Document 15gnq4EJwpLYvrqwXoqpgkNpj

Technical Service Report Report No. 240-82-814-23C-486 T0 C. L. Much Conoco Inc. Research and Development Department Analytical Research Section Ponca City. Oklahoma __ _ _ CONFIDENTIAL From Date T. A. Snow March 4, 1982 THIS DOCUMENT IS CONFIDENTIAL AND THE PROPERTY OF CONOCO INC. Subject Quantitative Characterization of VCM Light Ends, Tar Product to PPG and Tars from Still Pump-Out OBJECT To characterize samples 4409-107-1 (Tar Product to PPG), 4409-107-2 (Tars from still pump-out) and 4409-107-3 (VCM Light Ends). " CONCLUSIONS The lightest fraction, sample no. 4409-107-3, contained chlorinated C^, C2 compounds and chlorobutadiene. The other two samples contained chlorinated C21 C^, C^, Cg and Cg compounds. A major component list for each of the samples can be seen in Tables I, II and IV. Due to the complexity of the heavier samples (Nos. 4409-107-1 and 4409-107-2) a detailed list of components can be found in Tables III and V. DISCUSSION The GC trace is found for the samples in Figures 1, 2, and 9. Various single ion chromatograms (SIC) were used to show the location of selected classes of chlorinated compounds. Figures 3 and 9 show the SIC's of 122, 124, 126, which were chosen to show the locations of dichlorobutadienes, dichlorobutenes, trichlorobutenes and trichlorobutanes. Figures 4 and 10 show the SIC's of 156, 158 and 160, which were chosen to show the location of trichlorobutadienes, trichlorobutenes, tetrachlorobutenes, and tetrachlorobutanes. Figures 5 and 11 show the locations of mono-, di-, and trichlorobenzenes. Figures 6 and 12 distinguish the trichlorobenzenes (cn/e 180), trichlorohexenes or tetrachlorohexenes (m/e 186), tetrachlorobutadienes or pentachlorobutenes (m/e 190) and tetrachlorobutenes or pentachlorobutanes (m/e 192). Figure 13 shows the tetrachlorobenzenes (m/e 214), tetrachlorohexane or pentachlorohexane (m/e 220) and pentachlorobutenes or hexachloro-- butane (m/e 224). DISTRIBUTION GLH OCK PLF VVC 000013576 TSR NO- 240-82-814-23C-486 Page 2 Finally the Figures 7 and 14 show chlorinated Cg's (m/e 207), pentachlorobenzene (m/e 248) and hexachiorobenzene (m/e 282). EXPERIMENTAL Mass Spectral data was obtained on the Finnigan 4023 GC/MS system. All three samples were split injected (.5 ul) onto an SE30 capillary column. Sample no. 4409-107-3 was'injected at 0 C followed by a tempera ture programming to 100 C at a rate of 4 per minute and 100 C to 260 at a rate of 8^ per minute. Sample nos. 4409-10^-1 and 4409-107-2 were injected at 20 C followed^by a temperature programming to 100 C at 16U per minute and from 100 C to 260 C at 8 per minute. Spectra were obtained at 0.5 second. REFERENCE File of MS data: G3159A G3160A G3161A TSR no. 249-80--839-1, "The GCMS Analysis of the Liquid Phase from EDC Tar Solids," Keen, G. W. (1980). T. A. Snow Chemist Mass Spectrometry Group Wc 001357? TSR NO. 240-82-814-23C-486 Page 3 TABLE I Components of VCM Light Ends Sample No. 4409-107-3 Peak No. Scan No. 11 21 3 40 43 50 4| 52 5| 6I 57 59 7 -1 . . 64 81 66 9I 71 10 | 80 11 I 12 | 103 103 Component |Chloroethene |Chloroethane with trace of butenol [1,1-Dichloroethene }Methylene chloride 11,2-Dichloroethene (cis) |1,1-Dichloroethane |2-Chlorobutadiene -........................... |1,2-Dichloroethene (trans) |Chloroform |1,2-Dichloroethane |Trichloroethene |Trichloroethene See Figure 1 Table II Major Components in Sample No. 4409-107-1 XjCn^T^V^- ProJuci- Component Dichlorobutenes Trichlorobutenes Dichlorobutadienes Tetrachlorobutanes 1,2-Dichloroethane C^-Dichlorobenzenes Trichlorohexenes Naphthalenes and Indenes C2-Chlorobenzenes Trichloroethanes C2~Dichlorobenzenes Tetrachloropropanes Chlorobenzene % of Total 1 11 1 12' 8.7_ 1 16 1 1 1.9 1 5.8 1 1.7 1 4.3 l 3.5 1 8.5 1 1.1 1 6.3 Total of major compounds is approximately 95% of sample. Balance of sample can be seen on Table III. % of Total 1 3.4 1 12 1 3.0 1 1.3 4.0 1 7.6 1.4 1 6.1 1 24 1 19 1 16 1 0.35 VVC 000013578 TSR NO. 240-82-814-23C-486 Page 4 TABLE III , vjcivi rflte Product Components of Sample No. 4409-107-1 Peak No. Scan No. Component 1 48 |1,2-Dichloroethane 2 61 |1,1,2-Trichloroethane 3 66 | 3,4-Dichlorohuta.diene w/ trace 1 | dichlorobutene. 4 70 |1,4-Dichlor6butadiene w/trace t dichlorobutene 5 76 |1,2--Dichlorobutene 6 83 |2,3-Dichlorobutene (2) 7 89 |Trichlorobutene a 99 |Trichlorobutadiene 9 106 |Trichlorobutene 10 110 [Chlorinated li 118 |Tetrachloropropane 12 124 |Tetrachlorobutenes 13 137 J Tpl- rarKlrtr^^iitienes__ 14 145 |Chlorohexadiene 15 153 j Dichlorobenzene 16 159 jchlorinated Cg 17 172 |Tetrachlorobutane 18 177 |Tetrachlorobutane 19 181 |Indene with a trace of chlorinated 20 194 |Chloroxylene 21 204 [Trichlorohexene 22 209 |Trichlorohexene 23 221 |Trichlorohexene 24 226 |Chloroethylbenzene 25 233 |Chloromethyltoluene 26 249 jchlorinated Cg 27 255 |Chlorostyrene 28 263 jMethylindene 29 273 jchlorinated Cg 30 284 |C2"Dichlorobenzene 31 292 j Napthalene 32 301 j Dichlorotoluene 33 307 jchlorinated Cft 34 I 322 |Chlorobiphenyl 35 333 |C2-Dichlorobenzene 36 338 |C^-Dichlorobenzene 37 348 |C_-Dichlorobenzene 38 358 [Chlorinated compound 39 368 |Chlorinated compound 40 378 (Chlorinated compound % of Total 14 3.5 0.21 8.5 6.3 11 5.6 3.0 3.2 0.42 1.1 0.42 0.42 0.29 0.44 0.17 15 0.80 0.52 2.8 1.9 2.8 1.1 1.3 0.77 0.15 0.13 0.38 0.06 6.7 0.77 0.07 0.05 l 0.88 1.5 1.1 0.80 0.35 0.04 0.06 VVC.000013579 TSR NO. 240-82-814-23C-486 Page 5 Table III Continued Peak No. 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 Scan No. Component 390 396 402 415 430 449___ 462 471 483 489 545 563 574 584 602 622 656 680 687 |Chlorinated compound |Dichloroethylbenzene [Chlorinated compound (Chlorinated compound [Chlorinated Cg | BfQfnpc yr. 1 (jpen r a 1Bromocyclopentadiene |Chlorinated rcompound |Ethylmethylstyrene (Chlorinated Cg [Chlorinated compound j Chlorinated compound [Chlorinated compound [Chlorinated compound [Chlorinated compound j Chlorinated compound [Fluorene [Chlorinated |Chlorinated compound _____ ___ % of Total 1 0.08 1 0.11 1 0.10 I 0.08 1 0.09 0.08 1 0.15 "0705 1 0,03 0.27 1 0.03 1 0.14 1 0.09 1 0.18 [ 0.04 I 0.11 1 0.10 1 0.05 1 0.07 TABLE IV Major Components In Sample 4409-107-2 ~pb 7/7/ Otrf~ Component |Trichlorobutenes j1,1,2-Trichloroethane [Dichlorobutadienes [Chlorobenzenes jDichlorobenzenes |Dichlorobutenes j1,1,2,2-Tetrachloroethane |Tetrachlorobutanes |Dichlorobutanes |Pentachloroethane |Bischloroethylether |Trichlorobenzenes |Tetrachlorobutenes |1,2-Dichloroethane % of Total | 24 | 18 | 11 | 6.3 | 6.6 j 1.3 j 1.8 | 3.7 | 0.8 | 1.9 | 1.7 | 5.5 | 1.8 j 4.9 Total of Major Compounds is approximately 90% of sample. Balance of sample is chlorinated compounds. See Table V. VVC 000013580 TSR NO. 240-82-814-23C-486 Page 6 TABLE V Components o Sample No. 4409-170-2 -fThe. s-// // pu/p Peak No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 Scan No. Component 47 55 65 71 78 83 89 101 106 116 119 132 135 138 140 148 155 169 194 199 207 212 222 227 234 239 253 266 278 284 292 301 315 |1,2-Dichloroethane jl-Bromo-2-chloroethane |l,l,2-Trichloroethane |1,4-Dichloro-butadiene j2,3-Dichlorobutadiene w/trace of | dichlorobutene |Chlorobenzene w/dichlorobutadiene |Dichlorobutadiene |1,1,2,2-Tetrachloroethane |Dichlorobutene |Chlorinated compound |Dichlorobutadiene |Trichlorobutadiene |Pentachloroethane |Bischloroethylether |Trichlorobutene |Trichlorobutene |Trichlorobutene w/dichlorobenzene |Dichlorobenzene |Trichlorobutene with trace of | chloroxylene |Chloroxylene |Chlorinated compound |Tetrachlorobutene ]Chlorinated compound |Chloroethylbenzene |Chloronated compound IChloronated compound |Tetrachlorobutane IChloronated C^ |Trichlorobenzene |Trichlorobenzene w/tetrachlorobutane |Napthalene |Chlorinated compound |Trichlorobenzene % of Total | 4.9 | 0.16 1 18 | 3.8 1 5.3 1 | 6.3 | 1.8 | 1.8 1 1*3 | 0.05 j 0.80 | 0.72 1 1-9 1 1-7 1 2.4 | 3.0 | 0.94 | 6.6 18 1 j 0.82 j 0.59 | 1.8 | 0.45 | 0.49 j 0.42 j 0.11 | 3.7 | 0.12 i 2.7 j 2.8 | 0.35 | 0.02 j 0.04 VVC 000013581 240-82-814-23C-486 Scan No. Component 34 322 {Chlorinated Cg and 35 332 {Chlorinated Cg and C^ 36 340 |Pentachloropropane 37 347 {Chlorinated Cg 38 359 |Chlorinated compound 39 379 |Chlorinated compound 40 383 {Chlorinated compound 41 392 {Chlorinated 42 402 {Chlorinated compound 43 409 {Chlorinated compound 44 417 {Chlorinated compound 45 431 |Dibromochloropropene 46 448 {Chlorinated compound 47 463 {Chlorinated Cg 48 475 {Tetrachlorobenzene 49 489 {Tetrachlorobenzene 50 491 j Tetrachlorobenzene 51 517 j Chlorinated compound 52 529 {Chlorinated Cg 53 538 {Chlorinated compound 54 546 {Chlorinated compound 55 556 {chlorinated compound 56 562 {Chlorinated compound 57 569 |Chlorinated compound 58 580 {Chlorinated compound 59 603 |Pentachlorobenzene 60 626 {Chlorinated compound 61 642 {Chlorinated compound 62 644 {chlorinated compound 63 649 {Chlorinated Cg 64 653 {Chlorinated Cg 65 659 |Chlorinated compounds 66 659 {Chlorinated compounds 67 669 {Chlorinated compound 68 672 {Chlorinated compound 69 685 {Chlorinated compound 70 688 {Chlorinated Cg 71 701 {Chlorinated Cg 704 |Chlorinated Cg % of Total { 0.32 j 0.70 { 0.70 } 0.26 j 0.14 | 0.02 { 0.06 | 0.07 | 0.04 { 0.05 j 0.05 j 0.74 j 0.03 | 0.18 | 0.03 j 0.20 | 0.20 | 0.03 j 0.01 j 0.32 j 0.13 | 0.04 j 0.03 j 0.04 | 0.76 { 0.37 | 0.15 | 0.04 1 0.04 | 0.05 | 0.04 j 0.03 | 0.05 { 0.04 { 0.03 j 0.03 | 0.03 { 0.03 | 0.03 000013582 VVC F ig u re 1. T o ta l Io n Chrom atogram f o r Sample No. 4409-107- CHRO 5 a OJ a co N o ro CO Csl <0 a o UJ ato co CM co a H* a 4a1trL.oh.03tQVU..; CsO0sa3G* oj is \ LlI 1 U*- COMiVaiflL2aU a;coa: ^ ii oH-4 a: 2U1 as COH w . wro ro ,10 *H(M Tt. - .to1*0* VVC 0000X3583 F ig u re 2 . T o ta l Io n C hrom atogram o f Sample No. 4 4 0 9 -1 0 7 - VVC 000013584 T3 C CC n{ON ^~ po<N 1 O' OJ soT N <r 01 e 1 1 OJ --a' iTJ to 0Ifl li_i (*E300 o sfulj oJ o DO 40J oEtm_" -3 nj E OL U hco-l Xo c l"0 OJ oc c CO 0 cn <j-u 3 00 b. in N w w ro 15 C\ LO o WD (VI ro CHM in 41 . N CM W in 5 in <T> (VI 41 . ffl ro .in tD v4 0J 44 . 0J w to ro in to x <r Q Ui to 00 CVJ JVJt ro 04 f4 *Q .. -*** to rUoJU .. .. <r*-i h_i <r<r DO <c Da 2 (V _I UJ <r a <1 uo -J HH EO<rO N1 S4 4) cw Ho <cy -o *<J5 *4J1 3 3 ja X> o uO j- o o X x u Huu f- * < OJ JvS ro N rof trt (A 01 <cu <cc OJ jj u3 3X X> O OI- Vo. o-- 4= JUHS *J<H-J OH ** M N N SJ O tno-r*- C0v-r^ N 0) <rw u SCO \ UJ rI 1 1" 1 4tf-JUJ V0 CM 0-0 O \ EZ 10 i-H C'.J -:T 'X W 0J CM Cl CO Ct u r r"i""i VJ- CM *- H ur in CM % <l ,* row <s wro CHRO * vvc 000013585 Figure 4. Single Ion Chromatograms of m/e 156, 158, 160 and Total Ion Chromatogram for Sample No. 4409-107-1 RIC + MASS CHROMATOGRAMS DATA G3161A #1 02 ''6.-`82 15130 100 , CAL I C06O481D # 1 SAMPLEi 4409-107-1 v RANGEJ G 1.1100 LABEL: N 0, 4.0 QUAN: A 0, 1.0 100.0"! 126 SCANS 50 TO BASE! U 20/ 3 350 156 -. 4- Tetrachlorobutenes ^ Trichlorobutadienes 1.14/ * Trichlorobutenes II i--i--i -*|^i i R 154 * Tetrachlorobutanes i --i--i 11 "i'1 i i i i--|--i -i -r -i 156.047 i 0.500 |--i--i--a--r--f 94.5-. 308. 158 I; | Ls f f 158.047 0.500 --i--, | ,--rlV^* |` i i--r' |--i----i-- | i--"/*--pi--i--i--i--| 48.2160 I 157, 160.048 V* * illk k II 24? viH1 T'-'T' (k-i--i ' r^ **|--i--i--i * i' f i i r A n i i *rr i ii | 0.500 453632. 90s fio 00 O CHRO : 100 1 40 150 2 = 30 280 3 : 20 250 4{10 300 5-00 350 SCAN 55 50 TIME 6o- cnV 0o0 sC <NI o -I CM O' *1 oo0 CJj ' 'si o z oc m a. fsl] sa Uco 00 O o wO- E Ou uJ j: cc <j> o Hoc--o --usovc. 0c0 c H O VI W 34i-1 00 ft * ro re CO m in if) CM re ^ in CM H to <frg *5 oj E5 (Ti CO Mr H M o 14 co CO <L 0 . tJ-O ^ in ft g H . Ct*M> CO re m # <1 #o <tto wrj- vo ^ CO re 150 Z a 3 G? <IH I--J <L<L ao co 4 Ul CD V. <r u -i o -- ^ <X I IQNQ O *-* Q^ XfO I *'tf0li*. (VI N. <cu N C J40O) O JS CJ 4) c 4) Nc 4J J3 oU o 5r. J3 UH Q - 8*- < in 41 NC41 JP431 O h o M Urt u H co in rf cj a zco * \ 10 rn"T + CD Jlli CM3.U O \ El CM -< 04 Z -X &.iSyX w rTTT CO CO ai r*-r r*r~r r~u rT-r in u-4 to CL Ch cr ZUJ <xr Om tOH ft CM . wre CHR0 5 VVC 000013587 Figure 6. Single Ion Chromatograms of m/e 184j 186., 190> 192 and the ToLal Ion Chromatogram for Sample No. 4409-107-1 RIC + MASS CHROMATOGRAMS DATA: G3161A #1 02^26^*82 15-30' 00 CAL I 006848ID #1 SAMPLE< 4409-107-1 RANGE; G 1,1100 LABEL: N 0, 4.0 QUAN = A 0, 1.0 SCANS 250 TO BASE IJ 20, 3 VVC 0 0 0 0 1 3 5 8 8 CHRO 5 Figure 7. Single Ion Chromatograms of m/e 207, 209, 244, 248 and the Total Ion Chromatogram RIC + MASS CHROMATOGRAMS 62^26^82 15-30=00 SAMPLE < 4409--107-1 RANGE = G 1,1100 LABEL: 100.0-1 207 DAT A * G3161A #1 CALI' C060481D #1 SCANS 250 TO 60 N 0, 4.0 QUAH' A 0, 1-0 BASE: U 20, 3 1 Chlorinated Cg's 8. 207 062 6.500 12.5-1 209 Chlorinated Cg's 1. 209.063 0.500 12.5-, 244 Chlorinated CO,,'s 1. 244.073 8.500 12.5-1 243 No pentachlorobenzene 1. 248.074 0.500 12.5-1 232 . No hexachlorobenzene 1. 282.884 0.500 RIC _ L--,--AJV* =*=*= 258 4 10 300 5 = 00 350 5-50 400 6140 450 7 * 30 172800. 500 8'20 550 9'10 600 SCAN 10:00 TIME WC 000013589 F ig u re 8 . T o ta l Io n C hrom atogram o f Sample No. 5 5 0 9 -1 0 7 - \ Ui 1 'oO-JLiJ CJ0.U o\zz wNCS 1-------------------------1-------------------------T" o CL o C-rL a 000013590 vvc Figure 9. Single Ion Chromatograms of m/e 122, 124, 126 and Total Ion Chromatogram for Sampcl No. 4409-107-2 RIC + MASS CHROMATOGRAMS 02/26-'82 14 * 28 * 00 SAMPLE* 4409-107-2 RANGE; g 1.25O0 LABEL: 72 ^ *' U9 , ip., V-r DATA5 G3160A #1 CALI- C060481D #1 SCANS 50 TO 350 N 0. 4.0 QUAN* A 0. 1.0 BASE5 U 20. 194 'F Dichlorobutadienes 3 4864. ^ Trichlorobutenes * Dichlorobutenes J- / 213 2?3 278 122.037 0.500 .V /' 1*1 A'1 * * Trichlorobutanes 15424. rL ; 124.837 0.500 w r, ,42* , .3?1. ... 9424. fuHH | N 1 Iv r I 1 | 1 --1--r ,3gl, , 126.038 0.500 583680. RIC. < < O CHRO* 100 1*40 150 2*30 260 3*20 253 284 250 4 5 10 300 5*00 350 SCAN 5*50 TIME XfeStlOOOO V X4*J T? CN C1 <C p*. c o-- \D 1 i-i O' c > <r o >? ^4 o z Xm^4 a; c i sf Isiw ww o g V--o tuGCC cS> Uo Ooo ft _os^e <Eovs- cj x u co c *H I--oI OJ C CC C -J --O W f- *o r- re 'fr * 05 a in in J- re re to in w re D Z X . O UJ 0*J re 2 H *Q <105 a* re -*re re UG <IH HO <r<r DO z re z. UJ <L re it a O _i o K OJ X l r^ o in IW t ' O * ct.*h *-** re * aw o \ LU 1 + re_jaj re f>.iLO Owf\j-HiaZ 'If & jji re CL i TT re in r 1 "TT . re g in ** nTTT re re Ch H r-rt o CL CHRO * VVC 00001359Z Figure 11. Single Ion Chromatograms of m/e 112, 146, ISO and the Total Ion Chromatogram for Sample No. 4409-107-2 RTC + MASS CHROMATOGRAMS 14 5 28 * 00 SAMPLE * 4409-10?-2 DATA G3160A #1 CAL I * C06O4S1D # 1 SCANS 50 TO 358 VVC 0 0 0 0 1 3 5 9 3 CHRO : Figure 12. Single Ion Chromatograms of m/e 184., 186, 190, 192 and the Total Ion Chromatograms of Sample No. 4409-107-2 RIG + NASS CHROMATOGRAMS DATA G3160A #1 02^26. -82 14 >28 >08 CAL I C06043 ID #1 SAMPLE` 4409-107-2 RANGE: g 1,2500 LABEL: N 0, 4.0 QUAN* A 0, 1.0 i314^ Trichlorobenzenes SCANS 250 TO SBQ BASE5 U 20, 3 78. 184.055 0.500 . ,1, ,T, X. Chlorinated Co,'s 380. 186.056 0.500 329 392 .,. MU1?. , J, Chlorinated C,'s 4 329 m .. Chlorinated C.'s 4 RIC 284 ___fL___________________ 3S2 GC Trace ____4^3. 49 ____^8 _ _5^g 92. 190.857 0.500 101 . 192.057 0.500 143360. 250 4:10 CHRQ: 300 5`00 350 5:50 400 6 40 450 730 500 8 20 550 9`10 660 SCAN 10:00 TIME VVC 0 0 0 0 1 3 5 9 4 Figure 13. Single Ion Chromatograms of m/e 214, 220, 223, 224 and Total Ion Chromatogram of Sample No. RIC + MASS CHROMATOGRAMS 02---26.'-Q2 14*28:00 SAMPLE = 4409-107-2 RANGE* G 1,2580 LABEL* DATA= G3160A #1 CALI ! C060481D #1 N 0, 4.0 GUAM * A 0, 1.0 SCANS 250 TO 600 BASE* U 20, 3 10. 214.064 0.500 26. 220.066 0.500 1- 222.066 0.500 3.8-i 224 I 1 * 1-- Chlorinated C 's 4 1. 224.067 8.500 F1 " f'I > T'7 I f 1 > | IT1 t" T"| I I I | < < r> 4* 10 5:00 5*50 6*40 7*30 8*20 9* 10 10*00 TIME CHRO* 000013595 fo r eN o JZ "V cco cfNc CC <CNr <JN- <NI -o OO' 1-I1 CM O' * -oo CN o -- o | a. "J e el C<Oa OU \U o e uc3 e u cc 00 -O<U13 40oJ0 e oe 4i=- ok-i cj X CJ c oc 1-1 !--o1 0 00 <C fHt 4oJ CQ H , NO 03 wvo -*m O N ro w 44 in CVi co <x u Ui to & <L CD cjcO o u So ^*4 si CO Tf IjO h vo too U(j <r .. z D G -_l <r<c QU Z cj _1 E UJ CO a <r u H CV] <to I EoO Nin a:co*-<w IN I -00 O fri^CV tf in CD <TW 1-3 ECO \u MD-JLU CMClU O*-*wN<Ex<Zc *0)0 r--r 4" N VO row ro rov$ roin O'. w -H CO CJ XI 0) ro VON in * * w 44 03 O o JorJa c u o 4O= *f NO rHQITi . COO *T OJ 44 <u c<y N c 4o=1 O u o 4= o 4oJ co ft. V0 5- VO l-VO r--r <r. OJ r-- CVI CO1^ T-. OJ r--i ro CO fr ro oj O' ^00 tn OJ CO OJ 44 <c<Nuu 4O>Oc4=1JuZ x jC=J zo r--r OJ ro OJ . CO CO OJ in N 01 CJ CO 101 VC O Cfc! 500 8=20 550 9 -1 0 600 1 0 -0 0 650 10*50 700 11*40 750 12*30 8 0 0 SCAN 1 3 *2 0 TIM E .. O Cl' X u 000013596