ifo 3411 w Si. 44 1 i*: vv Z~).T4* ?;.? V/ I 2*.*!I 359* w tOS.Olo *TT wv *3.54r St-1 v* . so; 4v ts.4;t **C3( w 441.31* 5401 V/ T4.1S* :i*s wv SO. 4*0 7|**% w 1;-. v4 17.397 442 4-411 1140 V 14.*03 MX wmtmmcinc-oio 941 10* OV 111* w 1*33 V8 tt V 3*3 V8 7.94* Ml) 14.014 44.431 13.441 4.044 25 MOMS 22064*3 TABLE 1 (continued) AT I. ;< 24. n ;*. U.!4 ;<. * i ;c. rt 24. t*. 46.*. i* r ;* * :r.4' JT.Pf .i .0. ?f, i: ii. il :i,i: ** r . * rt.r*: 1 -' ^ i; i . i " .!. *. .' *. i *. i; i*`. :. l- . * . ! j*.. i* i .ot . l: ; i. 1 i i. * 1 tl. ll. ** i;..* U.M i:.* u.i: 33.0* U.II 32, 3* M.U 94,00 94.22 34.32 34. *4 94.40 35.24 Mttfc v./L i rsr 9v 73.004 4* V4 11. 543 tv 7.*:* 54: w 7.933 |t|6 *v V9 9v s-?-; w ? Tl W> l..M s.r* T.TTt 31 .7 3*. 7*1 2i. *r I3?t v5 V( 9* t; V5 I*.137 ii. 11. T* f ;t ! V5 ;* 45 . 23 4 J. t;-: 1. 3.1 ;t 55 til i 54 ..... t * . 2 7. Tit. vv l.Olt o; V t*.;<i i/V .Cl. 377 3d* ? W ** W n:.Ti l<-# 6 v :;t 4< 1 w I.*73 o( v5 3.311 1 4 1 ' 5. 1 * . T| ^ v . ;*. * t t` V , i.t'-i *; * 65 TC' y**. 5\ 1 1 . [< T V* 11'. i- vb 1 ~ . 7', I **ic t. v5 5. t: . pi * it 1 55 454 v5 *.Cl*l 4v 1.7(1 *; v5 1 o. ;o*. lt-4. 5v 14.30. 1*"T*'*4 5v !*..*; l*ti 45 20. lit *1 1 95 a. *9* 514 94 7. TO* loii 99 >0.3*3 20; 99 2.022 944 19 4.00O 44 9v 11.70* 1*4* W a*. ST* 4544 w io7.aos 54* 99 7.000 >441 tv aj. 032 512 V9 7.3*0 442 99 *. >** 444 99 *.797 W-4 tv 9.930 251 V4 9.4** 44* 99 o.ooa 444 0.3*9 1*14 99 33.000 rTt-t'ic> 26 HONS 220664 TABLE 1 (continued) ?.; 7*. *; :i,y. V.TT W>(* 0f ro M: n J It *.It . <li .5 )*).; TOT*. *'!. I *<-X(iUd I*'* ruti I'lU *** DAT* riLti 1*1 Vk 1 t.| *1 * ' * t T it **' *1*4 IrM t*t <4*1 1 1 * , (,/fit I (#.. i*i.* <>1***4* *< 4 BK 1 M > . t i r * t * 1 ( v * 1ft* w , | ' * i < 1 **. r 6.> t I >f It-* 4* tl* < * * + M C ftl.C ><t r t l *' U/( -*lt**1*.` I vM-* '( tt4'4*'4* 4 1t.4 **l I* '<*]. ,, t n(wi.ii.f i>-> ui , , t >*t*6** t* a*w4t t* tt-# iAt*h*i pt.* |1*rtU4 (I4*M|M*<9 t U' ' (till |m |M kk**-v*4 4'* HJ*4 t 6 t Irt * *t*-*lt i* > ? * 1 * > 1 i ,ii' c ((<(' i* n i1 --I i:; w* >l . C **wuM Ml *44*4 It. 'vlifi Tt, ili-fi I'tl.m |" >w Jlf tit (hrttUtr4BMtl| 4 ,,! i t|U ti *1-4 i*-000 l*M(fk ctrT#|*,.4l i , ' i * ..* . * * " * . * : . v * t 4t<4 ct'k 4* l< I' 1 ** I - ** C*- **T **** 4?T ( * 1 * I , n P* 4t *< . ?H .* ' ' I' r l! Il l Utt'1 *'*%< 1* !# ,#> 4 , * , *; P li tr> 4* t* 6 *' lit *1 **f 1* t'ttl+f tM*f. ! ** l I* i > ,, * i w * **!,. i- * 1 ** *4*t *<'* 4* i * ski**'-*: !.** ill*' - f> >1, I i * * w * l t4 I t . 4l Kvll* i II I 1*4*' Mtll . 27 MOMS 220645 PI * . 77 i. + T, * i. r* * . * \* 1 1 .* I*>p4. JO.* ' II.S- ;. - i j i.; i;.:; i *. t* t 14. | ? 14. ;T 1 * *i is. i: \* iv is,;* k.k u* ;* 14 .tT l*,M 17, It |7*2C l7,fc* it,:'i4,;u,4* If .id ;<>.(? ;*. *; If.|7 W/L ?Q7 :.rr* MSI pp 13. *47 Ty+ pp It 7.3*7 iO pp 11.13* 1 TA*. Pv in. *53 V* 1TI0 Pt ; . 4: ;i V . S7.1li t. VP ***.up 4;*. pp t. P t; pp .34J 4. *r pp ;c-4 pp I.7JT t*T-* v n.*: ;t:s: VP rp*.sj w P 11.113 ?74 Pv sic.*;* 4*;? VP i*t ** H 3.TI-. 4i3; Pv Pi-lii 2*+\ w 3*. 1)1 ::>:i V* ii.n* 6>r pp ,a* :t*v> P SC.*I* *.*i? 1 341 pp tt.Iti r * 417 pv t:*.35f St>4 vp n.*n 4** Pv P.PSO 3<*2(- vp **i.*ts 141 pp n.jti sit: pp IP.*13 :7* p. 3,*7* ; w II*.0*3 114 VP !.* TSO* pp IW.HP >U pp 10. 372 i :<*: pp 1*2*.3 tn pp 7.0*7 2244 N 30.14* |04t Pv !*** 21 MOMS 220646 TABLE 2 (o4wH) it i,;* 1.4* 1 ,4 l 1 " i,4t :. rt ~ * i* 4.4. .4 i. 4i?.*? l.v` 1. ; *; 4, i *N Xu V* r* M rtrf*r ** r: fc* >> i; ?4 -4 7, l< < 4>0 *1 4* M tt tt tt - tl ;7>* tt tt i tt 4.0>4 *. ?l% *1.0* 4 *.t:4 4,0** 4.0*7 It. i . 7* 4.1 7 . 1 *. IU 5*. M 4,|4; i. ',**, K* ub<TifhAa4*rir tQHk. w4'L |o;i.tt^. Ft-XE : : Ct I'*-- *UC s Ml < i fcAl* OATA FfLEl lftJt.1 Tl r <hm u ai irA n>? .,t*t>i*' t-. /*;( .!.rt 1 (* (I 'M lit lr|(t *4 (|4K *< |4* T f I lWf, t t A* UM tl *f Atlrulf> fr. |r* v ,, ; ' Ml * l - . r 1< > 1 *.4 11t* c ***i'*iffl CwrtilitWIlr-'it t v* ... I - utl*-* litl-t>l t< I# tltf ** It !<. } .r (. Alt ** i * a |i>* v^A..-*r,g rtt*A|t a* I (v ii<* t<T4' i>t > Cm ' (tAttwP>ai || v I 4 f*A I fr * 4 4 f,* ( M*t w<-<jt wl.l't t( *44*4 H- IM * I * t % I ('*' . t f ! T (.' 1* *t*v t*.r. itillA* Ml IJ4 1 *r*..T,.t mi*' i '< *r-1 * T < - < <* l<K' >j/Lr T|,. #}* r.| ) , || I Ihdtlvl *11 (l.4*,ut,44 r Ik V 7 i*> n(t |>tT*ffr' ? i WO ***4 t*M<s** <*i' i*> *-g# < y* K4<'Mt 4t t(#f t*t4 i * vt'it*. c**> # f l'IilH viHit it> tt- a** E't'*vii* ^m111 (*<11 1ft llfMit Pr#t#r,t It. Ill* 4tVf# H Ttlf'ta * T.*f a*+ (t|tl4r . M> tatl* *4*1 IM<, '-'."M IMt1 *UUM (**t(4tfr1 Tv It *t tvfl* r tattr S w L <* l tl|1 (if! *4 t*4 Ml| 4M(HI ttlt m*'41'`*4 |I.IT||| *+r *n*r at* tnvtMt lltctM* 1 2* MOMS 220447 TABLE 3 or anaHATOCMrHABLE COTOUUDS I DETECTED III THE BASE/XEUTKAL EXTRACT OF THE EFFLUENT SAMPLE DILUTED TEN TINES BEFORE ANALYSIS t >,44 i.l *. o< ?.*' 5.77 %, 11 <. r l .; <. *,,;; 7,7'. 7 , t* C . 37 ? .6 - t. .V t. : V, 1* ' .* i, i z w-.c-; t i: l j. j4 l'-,4J lf .t io.tr 1*. ! 1 1.07 II. U 1 1.34 \ 1.4S 11.34 11.4: 11.74 ll. u.i; 13-S7 11.34 11.44 ii*ts i;.?4 13.44- MU W/l, l>* v 1603. f`l 14*3* w 74*.47* 544*' v> 4>',45> 7V 4 11.4li 1 71 *-i * If V4 4ft.367 f r t. 77, 11* ; t * V. i *v;,z* W %i t. Bi c; v4 rr .; 4; <: 44 v.t.-- : u 44 *.< ;o 36# > v 47. 1 IB rrr- r w r*i,*it io:- vv if: * V. it*4.;i 1 4< t w :;i.?36 3^7if: vv 4*:.7.-i r r v4 7.74: 4 1 4.*if 4v t:*.:?? ?v< VV . :o: C:*: V* C 4 r , 7 1 TS8 1T : w 4:;,,1*! t* : Si V 1 At 1 . * * 1340! vv :<<>, 47 VV 3' 1. itr ;v'i: w 54*1,:? * VV 357.44u l?v.. vv 45.477 in: w }4.*lf tir. vv 45,to: JV14 w 41.13? I i* V* 3.477 SI40t 4V 1,543 *IC. w 13. V* Sl-V w ac-in w ?. ftl 404 w 1071 w 7*, #0< 304.144 10.475 *. 3#v |4, ;i4 w 334-.V.rt w #5.047 w 1533.37 w 372.*47 M( r><ia-{, CL2*"<Itl-[* 30 MOMS 220648 TAUft 9 (continue) *1 13.00 11.11 13. 11. 3* ti.: 11.34 13.13 w.ao 14.13 (4.3* (4. J7 (4.3' 14. TO .4-tJ 13.31 It. i*. It.Tl it. r IT. U.1I it.;: u. v 14.31 H . ' |T.f. IT.I ; it.tt IT.41 i T.t; i;. i'-' u.; 13.4.. 11.4: i*. It.': 1*.T? 3k'. i<4 30. :< *t 3*1. 44 20.11 11-II 31. 21.3* 31. Tt ;;.it S3. IT 32.4 33.30 23.04 23.14 33.23 23.12 22,44 22.42 23.44 33.04 14.13 4MU **i\ w 1.14? 4091 w 109. iro 400* w T4.I4* #r*i wv 117.1*3 4T04 14*. 103 12*2 M l*. 034 1341 v> 34.?* t K 3*4.314 TOO? w M*.OCl ::to4: w :4,04 :**: w 4os.4<.; iik Vi 44.14; 404 II 4.3'^ :ti js iv 4|4.*TT 4 JJKO w 4*W.f? ;it;;i vi 33it, ji 1014 IV 31.004 :tj i. 3. t;.. 42. 4 w lit. w. s;i w 01.314 |t|4 w ?4.4r.4 :n Vi J?. 04* 201S *V 3047.Tu i*l vv 12*. JIT i '*i vi 4.('2t. :*<4 it 42,34 1 if 4 VI 4. " : J > ; / It T! ,|7> w itt.o;;. 7 : 7 i Vt 1l>4.t| tv; vv 1 >T. 31S 41*45; w t.;*i.** Vi 3--.3TT 1***1 Iv 330.301 inn w 343.3i 1 ) Ml vi **70 iv :*4 II 4*17 iv ?.*? vi 2".i| II IT.0*4 44.401 4,314 70.*44 0. 403 3*.t;o II t-047 311 II 4.0*0 lilt)) iv 2*1'' , 3? *%.. 1 vi *.301 414 i 13.4*0 57 ii 14.713 |t*7 ii J*.T4I zip ii 3. :;t i35t; iv 202.250 r*r- vv 0*.*4* |04 w 14. k*; vi 4.047 2370 iv 31-7*1 3331 w 31.101 4453 w 00.103 m v* 4. 1*5* M 39.000 31 MOMS 220649 TABLE 3 (contloMd) ftT :. 4, ji it.r* ;..<( ; *. Jl 4 i' '..i; Ml* V* u^n* UTl M KsSU ftt* ft.4 ?Z *3? 14.470 To* T 4ft 104.1 ni T ft ft, ft *. ftftII?#. j *jV if i.i 40i>. ll ftft.4.1 ftft 1 1+*< i*^ ::i i: c i- Ut'i r ;-ti hr ) MW rnW.DIt CM.rtC*0t4 TQTt. u*/L - it** MUi MU MU l KIS7 to'lt: tt,* *1*** r**t 1ft Ipm 11> Cft*iltftr f/f i; * ft * It* .!## (hlrH* fatrict ft* ft tftMC 1*f I 9-* , |l>. tf.f tm T*` vhatl ft# ft 1 (.ft ftf ftft wr , t l ' |r.TrT*t Cf-M*-tft ft*, ft t Kft tft***ftftt CfthCftOlfftt Iftt.ft (uft'D* ft* * <ft '#l*l*1 1 Uf|4ft ftt ftftftftt ftft * I# tfcft ftftftl ift (tftftftft* *^AM>ft 1 *.* *.!*>.-<. cftftftV*ift *ftftftftftftft Ift ftftWftl t thft )Mft**ifti tlft*.4lft< 'll.#* i<> Qia.ftt ftftwlftffttftft Cft*ftftw'<ftft Iftftfttiliftft 4`ft ttff t`Ml v* I I * t *.** vW'tl I ft I* ft# ft ft ft ft* ft t ft tt* Mtli 14 ft* l m 'trftftft. .C(< ftvltfft* Cft*W*4 *ft| ftftftftft tw '<* Vft | r ft f.* ftM ft T * ft*. IOO Wft/L. 1< r |{.f %il* .%lt i. ( : p.. . ,. tft,< f,* r*. (f r RfiMl tl' ftll (M*N1lfl*tl<l# <Kftit.j W* ftf.ft #4.-0O0 <***' t.. * *. tw<4 I im mcI cr> ft* Ir<tft4 t-irft<lief Prfttftftftl. 1r.f | J r. T it , ** t t,<r 1 I * ft*|twtft**t C ftCxaftftft * f *>'* Ift * If. U>* ]* !*> Ml ft* Iftvfttft f'ftfttC* - Wft/l Cftf* ft* i >1 I 4 f r J 1 * W * ' ft* I M ft* ftt 1ft T i (*! 6#(M Mil ftftfttL I * ft j (ft tiTftlAf# v * * ft * i lU* 4#.* : . i ift# fttuntT fti Mft* n* ** I*!** i * 32 HONS 220650 TABLE' 4. AMOUNTS OF CHROHATOCRAFBABLE COMPOUNDS QCJSCEID IN THE ACID EXTRACT OF THE EFFLUENT SAMPLE.. DILUTED TEN TIMES BEFORE ANALYSIS 51 Mm v*/L y.u 7. i* 4.;; \ .46 Ivi >. l*.4 U.4 i..* v r., T 1i1 l i I*. :* *. V l*. 14 l4 . ' i* . :i ir. i . - . * l r . F* 1 ". 1 : -;: 17,<: i:* vis. 14.:* ' i * -- ll1. 1 i :i. i. i* 3*.*'. 17.4* 3M7 si,*: z * tt i.ni 31*4 tt i*-^i i x< t* lr 1*7-44 I74vr vt 151*473 1 > .* tt *. *6^ : t * <. or-4 rir tt k'i ** -1 * tt :* i .< i Ik T* k i . i * r,4- J vt *.*..t: 54 4 r !<#* * vt 1 4 :. 4; Ml* tt |4. W-i 1 tt s..*,- 11!. tt + , ti V*"l tt : i- :. f 4 7 t.74| it*. tt i. 7t t* t : * VI *'* t* 4 1 . t-*f *.*: i 4* i: * vt 40^.:*-4 Zi tt t.44| I 141 tt itt?:*. IT* tt T4'4 t. ** vt ll>, t '] li*. ( Ji* 7r *7r?<- tt < >7 tt 11. i: t tt M . *vT' : 4 : tt 4*T?4 7*:?? tt * ; tt *4.1 - .1 tt ?,*#> m* , * ` * tt * 101 tOTtl MtCt titfiT: nociiUt ui* riLti t>u; *)OL-K TOTHC */L 10077.*7) MU D*T* riLIl I*it: Wifi li,* It,.. r***rt l itMitld <> w tli* ci<iUti . K/ll[i tMiiiu *f t Mli>'ln ihltrlH tulrtcl < *n tniit wtn I* V >1. !* rtttMIt* ll Will *r klhvtlli th* 4**4 uMtft Ihttf'ttH 4h4 t h IfWmM ltl*h i.tiLl < * .*,**** v <** . I M.t*l |. (Him ttl I * l< m* t (1 t. (ttakin til* .MmiM C*--**4 ***** It **<i*l It th* iMtllill ,*h4*l4< tMMtlllifllOi Clh*t Htlttttli ttHttlilt ittiilltllt tr* laidtili ItltlH tIMMMt Met * 444*4 t* til* Mill Iflf'l lltilK" Mil. ltk ttltlt CIWH** Ml UMI ll M 4 MU' (MClhliltiln *4 IM M/ll Tit* illn tit ludilll til ill MlHirill4lll iimmIiII Milt IimIi lilidl lilmi TiMO tM M>MO Cutlet cmiiimMi t- C? ttf*v*h CM MiMl tilniirlMil |M Will 44* t* ttlrtf 1*4 HIM It* fFA Itliivi IK L.tr*<11M trilulli It* i4*tlil> *4 mimiimiii **lt*l*tl immmmi Him t* t* HUM |ti It* *-** IMlilll tl l***l* *.**t*f IMI 5 M/l til t* MIIIMl t> #**th* il*r***lt| i*t *# it* Mil t***t*tl 4*1* *!* 4 ec/nt<M It* <**lll*l> *ttlt*l* Cm **l**lt. #*11*14414. 4144**1*4 14 4 1*1** 4*ttl*t. )3 HOMS 220651 tabct s. MoMr or chromatocrafbabu cqmkuk> detected im ths BASE/KEUTRAL, EXTRACT Op TBS StTUnWT DUPLICATE SAMPLE, DIUJTED TEH TIMES BEFORE ABALYSIf AT ?. ** 4. C-4 C. ` 7, < , 1? i `'f * . *< Vi 7. * T. < !. 1*11 4.4 A V . *> < *1? I*1. J v. 1 1 i . i* 1^.44 1' .Tfc l-'-.J-T 11*. 1 |.07 Il-n 11. it II t j.r.v J J-*$ U*? n.ii j;, ir ii-t? um 1 ; . 4*. i ;.r? ;.74 12.*4- Mi 'L uni irk*.si u:.t V* tu** v TT.S.O*: 4k!- 5. lil i ? vc'-* iw i*-o.*; 3K34 w TK3.5IS t;';4'. V J 1* * : -s-T-9 v* i-i.m it" vK :*s.t> <, 1 M *. i;i it' frr *. **< 1 it: frt 171 lv 157.41* w **.4*5 | <M l%> w l*7-.4* i;#c v* 5tV*4i w IrM. 4) ir;v w II.*.''* 44;/>i vv *i.JT? i:?t V* 3*.tiT 4:n* w *;.?** vuary w Kk, il > *-*:l*! *' * 1 jtf.*.-... i*t-;; V* 1130.41 i V* 3i.tr< JTT. . | .;. vv :*.; 1 ! L ' ? w i:`.*s.. i w U-tH ni; vv It . ("45 t*+* V V 11 0 1 vv 4S.u -VK VI i.o.i 11? tt 3.334 Hi >V 3.*l* 4 Vi* vv *3.111 111?*. w 31 1.0*4 *k*> V 13.115 rts w 4-301 H3 w M*t lit? vv IT.10* Z*ill w 334. *54 1014 w *4.ITS 104^)4 w It4>.*3 !??? w JM-53* WMC ui-ki.:cn*-c-* 34 MOMS 220652 T^BLE|5 l*.00 ll.l n.rr i:i: ii. * l?.rr 13.CS 14.0*t*. Jt >*.?4 14. 1? to,**1 |4,7C 14.5; 1?.21 iT .5^ IT T r t r. 1 : JT . 7< i'. i: j* It .4 / wc io. |7i" i t. ; tT.V i i; i:.t? k .f-w.;f jj .4: 11.41 15.71 r-.; j*. i -.t *.'. Ik-tlt XI, 4*. vV.4?` Tv. 41 2I.X3 XI. I1. 31.70 Sl.w za. i* a;, at 2J.W 22.1* . n.K <r'L ax27 W 4X| W tl.Ni yr* w *4.OS) 7^47 w no.*o 3W? IV 4.044 *14 w 12.441 J 4('l vt J0.404 * 1 `*K<t tv rr-4i w irt.4,. : > * ir vs * i^ i w 2?-: : w %*; Vt I.S * '. tv * *.t; i 47t?; w 44ZT.0I w j.n .(i* s*; vt ::i tt 4 T Vm *.*t ..;.** >* w u*.**: !* W V 43} ; ?* w Ji.OI. 777| vl 40.*10 :::* 1. 5*1 *.4$ I-* 7 - V* VI ,.;t* ; i . >1 4( .54- i;: *. tv . i.ir-4 vv 41 .71 J17'T- vv 1 T j. J i i 114,; V. *74t w J*i.*** 4r v;c i V. ***?.i; I'nr vt 4.14? 140? tt :i.sw I7v * tv zv., ** w a* i. 443 JTCiT vv :vo*i 7;? VI IW.<4* 1?72 20.14* 4f.| tt s.a %%jf tv TT.*4T ?43 VI 11.2)1 2327 tt 2. I T 404 tt 33 tt .*2* t.*T3 217240 tv at*a.ia til* vt *4.414 Ml tv 12.3*. St+ tt 1. I* ;* tt 2T.lt) 4 44 . I4T 19424 tv aa.*4 4407 w 100.0*4 1410 w JO. M* M vv I2.4V4 *44* vv 42.9*4 im w *4.4Tt M> )) MOMS 220653 TABLE s (eoetimtd) r 2*. 4` i*,4j ** `..*1 ;t. ii ;*.t! :: .t* :t.t" : a* : t. * Mil Af*/L V* 77.WI' 704 T v 4:0* V* 41.700 J'.T 11*; M 4.144 1.117 :7.?f 4u; S. *u*. iftT-* Jt.420 ;ur ! a.or* MIS 174.7*1 Ml 11 1*.: 1 : " 1 fr* 1M. V* 41 u n- to. . *<> : *0 tt * . 4 ;. t M 1S7.4S; CHH1K-DI2 TOT**, W*/L * b*T4 riLEi MU* o*f* ricfj ims* N T( ; Tl. 1* t l>* ctajllft*. C*: ^ am: hi <* 4 MU- J*i.* v* * l*t 4i>' U*> 1 " 11). 1*`* ***<.4||.J. 1 I M V-ltl Art 1 (. *< ti u`.i! |i v * r (**.! #. fi C6**6*At <#(** t * 4 11 <*>. UM ' 1 -'' Avl'i't l< AIIMA^BIa I# Tht It '6-*J -- 1' lllvH'l I1* w''l ItAAvftt* it Mul 1 t*.* |r.U> > '* j' i- A'-"* A , Cl*l |4ttA14 |4M|>>*>1 m> * * - ' >-*6 1 # * * 1 I C .*- k t*r,41 mi. |<|. Al 4 4 4* 4 I V Mlt M*- <t t*4*K. (#')< tll IM Ml A4J t *(' A* 6* 1 C--* w4<'L.< T'- 4l>/ * *r>Al<m A*Mk't ylU * ftAtl 1 < i > f I ((***< 7.0**J 4<>J C 6'r * A #. f'0* V - C* IF.r.yAf i;4 *'UMl < 4' t CA'444 M(ti C4. la tH AM4 uii. tUt nti>4* E.U|{tif. 1141#c J * t itfMlti A# A44.-AI M-r I t I tiUwIMI C*4ttt.U MF` H M *> M* 11*4 |vv* IMUliA |l Wvt't frillir 1Mi t f/L t# vtl6r>,` t>i tiitirtf AtAltth 4* H* MM 4*4(1)41 441* *114 1^4 4 Mt If.a (*6|1l#r 1 GC'R* IMlTlil M*M1 MllytlMti IlMuHfl I*. 4 )4l#4 MCtlAi.* 36 HONS 220654 (TABLE 6, AMOUNT OF CSROHATOGRAPiiABU COMPOUNDS DETECTED IN THE ACID EXTRACT OF THE EFFLUDT DUPLICATE SAMPLE. DILUTED TEN TIMES BEFORE ANALYSIS M MfA */L MM 7,34 ,4 UuTT n.s; 1 . r- 14, ic J4. ; J4.V .1 * : i*-.' 1V 5 ^ .iv : U.(* j.j- 11<; .; : j 13 . *v.: 1 ! > .# .j ;4.4: ;,* 17**7 ;4s^c 3*3 t# *.* 374: * So.r%> I^*t7 *v l**.0fc* >74:1 V* tjt.i:* II Mi.?*: :ti*77 I* jmt.s; I-1C* v *1.04) * - V- J v* TH.Mi Kmt #* I. t > >r.;t V* i*i.*;T 'a!' ** 1 j.O*. I3.it* II i.u: V*. 11 It 1< 7vr h n.xti ::.*n t;v/. </ Tti4.*i: 7 *. 1 V* im.ti: 4:vV# 1* 371.341' * !* *1 4*i I* 9*.r #* 7. Ii; 12.*3'. 1l.*2i 7144 * *y.rz It * 14 It ; j`-; It Wi It *7*% *4.4*3 I2TI.33 1C>.*I* :*.;io 34.T* I.Vlt 74*17 310 4; It II II 4.3*4 *.303 :?r II J.*4l 30} H *.03* nM0L- OJ~K4tD<-ft* *n T*a*cE*a ' 01 <j 1C14* Mm a fmoccmco Uili* ricti i*j TO***. *'L mm 6*i* filo Mt*3 NO If I Tl>* tl.t Pt.tri I* M.tl.H #'M *4* C**lll4'< C^/Fltl *l.*l.*l* k< MUilM (!> * * Itl4|( Ml*. >) IH> < SI. T4 ttllltllM t |M MU 11* . U. *r*4 ,lt *'4 ***' C 4441 4 *44 *4* * .! C*h*4t * t | 4.1* *U*.'L> ... itliaKUt < talMMIC **44*r4*. If *4* Mil I* MM*. 4. *, 4II4|I>I III CMlll niMIII II **Ol t* *4* lllulll IIHW*' IIIMlC|lf*l|(> QI4*f 4llf.4H4 CMMa.ll 4***<lfl*4 l>. |a<.M4lf **l*|4* IMflaMI *4144 IM *44*4 I* 14a **<*r I|M|| Him *.lr*ctl*4 MMI. III! *|kl_4*_ j****<a4 all *44*1 I* fr*fali T4* *|lal *4*la4|* lft(l*4** *11 CMa*iM*r*.l||l| Ui.l.Ml alll ** I44lt** Mlaatl T.000 **4 M-OM <*4*c4 c*.r***aM* I C7 iviam CM ***! 44lllrb*** 1 *44 aMl c* M **lr*cl*4 aiM 14* CM I4ll*4 CSS lairiiliM r**t*c*l. T4* I4MIU. < ***-! I*a Ita **llt*M t**4*t naan I** ******* *4 *4* *44*4 4441**1* 4* 1***1* ITMtir *444 S **/L 44 |* 41*44*4 |l #4**44* *********** |*4 *4* ** *<**) **t* ItltiMI mumIn* *4* MMll*r* 44*1 **** #4* ******** **lt4t**tl, 4|*Cw*l*4 *4 4 ***** ***!*. 37 MONS 220655 TABLE 7. AMOWT Of CHROfUTOOUPEUl* MBWM tmil> a THE METHYLENE CBLOftlDC .EXTBACX 01 TIE SDHMEVT ? SAMPLE, DILUTED TO TJS BETOR! ANALYSIS n V,4 . . 4* ;, *, , . . .i .i . .,, :, *s ' ., ; ; ,,4 ,,r ' .* . `? . * . ' . '. .t *' t,i s': *, s4-' 1 s ' .\ #;i '; ,4' .u , t* .74 /; . * i ls>` i. 1* */ ;j jo v V* M 1. I7 II .4*0 fM :v4 H > II . i -, |. *tt ftv 4. i 7 w `.17: i. k: ii. !>* 4.U7 *0.704 u ;* V * i; ; V** I. !-< I< . . Vi.(4! 4- J'v w `.i; I64T' IV i '44 fr. 1 >4.1' , iw * * V| 2v. 111 7.t*>7 1*; 1* 1 >' i I'li t iV vv *i: titlt w 4 > * i: vv 5*2.074 w * V* ; i;; i -- 4:;, \* IV ' #' Vs : v- r * *., *, m. k.: 5. MT i4.ii z-i.. 7. i: .1.4* 70.. ii;.*:* oil vv 4 i.;; V ' H.*:; 0* . $40 t: i ;;. i jt-; **'* It IV w VI II :, 114 :;.o47 i7.g>H 2.44,1 V 3.0*0 VI 2.4*4 II 4.*37 w? VI 0.319 :i v lY 10.712 4 **? VI 7.074 t- i IV 7.200 w III. ft#. 34 MOMS 220656 TABLE ? 1 llo*J ixa& i.i: I*.*; 1*. H 15* tt.: 13.*> It* *4 1*. 7J it.;o |7.3 IT.*. 1 7tu 17.^6 ii. r* it.:: 11. i .i i' -' ; i -. r i i;./ i. i*. * lv-4 1C ** ' . -* if.. iT ie. or ;r.. 2... r.. so.t-'i 2>. ' ill* II. i: .!.< i1. i. * iZ. II 22.01 22.51 21.44 22.2* 11.04 22. n 22.42 lll 23.22 Z2.00 2>.9 i.r*' I It / 7W M 9.005 903* to It.*22 to7* to 13.008 1441 *0.0*0 4tJb w tu.rro 4644 to to466 to10ft* 0*. Ill 0.900 >0.20* 2*4* it 2" 01t5* IV V* 29.200 0.000 3. 05 4lo 44 M4 44 0.020 7. I ' It *i; 2<fe to4 5. 002 2.000 t;? 44 IV..> ** 4v 121.070 it; i W 20.070 *7 44 ;1 to `TT 44 0. *2* >.3*0 5.1,77 44 5. ICO * *0 V4 13.000 M 71 >4 7:. 5t> 17?.:. 14 ;*.I7i 44 o. 7!- 1 .i 44 I.) 44 11 r* 4- ;.c.i to .5.-1 lb. 202 5.01-0 ::*.. 44 5. 057 : 4* 0.70* V* 1.050 *23 vv 11.135 441 w 7I.7W. Oil V4 i.m o'-io V 05.19* 2il w 22.no: 222 to 30* 44 3. 1*2 I.M o'* 44 7.915 1*22 44 20.200 *l 44 *.>20 m0*4 Mi 7.0*0 2**0 **.*99 104.0 to 15,07* I40T to 22.031 I4u| w 27.027 2*4 w *.*OT 1*07 w 27.132 10)0 W >0.105 :ro 44 17.0(1 Site w 71. OM 1*2* w 27.912 m w 1*.118 1290 w IOoS w 040 W I0.0** 0.959 >2,.*3 MOMS 220657 TAME 7 fPDCUUdI Rjr 24.0b Mll 124.001 221* W 02.440 4340* VW 434 V* *.Slt MHIMMt-tlt 8^4 0 :z.i4 or 44 1341 4V 1021 W 3.172 22,205 14.317 iz*rr M.: 1724 V0 Ml ao tj; 44 T.0 *.*30 10.774 <1"* ; <, i j ii.ii 2*3 44 2** 44 1m 44 3*4 *4 r/ *4 4(T 4. 3.4.76 3.341 3. 74* t.T.** 17. 7* f. . ' ;* >i :*.. * *.. r * ?*.4> .4: * * * it-; j*: v 1*4* *v 2;.: wv 13*4 V4 >M 44 k.i 44 l.i4 73. *31 l*.341 33.345 II.M, ; f, ; . . ". :: 44 7321 v *:. 3',* 1 ' A i. 1V4 * r. v* ` " . * ir. I* 4 4 * * 2K*. vv *1 f, v4 !*: . 4v tv v. i.ir: t. 7*2 w 1*, 4 * *.; 34. U 1 ;- ' ; I>4.*UC 11.277 PV4t*-4ll. ;j * *i i:.i* ; *, i* i ^4 ; .***-* mf. * 4 :*. * i .... x ; jl* 4v 4, 75* lit" 4V If.#'' 1237 >* 17.441 * .1 4. .14 4* 7-- .214 |l* V 17.043 14* W 10.411 73 1 vf, II. 3*4 *3' 44 .**<* 1 -4 44 77uf.74 a* * - * *. 1 . * T 1073 44 13.230 ** 44 24. **7 : i i * 2- *. 1| 44 *- 44 741 40 13.00* 0*.427 *,0t>4 o* mis-Di2 . i 1*71 44 20.214 Itim* MI(A * (4 '*Mi tom **/ 1140.914 nxt. ;[ tu-.i . ui iphj Mu 0474 nut Mil) MOTtl TN ** f**#M 14 NotrilM IrM IM ciMIlin K/IIO toll III *1 4 MllulM* llilHIM IMIt * 4 IIIIHOl I*WI|| Tit* ttUOlIM DM **ll* 41* tlMlMt IM 4*44 yoill ** l(it***t*r tttM.lt 4ti4 IM HtttMll fw>(44lr4ll40l **'*> * 4414*141*4 M *41** 4*14*4114 44*44*<4. 11 IM **44 14 4*4*4. yt 4. *t*444* 44* *A44M* lt*ll|M ******** |4 ***! * 14* 4**tl* 4* *I4*<**-4I0, OI4*r **larl44 <****4* i4*ntlft*4 at* ftit***i* ItlllH ty*tMM>4* *4144 ** 4*4*4 *4* 44*l* ****** *.tl*ttl*M 4*444* Ull MtllM 44444*44 44* 444*4 * M*lt **4l**4t CMIMIItllM. *1 200 */ Tl* 41? ,ti utot* ih4vo> few l mom ?4><kt*% *m4 )4i C -- wMMU ^wftoiNMi*|* 40 MOMS 220658 TABLE 7 (cootill0*4 CT ** 04 Mritl 4*4r44rt4(i) 4*4 table ) cu 4* ,tiH Mtkitiw (DUriM tt ttlrittlH TK 4* MnvlWlIl *4ttat4tt C t |w> 1t M trttttl It 4fc#4 IMlitlt 41 *4v4t |P44t4r thtt 3 t' tin 4* *4141*44 4* 4*Mtf Itttrvr*44*14* *4 144 M44 4nt|t4l 44t* IM4IM4 i t ** t !* tt*i l >4* OC /ft! htl*M4 4 *4 it|*i |1 44114 44*1 t * It 4 14*4' *44*11.*. 41 MOMS 220659 TABU a AKOUn or CHROKATOGRAPHABLE COMPOUNDS DETECTS) IN THE KETHTUNE chloride extract of the sediment duplicate sample, diluted ten tikes before analysis rt *.* 5.47 T. 40 * . U> 7. y. 7..4..* ; . . <r . 17 ; . <-o 4 .J* v. I,; T . *7 1. t 5 1 . 77 li-. 0* if. . ' Iv. * If. t 10. 'I 1# 7 **>. 7 l l. n .: 11.4V u.?.; 1I.7 li.t;. ; .. *'7 1 Sr. 11 i;.:i li.4t U.T i:. a li.v; 3.01 13. it i:. i \ 1J. li.K :i?i ov 1 I 44 v 14.474 1 109 it 74V) *v t7ii v II.UJ 45.154 44.07*. 1451 if ii.%*. 1 >2,4 44 30.!*< 4? 77 fV ft** W 45.744 r.t; w ;-*.** 23>* w 34. >41 vv *7.0?^ s*:7 vf 75.707 1 t 7 - J iv 114.(7 I'*4 7.. i* t::. ** w 2 t-*5 of fc, 7t; 4v 13;.7i; it: t w 4*. ('. ?u. *. w *74. '<? vv $**. on, ; V. 310.7*7 i: i vf 4.2.: 2*V1 4v 21*1: vv 4w 34, Ji* it.**.' ' * '>> w li.cl? 1 . * ' vH 1 * n** . i 1 44 4, 111 *:> iv 1 13. r*4 7JC3 w t>.nts 54-1 V4 44.754 -* 44 7.*<0* i'o ' it 3. t *4 If40 iv 33. 4>7 1*71 w ii. *\t> JO: 44 :4v 44 ;.?>4 3. 1* > >74 if 4.774 :**r. 4V >4.1*4 7*3 w 10.123 751 w 7.5*3 7T*4 vv 101.7J3 ;n Vf 7. 77- 4-17 iv vo 4.3.367 --nx-o*. CL?-tN!Xt -Oi 42 MOMS 220*40 TABLE 8 (continued) R1 t.ta 1 *>2V !*? U-7* ?s.v i*- >4. >4 16. .O 1- , M i iv J4 1 <' I-. >7 |7. JO i'.L i ii: 1 ". 4v 1 V61 it.:.. iv?? K> " l ' , I . i*.vi ;<. it LV *('4^4 Vh<+ 20, 4^ *o, r* :.<4r i r> :i. i* 2i.ll Li .U* 21**5 ;t.ti 21,*f 22,12 4* 22,92 22**5 22*2? 22*i? il.ti ai.oo U.II tl.u M(6 --/ 1202 V ts.au 205 V* tin r* 3.SC2 ro PV to.m 10447 w 133.400 T4 w Ot.0,2 rw V* 00 3.173 .MI 124*1 0 2 21? 25* *v 13,**-t 41.|33 3.734 ;i< v 5; 7 II r: ' M 3.103 .too :.i7` rt > IV 2 * w* 3.47* 3.440 II *.05* 770 4 J O * *.;* 3.334. 5X- VK *. Kt y 1 II .*** is-. * tv 11 .231 irv. ^ w 1 Ji.toi vv :z, 4-4 34 1 4.141 21 F 1* |/ 7J 1 S'? |v 4.04C 13.74.1 73. 74(< U'<l 1 4 * V I J.-4* V* 4 rr* II 24. V3.> 3.30 3.**l 4.047 ni*3 tv ?: 1 VV * v V4 i7,;ji 4. *7 * 5. or.: V 10.l*V 2rl vt jr>cj V 5545 w .7 3 vv 5l 4 6 w M** 'l '. vw cv-o v 5*1 IV 3,4*3 13.004 0.33 03.44* 3'.. 033 4.221 7.W. W v 10, *70 TCi M> 2.304 1540 II 11.070 40 33 3-430 514 M 0,3*3 M4 03 44.120 1U3 tv |7M V* 2024 V JvT* w 1*47 w 1044 w 14.21* 72.TOO 23.032 3t.44C >0.04.7 13.041 272| IV 5347 w 2034 w 30.040 00.333 24.031 43 MOMS 220661 : 2.`*4.. r4i ;?.4* 2;. 77 2:,t-. k* .!* ; * - -i ;V n . ;*. i _. \ * . ' r*. * ' m ' f*' . ?i 7r . ? < r..i: v .* Z- I;*.. i ;.. u . <. 4 . , 4 *.4 *. ; *. t J' ; `. 42 .t : - . r. ; ', - *:,, :7. < 2' . 1 7 ` . *" 4 :. , ; .t> :i.r C-'< sn.o;- i ,,i* 7'-, K. ; *I* >..K 30.3<> 30.41 30.73 k.tl 3i.3: 31. si, *7 33.1* tt.lt U*M tt.ll ... , * TABLE 8 (continued) M*4, **/ **: w 131* v* 1*33 V tn w 13.3*4 17.333 33.*13 n.ij* ** w 133.09* rv* IV 3:.** U> v* 3*1 M 7.1*0 2CO 1 V p* iTt l.tO W 30.3*0 i <r-fc vw 14 4 q2X ]; vi 14. %M tCC i*t 4?t* 7 * * k* : t fi io 1 iv 4.444 4. i}4 3.43V t-u 1 w 4.m 337 V* 4.301 4*4 11 3.. + 2T 1*4* w 10.4*4 71* V? v. in *.:i M 4. 130 if:< hJ ::. r? 174 w 33.111 11*3 w 17.474 1U *v r l>4 ii* if ' Vi 31.74* V* :.7t; *.J?i i* 7.;i4 2\ 1 . 41.14* ; * -V 24. >4*. W T* 6 :; .* . tii. M 4. S* T*.4* iv ?:. Jf41 w 34.0*4 I(,7l7 w io7.n* im; w 14.3V* T: c* f 3.*34 i y*> i* ) r. 7*4* *14 w 4.313 :v V* 3.033 w f* 3. *43 |6 4 3.. Sv 4*. '.'V *>* 4U> 41 33,174 SV k* 3.303 7*4 3.*2* Ml M a V MS w* 7.01* 3.3*4 10.337 :i*** IN 2770.Cl 1*3* V9 30.733 4*4 M 7.00T *? Ov 13*3 *v It. *31 *13* V* 109.0*0 3*0 M 3. an 3*9 M 3.30* J|4 P* 4.00? >610 6WOC*D10 Mmnceu 44 MOWS 220662 TABLE (continued) j:.a* rzr.i 3S.47 m 04 a.oio rov, to ' rs.rji 109 00 O.oio TO**l Ot* * 7*0*71 nuctiiin 0*t* riL(t *! Tvnu, - 0700.071 **m P*t* fiu< Wi MVTtl It.# #*-* .#*! I# HM'IlM ' *1*# C*I I 1 If . . . fli- #>.<> ... lkOlo. Yr.* ct.1#n* *#l.*c> ri itllWM t M bM|| #t tM 4f wi.MI 4' 6 (l.lri'll.' Ob'U Ml# lt^l 4* 4 * Mil'll Ibt'-O") l< lU4*> ! 1* tl) Oo#i ) *#*- . * L-. I'.f Of.' M.O'I *i*v*44 t* lb (hio* .! ill'.Jl* Jt 4>rtr4 o'# -M # * i'l '** |o'i<o**l* t (tMfuii.lt n)bl l *<; 4*4 b* * *0 #kr%%li" <##* feel' )*ik t*** * c * 41 i v*< b 2D0 M| t Mif |4**l# | od#d | # o4ii.o !*, lI'AO* |M|I iltl Iriclulll til C M #*t 'I (4#.yi-4 Mili kti| )AdiC* b*l**A T 000 iM i4'000 tor ( .. ( t !)./-( f 1.4 * k i.. 1< 4>>d i. h L (|i. b+ # 41 < I * ; vtti** *'.** tUlwrld* * *- tuUohi. Tl.* |l' 1 ? I** I** f i I | k V 1 1 Vt 6`<t t OOOoMflil i | (v , * r. o %r ) t* IW %<' > II *#*)> Mll U O'- " u4' <,*' .* l .f 4 4 14#l | (# I 0* t 4 1 6 1 o * W * I ># *4 ol #*. I ` # 4 4*1 I.| ,41 .r 14 v * tl.O k|l 1 ! lV /r , | f\4 #> t<r* It* ^"1 lulll.t*- .lit -4t.. Ill 4 * I #4 OK'i M 1 . 45 MOMS 220663 TABLE 9. TOTAL CONCENTRATIONS OF EXTRACTABLE COMPOUNDS PRESENT IN WATER AND SEDIMENT EXTRACTS. ANALYZED USING THREE DIFFERENT METHODS Total concentrations (yg/L for water sampler and vq/q for ______ sedieent samples)________ Extract identificationGC/FID GC/HS-total GC/MS-T? Influent baae/neutal extract 54.000 20,000 5,200 Influent acid extract 10,000 5.500 12,000 Effluent base/neutal extract Effluent acid extract 63.000 10.000 34.000 6,800 3.700 11,200 Effluent (duplicate) baae/neutal extract 65.000 36.000 3,900 Effluent (duplicate) acid extract 10,000 6,000 10,600 Sedieent extract 0,500 9,700 7,810 Sedieent (duplicate) extract ,B00 6,900 7,360 MOMS 220*64 TABU 10. PRIORITY POLLUTANT SCRXENIMC UEVRJ GC/NS Ctwil hrMlai 1ml. m/L krmlef level, IM/l ACld; fwifrcttwlf 2-Chlerophenol 2S 1 ,, I'OitlliriltMiM 10 2-Mitrephenel Phtnel 2.4-Obcethylphenol 2.4`Dichlerophenol 2S 1,4-Oichlereberuen* 10 2J Hemochl r*tUM 10 2J 1,2-Dichlerebeneea* it 2S Bit(2-ehlerieeprepyl) ether 10 2.4 C-Tnehlorophenol 2S Hezechlerobutediene to 4 .e-oinitro*o*cre*ol 2 4-0initrophenol 2JO 1.2,4-Trlchlerebeaeene 2 SO M*phthel*n* 10 10 g-Chloro-a-creiol 2S Bli(2-chlore*thyl> ether 10 Pen i echlorophertol 2S Heuchlerocyclepentedien* 10 4-Mitrophenol 2S HUrctMtlM 10 ll(2-chl*roethery) a*then* 10 2-Chloreaephthelen* 10 Chloroewthene 10 Acenaphthylene 10 01 ch 1 o r odi f 1uoreae thene 10 Acenephthen* 10 Iroaoew thene 10 Itophoren* 10 vinyl chloride OiUiNthu* 10 rluoren* 10 2,4`Olnltrotoluene 10 10 nethylene chloride 10 1.2-Diph*nylhydr*iia* 10 !> ichlorofluoroe* thene 10 2.4-Dinitroteluen* 10 1.l-Dichloroethylen* 10 M-ni t rotodipheny lee in* 10 1 1-Dlchloroethene 10 Hezechlorobeneen* 10 Trem-l,2-dichlOroethylene 10 4-Bronophenyl phenyl ether 10 CMoroforn 10 Phentnthr*n*/*nthr*c*n* 10 1. 2-0ichlorocthene 10 Dieethyl phthelete 10 1.1.1-Trichloroethene 10 Diethyl phthelete 10 Cerbon tetrechlonde 10 Fluoranthene 10 1 r oaodich 1 orone t hen* 10 pyrene 10 ItMchlereaethyl) ether 10 Di-n-butyl phthelete 10 1,2-Oichloropropen* 10 lent idine 10 Treni-1.3-dichl*roprop*n* 10 Butyl beneyl phthelete 10 Trichloroethylene 10 Chryeene 10 Dtbroaochleroaethene 10 Bie(2-ethylheKyl) phthelete 10 cii -1.3-dichleroprepene 10 Beni(e)enthrecene 10 1.1,2-Trichloroothen* 10 Beneolb)tluorenthen* 10 Benzene 10 ente(k)fluorenthen* 10 2-Chleroethyl etnyl ether 10 Beni*(*)pyrene 10 Broaofore 10 Ind*n*(1.2.3-cd)pyrene 2S Tetrechloroethylone 10 Dlb*nto(0.h)*nthreeene 2S 1.1,2.2-Tetreehloroethene 10 Ben>*(0,h.i>pery1enc 2S Toluene 10 M-NI t reediM thy lesiM 10 Chlorobenzene 10 K-ni treeedi-n-prepy 1 Mina 10 4-Chlorophenyl phenyl ether 10 Dlract laiecteblee: 3.3-Dieh1cretonneidine 10 teroltla 200 Di-n-ectyl phthelete 10 Acrylonitrile 100 47 HONS 220665 mu ii. scwning umi rot rtrriciDU/KB't EXTRACTABLE PRJOftlTY POLU/TAMTS compound Aldrin -6HC P-1HC y-BHC (lindane) 4-BHC Chlordane 4.4'-DDT 4,4'-DDE 4,4'-ODD Dieldrm Endosulfan I Endosulfan II Endosulfan sulfate Endrin Aroclor 1248 Aroclor 1260 Aroclor 1016 Toxaphene Methoxycftlor screens irratmii WMI M/TC 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 FOR VOLATILE ORGANIC PRIORITY POLLUTANTS IN WATER SAMPLES. q/L (ppb) Analyte Methylene chloride 1.l-trani-dlchloroethyleae 1.1-Dichloroethane Chloroform Diehlorobrononothane 1.1,1-Trlchloroethane Carbon tetrachloride Trichloroethylene lenten# ChiorodiBroanM thane Tetrachiereethylane Toluene Ithylbeaseae Chlorobensene ,, Blank NO* ND. <1? ND ND ND ND ND <10 ND <10 <10 <10 <10 Sanple ID 9:15 a.*, 10:23 as. 20 <10 <10 690 30 10 <10 <10 5,350 <10 <10 530 430 2.540 60 <10 <10 460 20 20 ND <10 6,020 <10 <10 710 460 2.660 1115 a*. 150 <10 <10 430 20 20 ND <10 5,900 <10 <10 1,000 380 2,560 *ND CMpcisd not, detected. rifnneifl observed, But was .below screening Uvol. 48 MWS 220666 TABLE 13. ANALYTICAL RESULTS FOR EXTRACTABLE ORGANIC PRIORITY POLLUTANTS IN WATER SAMPLES, tig/L (ppb) Analyte Base 'neutral Blank Sample ID Influent Effluent Effluent duplicate 1. 3-Dichl^rObemer.e 1.4-Dichlorobenzene 1.2-Dichlorobenzene Kapthalene Diethyl phthalate Di-n-butyl phthalate Butylbenryl phthalate Bis(2-ethylhexyl) phthalate Di-n-octvl phthalate Phenanthre.ne Anthracene Fluoranthene Fyrene NO* NO NO NDb < 10B < 10 NO <10 ND < 10 < 10 < 10 < 10 60 720 700 S30 ND 10 2.990 ao 70 ND ND ND ND 70 970 1.290 3S0 <10 <10 1,040 <10 ND <10 < 10 ND ND 70 1.000 1.3S0 380 < 10 < 10 1,070 <10 ND < 10 <10 ND ND Acid 2-Chlorophenol 2-Nitrophencl Phenol 2,4-Dichlorophanol 2,4,6-Trichlorophanol Pentachlorophenol 4-Nitrophenol NO 160 ND 2,790 <2S 17S ND 390 ND 960 ND 30 ND 4.380 290 4,760 130 1.200 1,250 <25 3,580 260 4.470 110 1.090 1,110 <25 3.540 aKD - compound not detected. b,,<" - compound observed, but vat below screening level. 49 NOUS 220667 TABU 14. ANALYTICAL RESULTS FOB BCTMCTABU ORGANIC PRIORITY POLLUTANTS IN SEDIMENT SAMPLES, vfl/g (ppa) Analyte 1.3-Dichlorobenzene 1.4-Dichlorobenzene 1,2-Dichlorobenzene Napthelene Di-n-butyl phthelate Butylbenzyl phthelate Di-n-octyl phthelate lemole 16 ---------- Sludge 51 udofc duplicaTe 20 240 330 70 30 7.100 20 10 140 240 60 20 6.420 30 TABLE IS. QUALITY CONTROL DATA FOB ORGANIC PRIORITY POLLUTANT ANALYSIS OF WATER SAMPLES Spike* Dichlorobenzene-d, Phenol-ds Pyrene-d,o Chrysene-d,2 Sample IP, percent recovery Effluent Blank Influent Effluent duplicate 66 56 88 80 39 28 30 26 117 29 20 21 64 31 73 82 *SFike - 100 v9/L TABLE 16. QUALITY CONTROL DATA FOR ORGANIC PRIORITY POLLUTANT ANALYSIS OF SEDIMENT SAMPLE Spike* Dichlorobenzene-d4 Phenol-d Pyrene-d,0 Chryaene-d,t Semple ID. percent recovery Sediment Sediment duplicate S3 SO S3 39 S3 64 49 63 *Soike Uvtl Sediment - 147 tiq/q Sediment duplicate * 14S vq/q. SO MOMS 220668 TABLE 17. NOW-PRIORITY POLLUTANT ORGANIC COMPOUNDS DETECTED IN THREE VOLATILE SAMPLES FROM SAUGET TREATMENT PLANT RT (aim) i.( 11.4 15-5 IT. 1 2: s 22.0 is 9 316 16 6 18.0 19. S Tentative identification** Unknown (44. 41. 42, 41 )C Unknown (56. 41. 41. 19) Acetone Unknown (4 5, 41. 69) Methvl ethyl ketone Unknown (41, 42. 41) Methyl ncbutyl ketone Unknown (41, 68, 57, 69) Unknown (81. 41. 154, 108) Sent aldehyde Xylene-Home r Concentration* (uo/Ll Sample identification 9:15 a.m. 10)21 .m. ll: IS a.m 1 NO 17 29 1 8 86 17 22 55 890 1 4 1) 70 4 29 170 18 44 81 850 NDd ND 24 15 8 10 98 47 21 11 670 Estimated concentration bated on the area of the major ion of the identified compound to the major ion area of benxene*d. internal atandard. ^Tentative identification, not confirmed with authentic etandarda. Major mattea of unknown compounda are liated in partntheete according to decreasing intenaitivea. detection limit it 1 pg/L. 51 NONS 220669 TABLE 18. IDENTIFICATION OF MAJOR EXTRACTABLE ORCANJC COMPOUNDS IN THE BASE/NETURAL EXTRACT OF THE METHOD BLANK' Retention Peek time. Ho min Compound (mar >tin) Internal itandard^ 2 11.18 Anthracene-d,, Amount Amount Peak area, detected, iptked. percent total count* ua/L pa/l recovery iooot too kecovery atandardC,d 1 7 81 1, 2-Diehlorotwntene*d, : 2S 42 Pyrene>d|o 4 28 27 Chryene-d(I ienj Organic* detected Hone detected 278S84 424101 187081 44 100 44 0 in 100 m.o 44 100 44 0 TOTAL CONCENTRATION *Includta all aubateacaa that war* found at or above a 5\ threthold on the BATOt peak identification program in the Havlett*Packard ayaten, corresponding te a detection of limit of 2 pg/L. bAnthrac*M-d)a Internal atandard added UMdietely prior to analyaii; SO ng/L injected eguivalent to 100 pg/L in driginal aample. cDatarated recovery atandard (aplfeaj, added ta original aanpla before extraction ^Quantitated relative ta area af major Ion far authentic atandard. MONS 220670 TABLE 19, IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE ACID EXTRACT OF THE METHOD BLANK'' PeAll No Retention line , in Conoound (najor *e*ae*l Internal atencUrd** Aaount Peal Art*, de tected tOtA) COHflf I ___ >*9/L - -- Amount tpil*d. Percent P9'1- f tcovry 2 21.2B Anthracene-dl(i noon ioo 1 6.70 Phenol *d* 19178 39 100 J9JJ ________________ Organic* detected Nona detected TOTAL CONCENTRATION 0Include* oil aubetoncee that vere found at or above a 5\ threthold on the BATQ< peak identification progrea in the Movie tt 'Packard eye ten. corresponding to o detection of Unit of 2 pg/L. ^Anthrocotwdta internal atandard added taediately prior to onaiyei*; SO ng/L injected equivalent to 100 M9/L in original eoNple. cDewtarated recovery atandard (spike). added to original *^l* before cetraction. Quantitated relative to area of najor ion for authentic atandard. MOMS 220671 TABLE 20. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE BASE/NEUTRAL . EXTRACT OF THE INFLUENT SAMPI.E, DILUTED 1:10. NOT CORRECTED FOR BACKGROUND0'6 Retention Peek line, No .einCompound (o]or eitei) Internet *tendrdc 24 21.27 knthrecene-dio Peek .ire. totel conntt Aao'int detected, Anount ipikrd. pq/L Percent. recovery IS2040 1000 1 ,2*0ichlorobenzene-d Pyrene-dm Chrytene-du Oroenice detected f,q,h. 1 2.22 Chlorobenzene 2 1.73 Xylene (leaner) 2 4.32 Xylene (itoner> 4 0.08 Oeiualdehyde end Cj-benzene (itoreer) S S.S8 Aniline 8 8.40 Cj-benzene (leaner) 7 7.33 Dichlorobentene (leaner) S4 100 S6.0 24 100 24.0 11 100 11.0 181187 144084 71887 171254 411008 113540 1388S3 5.1 * 10* 42 R 10J 2.0 R 10J 4.4 R 10* 1.2 R 10* 12 R 10* 3.4 R 10* (coniinued) MOMS 220*72 TABI.E 20 (continued) elanlion Peak lime, No. nin Compound (]or masses) Organics detected {connnued) a 9 10 u 12 11 14 IS It IT 11 19 20* 20b 21 22 21 24 2S 2t 7 47 7.58 7 70 7.87 8.02 9 13 10 10 11.23 11. S7 11.68 12.20 12.4? 12. tO 14.1 IS. 11 1S.M 1S.SS 1S.S? is.to 30.43 Unknown (111.12S.1S4. 71) C3-bntene (isomer) C4-benaene (isomer) Dichlorobenzene (isomer) amyl alcohol Unknown (119,121.117.93.91) Chloroaniline (nomer) Naphthalene and/or atulene and/or Unknown (91.I48.lt!.92) Chloroanilin* (isomer) Chloronitrobentene (iaomer) Chloronitrobenaene (Iaomer) Chloronitrobentene (iaomer) N-phenyl formamide Dichloronitrobentene (iiomer) Dichloronitrobeiuene (isomer) Nltroaniline (isomer) Nitroaniline (isomer) Nltroaniline (isomer) C|0'alkene or cycloalkane isomer Amount Amount Peak area, detected, spiked. total counts __ _______ PO/L Prrr^nt recovery 450^2 17 707 S88111 411639 262696 36927 14S42S 114324 2SS942 42047 41779 99S000 477200 16S8S8 434779 101830 774189 1229S 21936 66006 1.3* 10* SO 1.7 a 101 1.2 a 10-' 7 4 a 10* 1.0 a 10* 4.1 a 10* 3.2 a 10* 72 a 10* 1.2 a 102 1.2 a 10* 21 a 109 1.4 a 109 4,7 a 10* 1.2 a 109 2.9 a 10* 2.2 a 109 3S 62 1.9 a 10* (continued) NOUS 220673 TABLE 20 (continued) Retention Peak tine. Wo.sunConoound (na]or nesses) Orpamca detected (continued) 27 18.73 Ni troaniline 28 20.28 C*-phenol 30 24.S2 Sulfur (Sh) 31 28. IS Butyl benayl phthalate TOTAL CONCENTRATION1 P*k area. tl_r_?l'n ' ' A*oum detected. lip/L Amount spik*d. Percent i'q/Lrecovery I7225J 4M44 104111 577042 4 1 * 10* 2 0 a JO* )1 x 10* 1 6 * 10J 20 0 x 103 aFor background, ace nethod blank analyttt. Table 18. ** Include a all aubatancea that wera found at or above a 5% threahold on the BATCH peak identification m progran in the H*vlattFackard aya ten. correeponding to a detection of Unit of 1O0 ug/L. CAnthracene*dlv internal atandard added Mediately prior to analyaii. SO nq/L injected equivalent to 1000 pg/L in original aanple. Seutarated recovery atandard (apike), added to original aanple before extraction 'Quantitated relative to area bf najor ion for authentic atandard. f>atiaatad concentration baaed on area of total ion relative to that of anthracene-dm. internal atandard. ^Tentative identification, not confirmed with authentic atandarde. Stajor naaaea of unknown co^ounda are liated in perentheaea according to decreasing intenaities. Poealbla aolacular Iona are underlined. . ^Suanatlon of concentrationa of detected coa^ounda, excluding atandarde. ' HOWS 220674 TABLE 21 . 1 DENT I FI CAT!ON OF MAJOR FXTRACTAPLF ORGANIC (-rWOirNDP IN THE ACID EXTRACT OF THE INFLUENT SAMn.F.. DILUTED 1:10, NOT CORRECTED FOR BACKGROUND*' D Pt*k No Rtltntion ti*. win______________ Compound (aoior m| Internal ttanrixrd6 10 21.28 Anthr*c*nA-d|,, Apmiinl <rA. dM*ctd. toll coiinn |iq/L Amount spiked, _|ig/L Prc*nt rotavtrv 431021 1000 ( A || Organic* detected 1 8.00 Oenteneiwthanol 2-3 10.2S Nitrophonol ltoatr 4 10.82 Dichloroptwnol nootr S 11.8S Mixture of 2S\ dichlorophenol ltower and 7S% chlorophenol nootr 4 14.02 Cl-touttlitlnq unknown (121,43.44,173) 7 14.SO Trichlorophenol lutir 114148 1124444 100080 133442 128434 3S7472 28 100 28 0 3 6 x to1 2 4 x 101 2 3 x 10' 3 1 x 10* 3 0 x 10* 8.3 x 10* (continued) HONS 220675 TABU ?l (continued) Retention Mk tiK HoxinCompound (m]or mh> Pe-'k re. lei.'I co'ints Amount Amount di**r*cted. spiked. Percent pq/Lpq/L recovery 6 it 02 Cl ;*eont*ining unknown l 207 70**.97.lilt 4 17 t] Ni*rophenol iiowt TOTAL CONCEWTRAT1OH1 4M27 117644 | I H 10: 7 4 K 10* S.S n I01 *for background. see oethod bltnk analysis, T*ble 19. ^Includes til substances that were found at or above a S\ threshold on the 8ATCH peek identif.'cation progran in the Hewlett-Packard lyiteo. corresponding to detection of liait of 60 i>g/L. eAnthrscene*d(o internel stsndsrd sdded iseaediately prior to analysis,- SO wg/L injected equivalent to 1000 ug/L in oriqinel teople, **Deuterated recovery standerd (spike), added to original staple before extraction. 'Quantitated relative to area of najor ion for suthentic standard. ftstiaated concentration based on area of total ion relative to that of anthracene*d|0. internal standard. ^Tentative Identification, not confined with authentic standards. ^lajor oattes of unknown cenpomds are listed in parentheses according to decreasing intensities, fosaihla aolecular ions are underlined. SiMMtion of concent rat Iona of detacted co^ounda, excluding standards. MOMS 220*76 TABLE 22. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE BASE/NEUTRAL EXTRACT OF THE EFFLUENT SAMPLE. DILUTED 1:10, not corrected for BACKGROUND'1 Retention Ptik NO . t i*e. mm Compound tajor nesses) Internal standard 21 21 26 Anlhracene*d|0 Peak area, total counts Amount tlf tct ed, 1`9'L Amount spiked. pg/l percent recovery 1000 _ . Recovery standard*1'* 1.2*Dichlorobenz*ne-d4 pyrene-d|U Chryiene-d,} vO Organic* detected*'^'1* 1 3.2S ChloroOeniene 2 3 77 lylen* (iiwr) 3 4.37 Xylene (leaner) 4 i-12 Mixture Of 11% benteldehyde and S% <r3-beniane (1toner) S 6 63 Aniline 6 6 12 Cj'bentene (iiooer) 66 100 88 0 20 too 20.0 7j too M 0 423601 230111 12S041 216071 S774SO 170110 1 1 10* 6.1 x 10* III 10* Ml 10* 1 S K 10* 4 S K 10* (continued) MONS 220677 hit Mo Retention liar. in Compound (major maims) Organics detected (continued) 7 7 3) 01ehlorotten*ene (isomer) a 7 SO Unknown (ill .125,154.7)) 0 7 70 C4-beniene (isomer) 10 7.aa Olchlorobenzene (isomer) IJ a.oa tnzyl klconol 12 10.12 S0\ Propyl benzene and S0\ ehloroamlint (isomer) )J U 21 Naphthalene and/or azulene and/or isoawr 14 II to Unknown (01.I48.lt3.42) IS II.ts Nmtura of 47% chloroaniline (isoawr) and 33% chlorophenol (isomer) It 12.20 Chloronitrohentene 1f t 12.ta Chloronitrobeuene (isomer) 11 0A 1* 12. tS Chloronitrobentene (isomer) 20 14 12 Mixture of 80% N*phenyl fonaamide and 20% wkAown (151.153) 21 is.ia Pichloronitroheniene (isoemr) 22 IS 37 Oichloronitrobenaene (isomer) 23* 25 IS.S3 Nitrooniline (isomer) Peak area. total counts Amount Amount detected. spiked, PQ/l -- Percent recovery 367403 1440k 3 403485 847373 7(0824 357005 121408 825704 142507 124tt0 2210187 1107670 577204 st2tea 46023 1340050 1 .0 a 10* 3.8 k 10* 1 3 x 10* 2 3 n 10* 1 0 r. 10* 0.5 x 10* 3 2 x 10* 2 2 a 10* 3 6x 10* 3 3 x 10* SO x 10* 2.0 10* 15 x 10* 1.5 x 10* II X 10* It X 10* (continued) MOMS 220676 TAPl.p 22 (rontinuM j Peak No Am pm i on in". min Compound (>jcf m.sssesj^ Organics Jnectnl [umi MninU 24 16 as Chlorom t roam 1 me (isower) 27 16.57 Et hoxym i robenrene (isomer) 28 18 7 1 Nitroam 1 me (isomer) 10 28 11 Butyl henryl phthalale TOTAL COHCEWTRAT1 OH1 Amoun t Amount P' 'll ara d*leci*d. spik'd, Percent total counts y<|/L yq/L ffcovfry 66}61 91666 487624 1214 n 1 8 K I01 2 4 it 10* ' 1 * 101 8 6 10* 14 0 * io-1 4For background, see nethod blank analysis Tabic 18 blncludes all substances that were found at or above a 6\ threshold on the BATCH peak identification progran in the Hewlett-Packard syslen, corresponding tc a detection of limit of 200 pg/l. CAnthracene-d,0 internal standard added immediately prior to analysis, SO ng/l. injected equivalent to 1000 pg/L in original taaple. ^Oeulerated recovery standard (spike), add'd to original sample before eatraction *9uantitated relative to area of M)or ion for authentic standard *IstiMted concentration based on area of total ion relative to that of anthracene-d10, internal standard. ^Tentative identification, not confiroed with authentic atandards. Ntajor oassei of unknown compounds are liated in parentheaea according to decreasing intensities, possible salecular ions are uniter lined. !sMUn Jki I'unin' rati ins of detected ce^cnasda eacludinc standards MOMS 220679 TABLE 23. I DENT ! FI CAT l ON OF MA.IOR EXTRACTABLE r'Rr.AN IC COMPOUNDS IN THE ACID EXTRACT OF THE EFFLUENT SAMFLF., DILUTED I 10. NOT CORA FC'TF.L) FOR BACKGROUND ' Hfienltoo Peak iia*. NoNinCompound (*jnr_n*<ss ____________ Internal standard^ 10 21 24 Anthrc*n*-dh,, Amount Peak ara dtct*d, i9J_11 _c *jg/L_pq/L Amount tpiktd. Pftc-nl rectvc ry 41 SOU 1000 phtnoi-d* Organic! detected*' 1 4.77 Chlorophenol isoawr 2 6 00 OeiueftMMthenol 3 I0.2S Nitropheiwl iu*tr 4 10.42 Oichlorophenol itoawr S 11.44 Mixture of 2S\ dichlorophenoliioaer and 7S\ cMorophenal itoaer 4 14.03 Cl-cntaining unknown (121,43.44.173) 7 14.42 Trichlorophenol ii*tr 30 100 10.0 61141 174066 420424 370134 343470 142132 470441 2.0 x 10* 4.2 * 10* 2.2 x 10* 6.4 x 10* 64 x 10* 4 4 x 10* 1.1 X 10* (continued) NONS 220660 rttk No Itnlion win TAHL.r 33 (continued) CompQgnd fw*jorjiMsm i 'k itn tot 1 ^ Awonril dtrc1*rt <g/L Amount ipiked. tjq/L Ptr-ent recovery 6 16 02 Clj*contiininq unknown (107,y7 io9.I 33) b 17 62 Nitrophenol isoaer TOTAL rOMCEWTlUTlOM* * 2 MO 2J'/,r.J 6 6 x | O'1 Vor background, see ethod blink inilysis, Table lb bIncludeI ill substances that wort fourd it or above i 6\ threshold on the SATCM pt)k identification propria in th Hcvlett*Pickard systea. corresponding to i detection of liail of 70 ug/L. cAnthracene*dto Internal standard iddtd innediitely prior to analysis. 60 ng/L injected equivalent to 1000 pg/L in original pic. ' ^Deuteraled recovery ttindlrd (spike), idded to original sample before direction *<hjant i tated relitive to irei of Bijor ion for authentic standard. ^EtiLMted concentntion blied on irei of totcl ion relitive to thet of amhrae*n*-d|0. interncl stindird. `^Tentative identiflcition, not confirmed with authentic stindird*. Ntejor lists of unknown compounds ire listed in pirentheses according to decreasing intensities, rotsibl* Boleculir ion* art underlined. ^Suwalion of coneentrationi of detected compound*, excluding stindird*. MOMS 220661 TABLE 24. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE BASE/NEUTRAL EXTRACT OF THE EFFLUENT DUPLICATE SAMPLE. DILUTED 1:10. NOT CORRECTED FOR BACKGROUND0 pfik Mo Detent ion time. in Compound (a* lor aes^es) Internet stend*rdc 2a 2t 2a Anthncene-d!0 Peek ere*. tol.i) cotmt s Amount fWeCtfd J'O/L Amount spiked. l/Q/ L Percent r*rov#ry J6I2S8 1000 Recovery etenderd^* 1.2-Dichloro6en*ene-d pyrene*d,0 rhry*ene-dl7 ao ioo ao o :i ioo 2i.o 62 100 62.0 Orqnic detected*'^,h____________ i 3 23 ChloroPenxene 2 3.76 Xylene (ixaxer) 3 4.31 Xylene (lMnr) 4 6.10 Mixture of 63% benseldehyde end S% C]*ben*ene (leaser) S 6.63 Aniline 3444S4 226741 1S3266 23S243 603662 ti * 10* 6 3 x 10* 42 x 10* 6.S 10* 1 7 x 10* (continued) MOMS 2206A2 table 24 (continued) Peek No trim! ion t ime. in COWDOUnd (M410t ***fi) Organic* detected (continued) Ajnmjn l Peek ir't. dr I e :*d. total count $ ___ CS'L Amount *pikd. 6 t. 42 C,-bensene (irtmer) 7 7 3S liichjorotienzene (isoe*r> 21 IS]3 141036 S 9 N 10: 9 S n I0J a 7 72 (isomer) SOI 962 1 4 % 10' 9 7 IS Oirhtorobenzene (isomer) 82420? 2 3 K 101 10 e to Benzyl olcohol 740664 2 L n I01 11 10 12 Mixture of 70\ chjorosm) me (isomer) and J0\ unknown (9|.120.133 .1 14 ) 3SS9IS 9 9 n. I0r 12 11 23 Nzphthelene nd/or izulene and/or isomer 126060 J *, x 10! n 11 SI Unknown {91.141,163,92) BIS'00 2 3 X 101 14 11.70 Mixture of 70\ chloroenilme (isomer) end > 30\ chlorophenol (isomer) 134768 3 7 K 3 0* IS 12 22 Chloronitrobentene (isomer) 13ISS6 3 6 K 101 it 12 S3 Chloronitrobenzene (isomer) 23P029 6 4 N 10J 17 t Hi lib if 20 12.IS 14.1 IS. 20 IS 37 Chloronitrobenzene (isomer) N-phenyl formemide Oichloronitrobeniene (isomer) Dichloronitrobenzene (isomer) 1169099 S91344 S9B0S7 72967 3 2 K ,0? 1 .6 N 10' 1 7 10? 2 0 K 10* 21- 24 1S.SS Nitrosnlline 1392402 3 9 * I01 (continued) HONS 220663 TABLF 21 (continued) ietention peak tio**, HO CoOund iy r) Organic* detected (cori ijjufdl 2S 16.46 Chi or on it roam line 26 16 67 tlhoxymtrobenzene 27 16 60 Nltroaniline and S', chloromtroani 1 inr 29 26 13 Butyl benzyl phthalatr Peak urea f Ot A 1 count ' Amount Amount d*tec ted. spiked. J'9' L . ..... pg/L Percent r*eovf ry 67294 904 J 7 460I9S J244S6 1 9 * 10* 2 S x 10? 1 1 1 I01 90 x 10* TOTAL COMCnmUTIOM1 IS 7 10* *For background, see ate thod blonk analysis. Table IS ^Include* *11 substances that were found at or above a S\ threshold on th BATCH peak identification progro* In the Hewlett-Packard ayateo, corresponding to a detection of ltoit of 200 tig/L. cknthracerve*d,0 internal standard added laawdiately prior to analysis; SO ng/L injected eguivelent to 1000 Mg/L in original teazle. `Seutented recovery atandard (spike), added to original aaople before extraction. *Quantitated relative to area of najor ion for authentic atandard. flstiaated concentration baaed on area of total ion relative to that of anthracene-djo, internal atandard. ^Tentative identification, not confirmed with authentic standards. Stajor M*aea of wiknom eopowda or* listed in parentheae* according to decreasing intensities. Possible molecular ions are totderlined. *SuMtion of concentrations of detected coa^ounda. excluding atandard* MOMS 220664 TABLE 2S. IDENTIFICATION OF MAJOR EXTRACTABLE ORGANIC COMPOUNDS IN THE ACID EXTRACT OF THE EFFLUENT DUPLICATE SAMPLE. DILUTED 1:10, NOT CORRECTED FOR BACKGROUND*'D Petk No Re tent ion t IM . in Compound (i*ior **sses) lutcrnol n*nd*rjc 10 21 2B Anthr4en*-d,,, A/noun t detected. total counts ___ pg *woiint Spiked. im/L Pf rc f JU recovery 42MS8 |00i Rtcovtry standardd. Phenol-d,. I ,2-0lchlofot>nttn*-d< Pyrei-dt0 o> Chry**n-dti 2fc 100 2b 0 i b. 77 Chlorophenol itmr 2 7.44 ttniencae thanol 3 10.23 Nitrophenol itoatr 4 10.92 DicMoroptonol iioaer S 11. bS mature of 2S\ dlchlorophonol itouer ond 7S\ chlorophenol iiowr 4042b 130218 841SS2 311311 1249S0 14 10* 3 1 10* 20 n to1 7.8 N 10* 7 .6 K 10* (continued) MOMS 220645 TABLE 25 (continued) Peak No Relention tlM, in Compound (major misses) Or domes detected (continued) 6 14 OS cl-contsininq unknown (121,73.66.171) T 14 S2 Trlchlorophenol isomer 8 lb 02 Clj-eonlaintnq unknown (201.97 133.209) 9 17 (.2 Nitrophenol isomer TOTAL CONCENTRATION1 Peak area. total counts AffOUlU detected. I'O/L Amount spiked, mq/L Ptrcfnt rtcov*n 193047 416S9S 34)61 24IS21 oPm IT r-m k/1 15 101 It a 101 81 6 0 x 103 *for background. k( method bUnk analysis, Tablr t9 ''includes *11 tub*tenet* th*t vtrt found *t or above a S\ threshold on the BATCH peak identification program in the Hewlett-Packard system. corresponding.to a detection of limit of 70 yg/L. cAnthracene-d|0 internal (tandard added immediately prior to analysis, SO mq/L injected equivalent to 1000 yg/L m original sample Seuterated recovery (tandard (spike), added to original sample before entraction. `quantitated relative to area of aa]or ion for authentic standard. ^Istiaeted concentration based on are* of total ion relative to that of *nthr*cene-d|e. internal standard. ^Tentative identification, not confirmed with authentic standards. Nlajor nasses of unknown compounds are listed in parentheses according to decreasing intensities. Possible Bolecular ions are wderlined. ^SiaMation of concentrations of detected co^ounds, deluding standards. HONS 220686 TABLE 26. IDENTIFICATION OF MAJOR EXTRACTABLE COMPOUNDS IN THE METHYLENE CHLORIDE EXTRACT OE THE SEDIMENT SAMPLE, DILUTED 1:10, NOT CORRECTED EOR RACKOROHMD'1 kr < nt i on Pp*k Hw. MoinCo*poiind (mijor >uti) Amnunt r'>k ,<rv d'l-ctfd Iot *_t__ count a/q IntrrnAl AtanrlArd^___________________ Amount spik'd. nq/q Prrcrnt recovery 74 21 IS Anthr*crn**d,,, 1SS680 SIS 4 6.S8 Phenol-d<, 8b 7.7 1.2-Dichlorobfnttne-d^ 10 2S.2S Pyrerw-dl0 * 40 28.10 Chryene-d,t * Orqonici dotocted*11 q 8674 JS6JO 18800 11207 l J 62 1.4-Dinethytbeniene (isomer) 2 S S3 licye10(2.2.1(hoptene .2.2-dioethyl-l- 1 )S62 ethylene or licyclo(3.l.l|hopt-2-ene,2,6,6-tri*thyl- cyeloheierw.S-ethyl-)-( 1 -ethylethenyl)-. trtiu-(-) 11247 88 187 S) 0 88 187 5J .0 88 187 5J.2 82 187 48.0 SO 66 (continued) HONS 220687 TARLF! (continurd) p*k NO ktltnlion Amount Amount U. Ta.H arf,1 d-tfCtrd, spikrd. Prrernt PinCompound (n*]Of sma-.aa)loti ] jrtrnnM______________________ i,9/3u<t/Q rrcoyrry Orgonics dttrctrd (tontmurd) 3 S 9S Ci-btniK* (isowr) or 1 , 3-cyclopontidiw* , S- (l -mothylpropyl idrn# ) 1 3927 5 4.7] C-|-bni*n (ite*r) 6 7.20 Dichlorobtnttnt (isoner) 24832 31070 7 7.S7 CfbrnHM (iioittr) 249691 ll 7 63 80% C4-bciu*ne (itowr) ond 20% unknown <43,107.121.134) 71340 8b 7.7 30V Clt-b*nien* (ttoarr) *nd 70% Ctj-btnrrwd, spiking ttsndAid 3S670 9 4.00 SOX C-6*ni*n* (isoowr) <nd $0% unknown <104.93.107.136) 12172 to 10.62 Unknown (tS2,87,SS.tS4) 9322 11 11. to 8icyclo(4.4.1Jundoes-1,3.S,7.9-p*nt**n- Il-on snd/or nophthoitn* 9181 12 12.27 Chloroni tro-b*nzn (isoorr) 11 12.42 Chloronitro-bonitM (nestr) 2S310 8718 14 IS.03 Dichloronitroboiutnc (isoorr) 2122S IS 14.47 Unknown (87,68.83.70,134) 14 IS. 07 Unknown (83.87,48.111.70) 3677 6360 17 IS.30 Unknown (87,83.111.64) IS 14 . S7 Unknown (97,83,111.69) 7743 4S4I 82 1.5s 101 t a * to* 1 5 s to' 4 2 A 10* 2 1 A 101 7| SS S4 15 s I01 SI 1.3 I01 22 37 46 27 (cont iniicdj MOMS 220688 TAP.l.r 26 (continued) Ptok Ho Rflrnlton tin*, inCompound (wjot Organic detected ^continued) (4 20 02 Ph*nol.4l-(|.l.3.3-letr ameUsy (but y 1) 20 20 13 Nonyl phenol (isomer) 21 20 27 Nonyl phenol (iSOmrr) 22* 20* unknown (ns. 107. i2i m) 22b 20. SO Unknown (41.210,121,85.I 07) 22c 20 S Unknown (144.107.41.121) 23 20 47 Unknown (135.107,134.41) 2S 23 S7 Unknown (41.114.134.(47) 2b 23 40 Unknown (134.47,83.41> 27 24.08 Unknown 2t 24.3S Sulfur, oleculer {S() 24 24.40 unknown (ISO,47.81,144) 11 25.17 Unknown (41.10S.1S0) 32 24.50 Unknown Ikyl ben*ene <105.104.41) 31 24.88 BenieiMaine ,4-nitro-N-phenyl - 14 27.41 Unknown (41.11S.144.114.Ill) IS 27 88 Unknown (41.144,147) 34- 17 28. D1 Unknown phthl4te (144.41,204, ISO) Amount P'*k <rn d-t-tird. tat a l_ c d in t Ai.q/q Amount ipik-d. krrcfni tiq/qrecovery M'>2 fi'81 *?i til !4 2760 5184 3857 441 t 10445 8845 4877 4744 4037 44(7 34(3 3534 448424 17 45 .k 1L 44 16 31 2) 24 65 52 24 28 34 34 21 21 57 a (0J {continu'd) HONS 220689 TABLE 26 (continued) oitntion num Mount Pn* tino. P**k trt*. dettcted, tpikrd. Percent MoMinCompound <*)or !?>*)^oj .1 l_coimM____________________________________________ |iq/q|iq/q recovery 38 28 32 Unknown (91.119.10S,133 ) 39 28.73 Unknown Alkyl benien* (ICS.106.91) 41 32.08 Unknown phthalate (149.107.91.207) TOTAL COHCEWTMTIOH** 2849 994) S794 J7 59 34 9,7 |0 J * I nc 1 ud** oil tubotonco* thot wort found ot or obovo t 0 i\ tltrothold on the MTQt p**k identification progroo in the Mewi*tt*P*ck*rd tyttoo. corrttponding to * detection of linit of 10 wg/g. ^knthr*e*no-d)o intornol ttondord oddod Iwtdittdy prior to onolytif: SO ng/L injected equlvolent to 915 M4/9 in onginol tonple. cDeuteroted recovery ttondord (tpike), oddod to originol tonple bo for* correction. dQuontitet*d relative to oroo of nojor ion for authentic ttondord. *IitlMt*d concentration boood on oroo of totol ion relative to thot of *nthroc*ne-d,0. int*rnol ttondord. Sentetlve idontificotion, not confirmed with outhontie ttondord* ^tojor MiMi of unknown conpourtd* or* listed in poronthotot according to decreasing int*ntiti*t. Possible ooloculor ion* or* tatderlined- Ntanetion of concontrotion* of dotocttd co^oundt. excluding ttondordt HONS 220690 TABLE 2 7 I PENT 1 f l CAT I ON OF MAJOR EXTRACTABLE or, M|-r,i;Nr,c IN THE MFTHVLFhE CHLORIDE EXTRACT Of THE PEDIMENT DUEL,! C.ATI. |.AMPLE. DILUTED 1 10, NOT CORRECTED Fok BACH I -HOUND Pr*k No. ReIention tlM in Compound (nnnor nastM) I nternel it end^rd1' 21 2113 Anlhrecene-d,,, Peik *r*v lotkl counts A/nO'll, t detected. |iq/q Amount. spik'd. Percent recove r y P1407 725 Recovery st.snd.irdC ^ 4 Mt Phenol-ds 8 7.57 1,2*0ichlorobrntene*d 3S 25 25 Pyrene-d10 4So 24.10 Chry**n*-d|? 1 3 62 2 s.ss ] 5.45 5 6.75 6 7 18 7 7 S3 9 8.38 to* 9.00 10b 9. 1 tl 11.63 12 11.08 ffg Orwnict detected ` (S** previous t*ble for compound identifications) 8575 887)8 24681 16423 73 145 50 0 57 145 34 0 43 145 64.0 41 145 63 0 10472 8604 10654 28990 42636 266215 7 364 14848 19848 13516 8543 44 36 45 1.2 * 10* 1 8 K 10* I I ii 10* 31 84 84 57 36 (continued) MOMS 220691 TABLE 27 (continued} (tent ion Peak time. No.ain_______________ _Compound (ie*ior ***e_ijtola! count' a'** Organic* detected (continued) 13 12 25 14 12.40 15 15.02 14 14 45 17 18-07 IS 18 30 14 18.42 20 18 57 21 14.88 22 20.02 23 20.12 24 20 27 25 20.50 14 20.47 27 21.02 28 22.87 30 23, ST 31 23.00 32 24.OS 33 24.33 34 24.88 34 25.38 37 as. ss 38 2S 73 38 24.50 40 24.88 41 27.4S (Set previou* table for compound identification*) 2454A 4775 3208b 4434 8448 8247 4118 7727 2701 8040 18718 11118 5277 4142 1583 4080 4758 2287 14737 5187 15348 8231 5034 3111 8585 1200 10248 Amount d*tect-d. l`<3/g Amount pik*d. ug/g Percent recovery 1 2 * tO1 41 1 4 m 101 27 38 38 17 33 14 34 74 47 22 24 7 24 24 10 42 22 45 14 21 14 40 5 43 (continued! MONS 220492 TABLE 27 (continued) Retention Peek time, NoinCoupon n d (m ]or m y <> * )1 o lji 1 _r minn Peek ere. Amount dtpried ti<j Amount spik*d. ,iq/g Percent rer ni>rj 42 27 90 (See previous table for compound i den 11 f ica 11011* ) 43 A 28.OS- 44 28 08 4S 28 32 44 28 S3 47 28.73 48b 29 2 48c 29 2 49 32 07 h wj TOTAL COHCEWTMTIOK 2018 1406794 4897 4118 USS3 20 S3 20S3 9124 9 S 9 e tO1 25 18 61 9 9 38 8 9 * I01 *lncludre oil tubitencet that were found at or above a O.S\ threshold on the BATCH peek identification proqre* in the Hevlett-Packerd >,itta. corresponding to < detection of liait of 10 yq/q bAnthraeene-d)0 internel (tenderd edded iMtedietely prior to enelyds: SO mg/L injected equivalent to 72S yg/g in original aaaple. cDeutereted recovery standard lepike). edded to original aaaple before extraction. dQuantitated reletive to eree of aajor ion for Authentic ttenderd 'tetlMted concentretion beeed on eree of totel ion reletive to thet of enthrecene-d|0. internel tenderd- ^Tentative identlficetlon. not confined with Authentic (tenderd*. ^Hajor aeaeee of unfenoun ceapounde ere lieted in perentheeee According to deerteting intentitlet Pottlble aoleculer tone are tenderlined. . hStaxation of concentration* of detected cee^ounda, excluding (tenderd*. HONS 220693 TABLE 28. ANALYSIS OF CHLORINATED DIBEN.IO-r-DlOX 1 NS IN WATER SAMPLES Semple Effluent Influent ng DibenzofuiAn/1 iTrr (pptl __________ Ir.omcis Cit Cl , c_ij CJ. Cli cl* Cl, cll HD* ND ND ND NT) ND ND ND < 14 ND l`P|b ND {< 7 ) ND (< 6 ) 6 61 17 100 Influent (rep) f 14 ND ('16) NT) ((8! ND ('$) 12 140 20 no Blsnk ND ND ND ND ND ND ND ND Method detection limit 6 8 3 2 54S6 Spike level Effluent (spiked! Recovery percent 13 12 4 11 89 92 14 10 12 12 13 10 14 12 12 9 12 14 100 120 100 75 92 140 Spike level Influent (spiked! Recovery percent 130 120 97 110 75 92 140 99 120 120 130 100 120 99 130 220 120 170 86 too 101 100 78 65 Nd - non* detected. bND (<) - none detected (detection liait). HONS 22069* TABLE 29 ANALYSIS OF ntl.OR I nated r>! PFNZO-P-DI OX 1 NS IN WMF R SAMPLES Simple Effluent Cl, ND* ni Uibcnzofurcn. 1 it"! t PPl) ______________I som"|s________________ Cl* Cli ci Cl*. ND ND ND ND Cl. ND Cl, ND cl, ND Influent ND (<ll)b ND ('90) ND ND (<4| ND ND 4 11 Influent (rep) HD (<14 ) ND ('HOI ND ND (<4> ND ND 6 11 Blink ND ND ND ND ND ND ND ND Method detection limit 2 3 4 3 7436 Spike level Effluent (epiked) Recovery percent 4 6 7 4 10 18 4 11 4 4 8 4 11 14 S 11 100 67 114 100 110 78 126 100 Spike level Influent (spiked) Recovery percent 36 64 69 46 104 176 38 no 39 70 70 31 81 131 33 no 108 109 101 69 78 74 74 90 4md - none detected. bND (<**) - none detected (detection limit). MOMS 220695 TABU 30. ANALYSIS OF CHLOB1MATED DIUMZO.F-DIOXINS IN SLUDGE SAMFLTS Simple Sludge nq til 41| Ilosers cu <-ir cI7 CTT HI ND4 ND ND ND ND u 65 620 Sludge (rep) ND ND ND ND ND 17 at 830 Blink 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 ia 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 220 860 S3 100 62 120 12S 116 113 SS 4ND * none detected TABLE 31. ANALYSIS or chlorinated dibensofurans IN SLUDGE SAMPLE Sample Sludge - no DiOenzofunn/e* sludee (ppb) isomers Cl. . eiA cn Cl. cn C1R Cl, HD* HD HD ND HD HD 33 Clft 39 Sludge (rep) HD HD HD ND ND ND 25 73 Blenk ND HD HD ND ND ND ND HD Method detection limit 10 20 25 10 30 45 20 20 Spike level Sludge (spiked) Recovery percent Spike level Sludge (spiked) Recovery percent no 27 2S 1 .100 300 3S 200 no ss 2.000 2.000 100 220 130 59 2.200 2.700 123 140 no as 1.400 1.300 93 310 290 94 3. 100 3. 100 100 S20 $80 112 S.200 S. 300 102 no 130 92 i.no 940 83 370 410 B9 3,700 3.400 90 *ND * non* detected. 78 HONS 220696 TABLE 32. RCRA KETALS IN SLUDGE LEACHATE1 Analyte Artenic Barium Cadmium Chromium Lead Mercury Selenium Silver yg/L CPPb) <3 1.75 x 10J 1.88 x 10J 348 514 2 8.2 96 Re ference standard Quality Control Data True Observed value, value. yg/L yg/L Arser.e TM-7 Barium ERA 2767 Cadmium TM-NR Chromium ERA*1120 Lead ERA-1120 Mercury TK-C1 Selenium SRMA Silver SPEX-A 35.7 429 313.5 16$.3 278 IS.5 10.2 ill 35 460 300 160 265 20 10 100 Percent recovery 102 93 105 133 105 93 102 111 Analyte Arsenic SDi*eb Concentration added, yg/L . 50 Percent recovery 102 *Ai. analyses by AA. b50 m9/L of standard solution is added to leachate and amount recovered is determined. 79 MOMS 22069? TABLX 33. HERBICIDE AMD PESTICIDE CONCENTRATION IN LEACHATE Analyte Lindane Endrin Methoxychlor Toxapbene 24 *d" b 2.4.S-TF Silvex Concentration, ud/L (ppb) ND* ND ND ND ND ND Lower detection limit. vfl/L 1,000 400 SO 1 x 10* 10 10 Quality Control Data A known amount of 2.4-D and 2.4.S-TP Silvex were spiked into the sludge sample. The percent recovery was: Analyte 2.4-D 2.4.S-TP Silvex Percent recovery 120 105 aND - not detected above lower detection limit. ^Duplicate analyses performed. TABLE 34 CYANIDE AND PHENOL ANALYSIS OF LEACHATE Analyte Cyanide Phenol Concentration, pg/L 10 1,297 Analyte Cyanide Phenol Quality Control Data Observed value. True value. JJ9/L ...... wfl/L SO 60 118 12S Percent recovery 75 94 SO HONS 220698 TABLE 35. TOTAL METALS ANALYSIS OF SLUDGE SAMPLE Analyte _____ uq/g (ppm) Arsenic* 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 16.9 <0.2 5.7 2.8 x 10s <73.0 96.8 <23.0 78.8 45.0 4.5 x 10* 156.0 15.0 995.0 1.1 X 10* 361.0 2.5 X 10s 230.0 84.0 820.0 <2.4 X 10* 23.7 1.2 X 10* <519.0 105.0 <14.8 3.0 x 10s *Analyses by AA, all others by I CP. 81 MOMS 220699 TABLE 36. ANALYTICAL RESULTS FOR PRIORITY AND NON-PRICSUTY METAL POLLUTANTS IN WATER SAMPLES Priority metals A:senic? Mercury0* Se 1 e.n i um Thai 1ium Antimony Beryllium Ca-.iura Cr.romium Copper Lead Nickel Silver tir.c n-rnontv metals Aluminum Barium Boron Calcium Cobalt I ron Mages rum Manganese Molybdenum Potassium Sodium Tin Titanium Vanadium Sample ID, uq Influent Effluent* 31 . 7 < 0. a 14. 3 <63 <830 7 71 227 1.7 x 103 777 8S1 <250 3.9 x 103 4. 3 <0. 8 9. 95 <63 <830 12 <18 91 <35 <460 303 <250 133 890 187 388 2.6 x 10s <70 6.8 r 103 3-o x 10 457 S62 1.6 x 10* 6.4 x 10* <2.2 x 103 54 <150 <450 77 674 <210 <70 253 <70 186 849 1.1 X 10* <1.5 x 10 <2.2 x 103 <43 <150 `Average of duplicate analyses. ^Analyses by AA; all others by 1CP. 82 MOMS 220700 TABLE 37. QUALITY CONTROL DATA POR METALS ANALYSES Of WATER SAMPLES Analvte Arsenic* Mercury* Selenium* Thallium* Aluminum Antimony Bari urn Beryllium Cadmium Calcium Chromium Cobalt Copper I ron Lead Manganese Nickel Titanium Vanadium Zinc Reference standard TH-7 TM-C1 SRMA SPEX-A ICP ICP ICP ICP ICP ICF ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP Observed value, ud/L 31.7 i8.S 12.2 91.3 410 1,010 831 ' 173 SI 1.180 1S3 123 602 1,100 254 1,090 1,160 1,100 114 157 True value, ufl/L 35.0 20.0 11.0 100 515 1,000 920 165 SO 1,000 160 115 615 1,000 265 1,000 1,000 1,000 110 165 Percent recovery 106 93 111 91 80 101 90 105 103 lie 96 107 98 110 96 109 116 110 104 95 `Analyses by AA; *11 others by ICP. 83 MONS 220701 TABU 38. LOQ* VALUES fOE METALS >Y ICT ANALYSES Analyte Aluminum Antimony Barium Beryllium Boron Cadmium Calcium Chromium Cobalt Copper I ron Lead Magnesium Manganese Molybdenum Nickel Potassium Silver Sodium Tin Titanium Vanadium Zinc w/L 4S0 825 23 6 230 18 210 33 70 3S 56 460 70 3 65 60 4.3 x 10* 250 1.4 x 10* 2.2 X 103 43 150 26 `Least obsarvabia quality, 84 HONS 220702 TABLE 39. ANALYTICAL RESULTS FOR TOTAL CYANIDE AND TOTAL PHENOL IN WATER SAMPLES Analyte Cyanide Phenol Sample ID, ul/L (bob) Influent ^?fl"nt NR* 1384 10 1898 Quality Control Data Observed value. True value. Reference standardno /Luq/Lrecovery Cyanide Phenol 110 160 222 250 Percent 69 89 - analysis not requested TABLE 40. ANALYTICAL RESULTS FOR NCN-PPIORITY POLLUTANTS IN WATER SAMPLES Analvte Biological Oxygen Demand <Bco) Total Suspended Solids (TSSi pH Total Organic Carbon (TOC) Fluoride 0:1 and grease Sample ID Influent Effluent NR* 117 mg ^ L NR 19 mg 'L NR 8.54 NR 184 mg/L NR 1.56 mg/L NR 16 mg/L Analyte TSS Oil and grease TOC Fluoride Quality Control Data Reference Observed vslue, standard nq/l Hardness 3253 PCS PCS ERA 32S3 34 24.9 48.6 3.3 True value, mg/L 34 26 48 3.4 Percent recover*/ 100 96 101 9? *NR - analysis not requested. ____________ _ 85 MQNS 220703 APPENDIX A CC/T1S ANALYSES OF EXTRACTABLE 0ACAN ICS A-l HONS 220704 CC/MS ANALYSES OP EXTRACTABLE ORGANICS Introduction All GC/MS analyses were performed using the protocol developed for the EPA-spontored Chesapeake Bay analysis program. These analyses were performed by automated capillary column chromatography using a Hewlett-Packard 598S-A GC/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 SC-54 WC07 column - Column head pressure. 7-9 psi - MS operating pressure. 1 x 10* to 4 x 10`` torr - Septem purge on at 0.5 min - Initial temperature. 50C - Initial temperature held for 4 minutes - Heating rate, 8"C/n:n - Final temperature, 303*0 - 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 tempereture. 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 ISO pL of the sample extract into 1.5 mL sample vials along with 150 pL of a 100 pg/mL anthracene-dl0 in methylene chloride inter nal ttandard. The vial was capped and placed in the autosampler, which injected approximately 1 pL into the CC, operating in the splitlees mode. A-2 HONS 220705 Interpretation of Hass Spectra The following protocol wee followed in interpreting the mass spectral data obtained from Analysis of weter and sediment extracts: 1} Spectra of compounds detected as peaks in the HewlettPackard BATCH program with a O.S% or S% threshold (depending upon the complexity of the sample) were automatically com pared with standard spectra in the computerized EPA/N1H mass spectral data base using the Probability Based Search (PBS) software supplied by Hewlett-Packard. A goodness of fit parameter was generated (1,0 being a perfect match) for the ten matches closest to 1.0. 2) The results from these searches were reviewed by an exper ienced mass spectroscopist using the Hewlett-Packard sup plied spectral comparison software, SPD1F, to compare the sample spectra with the standard spectra identified by the SEAACH program, 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) 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 220706 The Approach outlined above was adopted to minimis* the cost and tine required for the analyses of large amounts of capillary chro matographic mass spectra by maximizing the use of computerised data interpretation techniques. Figures A-l and A-2 show spectral comparison plots which were generat ed from those "best fit" candiate compounds identified in the a computerized search of some typical GC/T1S data. These figures show comparisons of two different trichlorobeniene isomers with the un^.iown spectrum. From the difference of each of the two spectra plotted in these figures, 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 in tne effluent table for as "Bentene. tnchloro-1 isomer). '* These comparative mass spectral plots were reviewed by an expert rais spectroscopist who based cn experience in mass spectrometry ar.d miss spectral interpretation, accepted or rejected the oc.-puter-generated identification. In the example, trichlorober.cene (isomer) was determined to be the proper identification for the compound m 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 go into making 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 220707 rut s4 f^tcrivun ae* nu* in* cchtco Panaanw. I. i. 3* inch I are* I C 1 C I > IN Figure A-l. Comparison of the mass spectrum of the highest Batching compound with that of an unknown compound eluting at 11.0 minutes. HONS 22070A 399 s**CCT*un 4699 nu- 199 C6OCl3 taniana. 1.3. S-tr 1 ch 1 or* - <SCI9Ct> t HONS 220709 2) All mast intensities of multiplets present in the standard spectrum must slso be present in the unknown spectrua with similar relative intensities. 3) Since the DFTFP spectrum in the low aass region is lower than that given in the EPA criterion for this compound quantitative agreement of ion intensities was not required for masses below jn/e SO. )) if peaks are present additional to those in the standard spec trum of a compound, then it is assumed that the additional pea ks are due to the presence of an unknown co-eluting compound. !n 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 aie 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 atoms. 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 sa^>le extracts were performed in two ways. All levels of dsuterated spiking compounds were determined using the response A-7 MONS 220710 of tit* molecular ion of each of Um compounds, relative to the anthracene-d, molecular loo. Tharafora, all raeovary data vara calculated using authentic standards. The aaounts of all other compounds vara deterained assuming the total ion response of each compound to be equal to the response of the anthracene-dl0 internal standard. This latter calculation was made using the folloving relationship: Cori.entrelion of X concentration Anthracene-d 10 Total ion araa X in unknown Total ion araa anthracena'd!s m (aaaple concantration factor) The sample concentration factor takes into account the extraction and concentration of the 1-liter sample to a 1-aL extract or the extraction of approximately 10 g sediment and final volume of 1 mL in the sediment extract. QA QC for Extractable Organics MR: uses a routine procedure for assessing the condition of the mass spectrometer and the capillary column in the gat chromatograph. The mass spectrometer it tuned approximately daily using perfluorotnbutylamine (FFTBA) which is the basis for the Hewlett-Packard ALTOTUHE program. The output from an average tune is shown in Figure AO. Samples we*- run in the automated HATCH AQUIRE mode overnight, and with each batch of samples s system performance standard was analyzad. This included the compound decefluorotriphenylphosplune (DFTPP) which was analyzad by the Hewlett-Packard program: DFTPP EPA Criterion Verifier. The output from a typical analysis by this program is shown in Figure A-4. A-8 MONS 220711 6~V L*9SS-lf4i*0 CW.TC itan iam If I sets n ms K*CLLCitWil*. tn woLT*occu)>ie t**-JOOT(Vl..5 *"Vt Cel*.) IS inw cocusiut.js "U orrstT-ll3 Cut LSrv/nnu>M33 ness amis CAiN.t.eets? *-AAV< V 1* IS4 HASS AMIS Orrscr*>. IMMSI Chissiohiua IOr*S4 AOSITIvC tLCT, CHCCV*tW)-?# ACTUAL SOUhCC T ** LOG aha orrsct.i MI* Cf LIN-1I4M 73 I1C L|N>|(3t 113 M lIN>m ACTUAL ASS ft F1M ACTUAL ISO ACTUAL err HASS AM* ASUHP ISO ft* AM* ISO AATIO WIDTH tra lie** ie* ***.o? M3* Cl.l* soi.oo CM c.n .14 .* .M T* to lll.N 433 M3 M 1.14 D.*l a.it MO .11 .HT crriONT see Figure A-3. A typical result fro* tuning the Hewlett-Packard S9IS uii spectrometer with PFTBA. HONS 220712 A -10 D^TPP EPp C^ITEPION ^EBIFIE? DNI 22515 fPECTRUnt 2011 Rl . Abtinrf. It Si 68 69 7 * 187 197 198 199 ers 365 44| 448 443 9.95296 6 29.7839 33.4649 189 8.69613 88.8738 1.76876 14.7649 73.8387 18.8367 NOTE* '**' indicate ! *f Criterion 36-668 MSS 198 < 88 MASS 69 < 88 HASS 69 46-668 mf 198 < 18 mSS 198 9696 PE*K 6-98 mSS 198 16-368 m$S 106 > 18 mSS 198 < mss 443 > 468 mss 196 17-838 m*S 44* Uf&IUPW fW PHIW* t * Figur* A*4* Computer Analysis of mass spectrum of DFTPP. MOWS 220713 typically, the m/e 51 and 127 on our instrument fall tOMuhit below the normal ranga apecifiad by tha program. This fact was takan into account in interpreting ease spectra. If other peaks fell outside the ranges, the tuning of the mass spectrometer was re-examined. The substances present in the systea perfomace standard were: (1) 2,6-dimethylphenol, (2) 2,6-dimethylaniline. (3) decanol, (4) pentachlorophenol, (5) nthracena*d|0 added prior to analy sis. (6) octadecene, (7) octadecane, () DFTPP, (9) eicosane. (10) heneicosane. (It) pyrene, (12) aethyl stearate, and (13) chry sene. Figure A-S shows a typical chromatogram obtained from the standard. By examining the resolution of the peaks '20.7 min and '2-1.7 min. and by looking at the tailing of certain peaks such as decanol and pentachlorophenol. we visually determined the condition of the column. When the resolution and tailing were substantially worse than in a new column, the injection port in sert was replaced and the front end of the column was broker, off or the column replaced. In order to assess the accuracy of CC/MS quantitation, two stand ards were compared with each other. A Supelco phenols standard was analyzed on 8 February 1981, and a freshly prepared MAC standard containing many of the same 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 MAC 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-dinitrophenol, 2,4-dichlorophenol, 4-chlorom-cresol, 2,4.8-txichlorophenol, 2,4-dimtrophenol, 4-nitrophenol. 4,&-dinitro-o-cresol, and pentachlorophenol. A-ll MOWS 220714 d7*',la>-'EwIt t UL Dl* COL.PCnr.STD. aria'll inw so'4>-ea*<s> flTtaia Dae*12 i i**.Li Figure A-5. Chroaatograa of the coluan performance standard with the CC coluan in average condition. The numbered peaks are identified in the t*xt- ZX- MONS 220715 A-13 MONS 220716 ti?cn c.`F'L*.y>'coiT *.* rati aasia im Mm Ft CE-fl$T SC/PeiiS9 oaasia * .as v i.o 13 HONS 22071? Based on HRC standards tho average parcant daviation of tha values found froa tha statad valuas was 28%, excluding 4-ni trophanol, where 7 ng/L was found vs. tha statad 100 mg/L. The quantitation of 4-nitrophenol has baan a sourca of difficulty previously, as it appears to diminish in concentration with stor age tine of tha standard. The indication froa tha coaparison of standards is that except for a particularly troublesone compound such as tha 4-nitrophanol. tha average uncertainty in tha quan titation of clean samples in which tha unknown component is of comparable concentration to tha standard, is approximately 130%. A-lS MONS 220718