Document emmBjLM2gNqao8yGp6yaaK3YE

Monsanto Physical Chemistry Special Study 71-3 Job No. 1348022 MOM <N*M( LOCATION) --tL--Emery - Technology Depar-tma-ni- S. Second St. - St.--tru4*-- HtrtHthct TO January 22, V971 COMPOS,rilON OF COMPETITIVE POLY CHLORINATED BIPHENYL PRODUCTS Memo, R. E Keller to A. F. Regan, 11-5-70 R. E. Keller Res. 1 CONFIDENTIAL H . S. Bergen - GO W. B. Papageorge - GO W. R. Richard - GD R. H. Munch - Res. 2 E. S. Tucker - Res. 2 M. W. Dietrich - Res. 2 R. A. Baxter/H. S. Vodden/ R. A. Lidgett - Ruabon A. F. Regan - Newport D. Danna - GO P. G. Benignus - GO This is a follow-up to the reference memo for the purpose of reporting the results of chlorinated biphenyl isomer analyses on nine additional competitive products. The new samples were analyzed on the very same GC column and instrument used for the 11-5-70 analyses. . The results reported on 11-5-70 were calculated using electronic digital integration for measuring the individual peak areas, Further work on this system has shown that the automatic electronic integrator (Infotronics CRS-100) gives low results on the late eluting peaks (5 and 6 chlorines) which tend to be low and broad. The electronic integrator does not detect these peaks soon enough to properly measure the complete peak. Therefore, the very same analyses done in November have been recalcula ted using mechanical disc inte grator measurements wherein the analyst draws the base line and decides upon the point of peak end. This method of peak integration is more laborious, but gives more correct measure ments in the case of low, broad peaks. The recalculated values along with the new analyses are presented in Tables I and II in the same manner as given in the reference memo. As a check, the very same bottle of Sample No. 5 (Bayer Clophen 14057) analyzed in November was reanalyzed as Sample No. 16 in the current analyses. The two sets of values on this sample check quite well within the expected variability of such a complex analysis. The results show that Monsanto, MCL and all the competitive PCB products including Prodelec 1499 and 1500 contain from 3.9 to B.7% .penta- and 0.3 to 2.2% hexachlorinated biphenyls. However, the new MCS 1016 (Aroclcr 1242 distilled to remove high boilers) STLCOPCB4040729 TABLE I Sample Analyses Reported 11-15-70 Recalculated ________ Weight % of Chlorinated Biphenyls with Oise Integrator _____________ Number of Chlorine Atoms (to correct for errors 0 1 234 5 in electronic integra tion of 5 & 6 chlorine isomers) -L. 1) Aroclor 1242, Made at WGK - 3/9/70 2) Aroclor 1242 E-18, made in Great Britain 7/21/70 3) MCS-1016* 4) Kaneclor KC 300 5) Bayer Clophen (14057) ' 6) Prodelec Superad 0.01 0.01 0.7 0.04 15.5 49.4 13.0 56.4 24.8 22.8 8.7 0.85 7.4 1 0.34 0.02 0 0 0 1.0 0 0.02 0 19.7 10.8 18.3 12.1 57.3 58.0 58.5 58.8 21 .2 23.9 16,2 21 .5 0.8 7.0 5.1 7.1 <0.05 0.30 1.9 0.45 New Analyses Completed' 1-18-71 Calculated with Disc Integrator 7) Pyralene 1499 (12/22/70) 8) Pyralene 1499 (N 70/729) 9) Pyralene 1500 (J.D.S.) 10) Pyralene 1500 (12/22/70) 11) Pyralene 1500 (N 70/728) 12) Bayer Clophen A.30 13) Bayer Clophen A,30 (20198) 14) Bayer Clophen A.30 (20200) 15) Caffaro Apirollo . 1431C 16) Bayer Clophen (14057)(Repeat) 0 0 0 0.02 0.02 0.02 0 0 0 0 0 0.1 0.4 0.4 0..4 0 0.02 0 0 0.05 12.0 17.0 43.9 34.6 37.0 16.8 17.7 16.5 14.3 17.6 59.1 55.2 30.0 44.1 42.8 58.4 57.7 58.6 59.5 57.9 22.4 21.7 16.6 16.3 15.5 18.0 19.8 19.3 20.1 16.5 5.9 5.5 7.9 4.1 3.9 4.9 4.3 5.0 5.5 5.7 0.6 0.5 1.2 0.5 0.4 1.9 0.45 0.6 0.69 2.2 *Aroclor 1242 distilled to remove high boilers DSW 159032 STLCOPCB4040730 TABLE I Page 2 ( f DETAILED SAMPLE IDENTIFICATIONS (As written on bottles) 1) Aroclor 1242, Bottle 46, ABS #1, 3/9/70 WGK. 2) Aroclor 1242 E.18 Sample 8, #N701 9035, 7/21/70, made in Great Britain by Monsanto, 3) MCS 1016 1348560 Drum I, 7/27/70 Pilot Plant. 4) Kane'clor KC 300, from Fujiken at June 70, for # 111 samples of P.G.B. letter of June 11, 1970. 5) Bayer-Clophen Trial Product 14057, OW7095012, 11K 8072/2 (contains epoxfde additive, probably Der 332). 6) Prodelec Superad {6% Unox 206, Ex Dubilier condenser, from Peter Marsh, London. 7) Pyralene 1499 from Prodelec, dated 12/22/70. 8) Pyralene 1499 from Prodelec, N70/729. 9) Pyralene 1500 from Prodelec (J. D. Sullivan). 10) Pyralene 1500 from Prodelec, dated 12/22/70. 11) Pyralene 1500from Prodelec, N70/728. 12) Bayer Clophen A.30. 13) Bayer Clophen A.30 Lot No. 20198. 14) Bayer Clophen A.30 Lot No. 20200. 15) Caffaro Apirollo 1431C. 16) Bayer-Cl ophen Trial Product 14057 (Repea t of 11/5/70 Analysis - Sample #5). DSW 159033 STLCOPCB4040731 PCB Meeting Robert Reinert Matthew Zabik Howard E, Johnson Michael Gilbertson Michael E. Fox C. S. Hegre ' J. F. Uthe ' Robert E. Keller William B. Papageorge Jack T. Garrett Daniel W. Anderson Louis Swaby 3 U. S, Bur. of Commercial Fisheries Ann Arbor, Michigan Pesticide Research Center Michigan State UniversityEast Lansing, Michigan Pesticide Research Center Michigan State University East Lansing, Michigan Canada Centre for Inland Waters Burlington, Ontario Canada Centre for Inland Waters Burlington, Ontario National Marine Water Quality Lab. West Kingston, R. I, . : Fisheries Research Board of Canada Winnipeg, Manitoba Monsanto Company Organic Chemicals Division 1700 South Second Street St. Louis, MO 63177 Monsanto Company 800 North Lindbergh Blvd. St. Louis, MO 63166 Monsanto Company . 800 North Lindbergh Blvd. St. Louis, MO Dept, Wildlife Ecology University of Wisconsin Madison, Wisconsin , FWPCA, Washington, D. C. DSW 162165 STLCOPCB4040732 Retention No. of Time Chlorine (Min. ) Atoms 9.6 11 .0 12.3 13.0 14.0 14.5 15.0 16.1 17.6 18.2 19.0 20.1 20.3 21.2 22.3 23.0 23.4 24.3 24.8 25.3 26.8 27.6 28.5 29.7 31 .0 31.7 32.3 33.0 34.0 36.0 36.6 37.6 39.0 41.0 42.2 43.3 44.5 47.6 61.0 55.0 56.0 Ko n 0 1 1 2 2 2 2 3 80%3 3 3 3 3 3 3 4 3 4 4 3&4 3 4 4 4 4 4 4 5 4 5 5 5 5 5 5 6 5 6 5 c, 6 f, Peak Area Correction Factor .58 .71 .76 .93 .93 1.0 1 .0 1.2 1 .18 1.2 1.2 1.2 1.2 1 .2 1.2 1 .4 1 .2 1.4 1 .4 1.3 1.4 1 .2 1 .4 1 .4 1.4 1 .4 1 .4 1 .6 1.6 1 .4 1 .6 1 .6 1 .6 1 .6 1 .6 1 .8 1 .6 1 .8 1.6 1 .8 1 .6 1 .8 (1) A-1242 WGK 0.01 0.54 0.15 3.4 0.7 1.3 7.3 0.9 14.0 1.0 5.8 1.9 14.0 6.7 3.0 1 .2 - 4.2 3.1 2.4 3.7 3.2 3.7 0.6 0.05 1 .4 3.6 4.3 - 2.5 1.2 0.27 0.72 0.72 0.72 0.23 0.98 0.36 0.70 0.14 0.52 0.07 TABLE II (2) A-l242 Gr.8ritain 0.01 0.04 2.5 0.2 0.8 6.2 1.2 16.4 1 .3 7.5 2.2 17.0 8.2 3.7 1.2 3.5 2.7 1.9 3.4 3.5 3.4 0.6 - ' 1 .2 3.1 3.4 - 2.2 0.49 0.21 0.46 0.46 0.46 0.13 0.60 0.21 0.26 - 0.26 - Page I Concentration in Weight % (3) MCS 1016 0.02 0.7 0.3 4.2 0.9 1 .7 9.4 1.1 17.3 1.1 6.9 2.1 17.1 8.0 3.5 1.1 . 5.0 3.6 2.6 4.4 2.4 3.7 0.6 - 0.4 0.8 0.8 0.10 0.10 0.09 0.01 _ _ _ _ _ - (4) Kaneclor KC 30 _' _ 1.7 0.1 0.6 5.2 1.2 16.1 1.2 7.6 2.3 18.0 8.5 3.9 1.3 3.9 3.0 2.1 3.6 3.5 3.6 0.8 0.01 1 .1 2.9 3.4 - 2.1 0.5 0.13 0.48 0.48 0.48 0.14 0.52 0.14 0.24 0.02 0.12 - (5) Bayer Clophen (6) Prodelac Superad From Spec. Special Study 69-3 __ _ 0.02 - - 3.9 2.2 0.5 0.02 1 .4 0.2 9.0 6.3 1.4 1.0 17.5 16.9 1 .5 7.8 2.6 16.5 8.0 3.6 0.9 7.8 1.2 20.3 8.2 3.9 0.9 1 .1 -- 2.6 3.8 1.9 2.3 1 .4 1 .7 2.4 3.4 3.0 2.8 2.6 3.1 0.4 0.6 -- 0.7 1 .2 1 .9 2.9 2.4 3.6 - ~ 1.5 0.6 0.1 0.50 2.2 0.5 0.10 0.32 0.50 . 0.50 0.11 0.59 0.3 2 0.32 0.07 0.46 0.27 0.60 0.44 0.34 0.11 0.17 0.31 0.10 0.15 0.11 ' ___ 4.7 7.6 10.7 11.6 13.6 14.5 14.8 16.4 18.2 19.3 19.8 21.2 21.4 22.2 23.1 23.7 24.0 25.1 25.5 25.9 26.9 27.2 27.8 28.8 29.6 29.8 30.3 30.6 31 .3 32.1 32.6 33.1 34.3 34,6 35.0 35.4 35.9 37.1 38.1 40.5 K9 - ^42.5 DSW 159034 STLCOPCB4040733 Reteritl on T i me (Hin. ) 9.6 11 .0 12.3 13.0 14.0 14.5 15.0 16.1 17.6 18.2 19.0 20.1 20.3 21 .2 22.3 23.0 23.4 24.3 24.8 25.3 26.8 27.6 28.5 29.7 31.0 31 .7 32.3 33.0 34.0 36.0 36.6 37.6 39.0 41.0 42.2 43.3 44.5 47.6 51 .0 55.0 56.0 59.0 No. of Peak Area Chlorine Correction Atoms Factor 0 .58 1 .71 1 .76 2 .93 2 .93 2 1 .0 2 1.0 3 1.2 80%3 1.18 3 1 .2 3 1.2 3 1.2 3 1.2 3 1.2 3- 1.2 4 1.4 3 1.2 4 1.4 4 1.4 3&4 1 .3 4 1.4 3 1.2 4 1 .4 4 1 .4 4 1 .4 4 1 .4 4 1 .4 5 1.6 5 1 .6 4 1.4 5 1.6 5 1.6 5 1.6 5 1 .6 5 1 .6 6 1.8 5 1.6 6 1.8 5 1 .6 6 1 .8 5 1 .6 6 1 .8 on Pyralene 1499 (12/22/70) - - 2.1 0.1 0.3 6.2 1 .1 16.5 0.8 7.4 1.3 20.1 8.0 3.9 2.4 - 3.9 2.4 1 .9 3.3 2.4 3.3 0.74 0.04 4.3 4.3 3.7 0.08 2.8 2.8 0.10 0.35 0.35 0.35 0.09 0.60 0.13 0.33 0.14 0.17 0.23 Concentration in Weiqht % P e2 (S) Pyralene 1499 (N 70/729) - 0.9 (9) Pyralene 1500 (J.D.S. ) - 0.1 0.3 (10) Pyralene 1500 (12/22/70) 0.02 0.4 _ (11 ) Pyralene 15 (N 70/728) 0.02 0.4 3.2 0.15 0.22 10.3 1 .1 15.5 0.7 6.9 1.1 18.8 7.4 3.6 1 .1 3.4 3.3' 35.5 35.5 1 .2 8.4 0.6 . 3.5 0.8 9.4 3.9 1.8 0.8 - 7.1 0.5 24.5 24.5 1.1 13.0 0.7 5.5 1.1 14.2 5.8 2.8 0.9 _ 7.6 0.5 ' 26.3 26.3 1 .1 12.9 0.6 5.3 1 .0 13.9 5.6 2.7 0.8 3.7 2.3 1 .8 3.2 2.3 3.3 0.87 0.07 4.2 4.2 3.6 0.12 2.6 2.6 0.10 0.40 0.40 0.40 0.09 0.46 0.13 0.27 0.10 0.14 0.19 - 2.9 1.9 1 .5 2.2 1 .4 2.3 0.4 0.03 3.6 3.6 3.4 0.08 1.7 1 .1 0.4 0.76 0.76 0.76 0.27 0.97 0.28 0.80 0.22 0.42 0.40 2.7 1.7 1.5 2.4 1.9 2.5 0.8 0.05 0.9 2.1 2.8 0.04 1.8 1.8 0.04 0.22 0.22 0.22 0.06 O'. 33 0.10 0.20 0.13 0.11 0.20 2.6 1 .7 1.3 2.3 1.8 2.4 0.5 0.05 0.8 2.1 2.6 0.03 1.9 1.9 0.03 0.22 0.22 0.22 0.06 -----' 0.32 0.08 0.19 0.09 0.10 0.16 - DSW 159035 STLCOPCB4040734 Retention Time (Min.) 9.6 11.0 1 2.3 13.0 U.O 14.5 15.0 . 16.1 17.6 18.2 19.0 20.1 20.3 21 .2 22.3 23.0 23.4 24.3 24.8 25.3 26.8 27.6 28.5 29.7 31.0 31 .7 32.3 33.0 34.0 36.0 36.6 37.6 39.0 41 .0 . 42.2 43.3 44.5 47.6 51 .0 55.0 56.0 53.0 No. of Chiorine Atoms 0. 1 1 2 '2 2 2 3 8033 3 3: 3 3 3 3 4 3 4 4 3&4 4 3 4 4 4 4 4 5 5 4 5 5' 5 5 5 6 5 6 5 6 5 6 W Peak Area Correction Factor .58 .71 .76 .93 .93 1.0 1.0 1.2 "1.18 1 .2 ' 1.2 , 1.2 1.2 1.2 1.2 1.41.2 1.4 1 .4 1 .3 1 .4 1.2 1 .4 1 .4 1 .4 . 1 .4 1 .4 1.6 1 .6 1 .4 1.6 - 1.6 1 .6 1 .6 1 .6 1.8 1.6 1.8 1 .6 1 .8 1.6 1.8 Concentration in Bayer (12) Bayer (13) Bayer (14) Clophen Clophen Clophen A.30 A .30(20198) A.30(20200) - 0.02 - 0.02 - - ` 3.5 3.4 3.4 0.5 0.5 0.4 1.2 1 .3 1.2 8.2 9.2 8.2 1.3 1 .4 1.4 16.8 16.5 16.7 1 .4 1.3 1.3 7.5 7.5 7.6 2.7 2.5 2.5 16.5 16.5 16.6 8.0 7.9 8.1 3.7 3.7 3.8 1.2 - 1.2 - 1.2 - 2.9 . 2.9 2.9 2.2 2.2 2.2 1.8 1 .7 1 .8 2.5 2.9 2.9 2.9 3.0 3.1 2.9 3.0 3.0 0.8 0.9 1 .0 0.04 0.08 0.05 0.8 . 0.8 1.0 2.1 2.5 2.5 2.6 2.9 2.9 0.09 0.08 0.14 1.7 2.3 2.2 0.48 2.3 2.2 0.09 0.08 0.05 0.43 0.31 0.35 0.43 0.31 0.35 0.43 0.31 0.35 0.09 0.55 0.25 0.43 0.30 0.21 0.08 0.49 0.12 0.30 0.09 0.15 0.09 0.57 0.14 0.33 0.14 0.19 1 .29 0.16 0.26 Height % Caffaro(15) Apirollo Bayer clophen 1431 C (14057)(Repeat) '- - - 0.05 -- 2.7 3.7 0.3 0.5 ,, 0.9 1 .3 7.0 8.7 1.3 1 .4 16.8 17.2 1.2 1.3 7.6 7.5 2.3 2.6 17.6 16.3 8.3 7.8 3.9 3.6 1.1 1.1 -- 3.3 2.7 2.4 2.0 1.7 1 .6 3.1 2.5 3.0 2.8 3.1 2.5 0.7 0.8 0.06 0.04 3.5 0.8 3.5 1.9 3.1 2.4 0.10 0.11 2.0 1.4 0.6 0.75 0. lo 0.41 0.13 0.47 0.41 0.47 0.41 0.47 0.10 0.13 0.59 - 0.73 -- 0.15 0.30 0.38 0.71 0.19 0.48 0.18 0.40 0.25 1 .26 Page 3 ', W DSW 159036 STLCOPCB4040735 itfcnsanto MOM N*Ml fr t R. E. Keller - Technology Dept. - S. Second St. - St. Louis r*T| ( fturwccT MCI tHtKCl November 5, 1970 COMPOSITION OF POLYCHLORINATED BIPHENYL PRODUCTS TO : A. F. Regan Newport CONFIDENTIAL H. S. Bergen - GO W. B. Papageorge - GO W. R. Richard - GO R. H. Munch - Res, 2 E. M. Emery - Res. 2 E. S. Tucker - Res. 2 M. W. Dietrich - Res. 2 R. A. Baxter/H. S. sVodden/ R. A; Li,dgett - Ruabon D. Danna - GO , During the week of 11-2-70, we analyzed a set of polychlorinated biphenyl products for chlorinated biphenyl isomers using our most up-tordate gae chromatography technique. Current Newport Aroclor 1242 was included in this set. Table 1 gives the weight percent ages found for chlorine homologue's ranging from 0 to 6 chlorines per biphenyl unit. Table II represents a more detailed breakciovn of the isonters separated by GC. Results show that Monsanto, MCL and competitive products listed in the tables all contain from 4.4 to 7.8% penta- and <0.05 to 0.9% hexachlori riated biphenyls. Prodelec 1 499 and 1 500 thought to be low in penta- and hexa-isoniers are not available in the U.S. for inclusion in this work. We have reserved the GC column for analysis of these products upon receipt of same from Europe. Results for the above Prodelec materials will be sent to your attention. Details of GC Work Our Physical Chemistry Group (E. Emery) analyzed the samples by flame ionization gas chromatography using the mass spectrometry peak identifications provided in Spectroscopy Special Study 69-3. Our SE-52 SCOT capillary columns have gone bad, so these analyses were done on a 200 ft. X 0.0'2" I.D. SE-52 conventional wall- coated capillary column. This accounts for the somewhat different retention times reported in Table II. Relative response factors have been obtained for the flame ionization detector to enable us to put the results on a weight basis. This was done by running a few known isomers and narrow distillation fractions containing only a single chlorine level. An average peak area correction factor was thus obtained for each chlorine level as tabulated in Table II. Each peak area is multiplied by this factor to give a corrected peak area on a weight basis. The corrected peak areas are normalized to give a concentration for each component in weight per cent. . C. db Attach. - 2 ' . R. E. Keller / n.io nrv ?i. DSW 159037 STLCOPCB4040736 1) Aroclor 1242, Made at WGK - <3/9/70 2) Aroclor 1242 E-18, Made in Great Britain 7/21/70 3) MCS-1016* 4) Kaneclor KC 300 5) Bayer - Clophen 6) Prodelec Superad 7) Prodelec 1499 ) 8) Prodelec 1500 ) TABLE I 01 Weight % of Chlorinated Biphenyls Number of Chlorine Atoms 2 3 4 5 6 -> 0.01 0.7 15.7 49.0 26.3 7.8 0.53 0.01 0.04 13.2 58.8 23.2 4.6 0.11 0.02 - 1 .0 - 0.02 - 19.7 10.9 18.2 12.2 57.3 60.5 59.4 60.5 21 .2 *24.1 16.5 22.6 0.8 <0.05 4.4 0.12 5.0 0.86 4.6 0.16 (To be obtained upon receipt of samples . from Europe) *Aroclor 1242 distilled to remove high boilers Detailed Sample Identifications . (As written on bottles) 1) Aroclor 1242, Bottle 46, ABS #1 , 3/9/70 WGK. 2) Aroclor 1242 E.18 Sample 8, #N701 9035, 7/21/70, made in Great Britain by Monsanto. . 3) MCS 1016 1348560 Drum I, 7/27/70 Pilot Plaht. 4) Kaneclor KC 300, from Fujiken at dune 70, for 111 samples of P.G.B. letter of June 11, 1970. 5) Bayer - Clophen Trial Product 1 4057, 0W7O95O12, UK 8072/2 (contains epoxide additive, probably Der 332). 6} Prodelec Superad (6% Unox 206), Ex Dubilier condenser, from Peter Marsh, London. DSW 159038 STLCOPCB4040737 Retention Time {Min.) No. of Chiorine Atoms Peak Area Correction Factor 9.6 11.0 12.3 13.0 14.0 14.5 15.0 16.1 17.6 18.2 19.0 20.1 20.3 21 .2 22.3 23.0 23.4 24.3 24.8 25.3 26.8 27.6 28.5 29.7 31 .0 31.7 32.3 33.0 34.0 36.0 36.6 37.6 . 39.0 41 .0 42.2 43.3 44.5 47.5 51 .0 0 1 .1 2 2 2 2 3 80%3 3 3 3 3 3 3 3 4 4 4 3&4 4 3 4 4 4 4 4 5 5 4 5 5 5 5 5 6 5 6 5 0.58 0.71 0.76 0.93 0.93 1 .0 1 .0 ' 1.2 . 1 .18 1.2 1 .2 1.2 ' 1.2 1.2 1.2 1.2 1.4 1.4 1.4 1 .3 1 .4 1.2 1 .4 1 .4 1.41.4 \ 1.4 1 .6 1.6 1 .4 1.6 1.6 1.6 1.6 . 1.6 1 .8 1.6 1 .8 1.6 n 5 1.6 . ss!o 6 1.8 O) A-i242 WGK. C.0 i% 0.5 0.2 3.4 0.8 1 .4 7.4 0.9 14.0 1 .0 5.8 2.0 2.0 14.0 6.7 3.0 1-2. 4C 2 3'.2 2.4 3.6' 3.2 3.7 0.6 0.05 1 .4 3.6 4.3 0.10 2.6 1.1 0.56 0.07 0.32 0.48 0.26 0.87 0..21 0.48 0.39 0.05 TABLE II (2) A-l 242 Gr.Britain 0.01 % 0.04 - 2.6 0.2 0.8 6.3 1.2 16.3 1 .3 7.5 2.2 2.2 17.1 8.2 3.7 1 .2 ' 3.6 2.7 1.9 3.5 3.6 3.5 0.6 - 1.2 3.1 3.4 - 2.2 ,,5 .29 0.02 0.10 0.17 0.07 0.48 0.09 0.21 0.16 - friiirpntra f.inn in Wei 9ht 2 (4) (3) Kaneclor Bayer KCS 1016 KC 300 ClODhen 0.02% 0.7 - - - 0.3 - - 4.2 1:7% 3.9% 0.9 .13 0.5 1.7 ' .6 1 .4 9.4 5.2 8.9 1.1 1 .2 1 .4 17.3 16.3 17.6 1.1. 6.9 1 .2 7.6 1.5 7.9 2.1 2.3 2.7 2.1 2.3 2.7 . 17.1 18.1 16.5 8.0 8.6 8.0 3.5 3.9 3.6 1.1 1 .3 1.0 5.0 ' 3.9 2.7 3.6 3.0 2.0 2.6 2.1 1.4 4.4 3.6 2,5 2.4' 3.5 2.9 3.7 3.7 3.7 ' 0.6 0.8 0.4 - .01 - 0.4 1 .1 0.7 0.8 2.9 1 .9 0.8 3.4 2.5 0.10 - - 0.10 2.1 1 .5 0.09 0.5 0.6 0.01 - - - 0.28 0.006 o.n 0.16 0.06 0.37 0.06 0.27 -` 0.14 0.25 0.07 0.58 0.12 -' 0.15 0.65 - 0.10 0.59 - - 0.68 (6) Prodelac Superad _ - 2.2% 0.02 ' 0.24 6.3 1 .0 17.0 .9 7.8 1 .2 1.2 20.4 8.2 3.8 1 .1 3.8 2.4 1.7 3.5 2.8 ' 3.2 0.6 - 1.3 3.0 3.7 - 2.2 0.47 0.12 - 0.08 0.12 0.04 ' 0.39 0.07 0.22 0.15 0.05 ^tention Time From Spec. Special Studv 69-3 4.7 7.6 10.7 11.6 13.6 14.5 14.8 16.4 18.2 19.3 19.8 21 .2 21 .4 22.2 23.1 23.7 24.0 25.1 25.5 25.9 26.9 . 27.2 27.8 28.8 29.6 29.8 30.3 30.6 31 .3 32.1 32.6 33.1 34.3 34.6 35.0 35.4 35.9 37.1 38.1 40.5 42.5 . DSW 159039 STLCOPCB4040738