Document 7OGxgnj0b5Z5L1e37N41JNgko

4 To: Joe Ledvina, Houston Intaroffkt CoiwmuwkaWow From: mi: Subject H. G. Coleman, R&D, Austin February 2, 1990 Analysis of Resins for BUS-80 VISTA Several samples of resins were submitted to R&D Analytical for gas phase chromatography (GPC) in an effort to determine the level of BUS-80 present from the EVC clean wall plant trial currently in progress at Aberdeen. Resin made with BUS-80 in reactor D-745 was isolated from that made in reactor D-700 without BUS-80. They are Identified on the attached GPC charts as "treated" and "untreated" respectively. There are four "trios" of charts that show the level of BUS-80 present, let me discuss each one separately. 1. These are methanol extracts of treated, untreated, and BUS-80 spiked untreated (Analytical spiked untreated samples with 50 ppb of BUS-80) resins. GPC fluorescence was measured. Significant activity occurred at the 16 minute marie in the spiked sample. The treated sample exhibited only minor activity compared to the untreated sample, and far less than the spiked. n. Same samples as in I; GPC UV (ultraviolet) was measured. Activity was noted at the same 16 minute mark, very significant with the spiked sample. Very little activity was seen with the treated sample. ID. Resin samples came from different production lots than I and II above. Again, treated, untreated, and spiked samples were analyzed, but this time the methanol was dried off and the residue was concentrated in a small amount of THF. Areas on the GPC fluorescence curves where significant activity is noted are at 14.5 minutes and at 17.5 minutes. Once again, the treated sample with BUS-80 shows less activity than the spiked (50ppb) sample and only slightly more than the untreated sample. IV. The same resins as in D! were measured on GPC UV. Peak activity at 17.5 minutes was noted on the spiked sample, with absolutely nothing from the untreated sample and only minor activity from the treated sample. These analyses show that two different resin samples made in D-745 with BUS-80, and analyzed using two different solvents (methanol and THF), showed levels of BUS-80 significantly less than known, 50 ppb spiked "standards". This indicates that the level on the resin is far less than 50 ppb and that most of the BUS-80 remains on die reactor walk or in die water discharged from the centrifuge. I hope this evidence is useful to you and our legal advisors in determining the FDA status of resin made in a reactor treated with EVC's dean wall agent, BUS-80. If you have any questions, please call me at (512) 331-2428. Harold G. Coleman Senior Group Leader - Resin Technology cc: Austin - RBQ Houston - EJM, RRS Aberdeen - RWS, RBN, KWB SOS l-Fab-90 17:2Si56 ringed oa 2--Fefc-90 at 9:43t2S Acquisition method Units Channel Injection Sun time Injection volume Acquisition version LAB 3 22.OC mi 100 uL o . 21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version FLUOR GPC BUS80 THF 1 ML/MIN; 2 50A COLUMNS, 35C UV ABSORPTION 225, FLUORESCENCE EXCIT-232, EMIT-270ac LAB 2 3 1.00 per Analysis 5.21 80-5 IN MEOH Chromatogram of 805 A Peak Nane Ret time Area Height Tvte Amount Intercept No Peaks, Try Again. Total Area or Height is zero. No Peaks, Try Again. Slone Response VEV-145152 802 l-Feb-SO 17:02:04 -intec on 2--Feb--90 at 9:39:56 Acquisition method Units Channel Injection Run time Injection volume Acquisition version LAB X3a 22.CO min 100 uL 6.21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version FLUOR GPC 3US30 THF 1 ML/MIN; 2 50A COLUMNS, 35C UV ABSORPTION 225, FLUORESCENCE EXCIT-233, EMIT-270nm LAB 2 2 1 1.00 per Analysis 6.21 A Chromatogram of 602 1000 mV 300 600 400 03 Peak NameRet ViseArea Height Type Amount InterceptSlope Response No Peaks, Try Again. Total Area or Height is zero. No Peaks, Try Again. UEV-145153 SPA l-Feb-90 16:37:03 . -ntec on 2-Feb-90 at 9:36:50 Acquisition method Units Channel Injection Run time Injection volume Acquisition version LAB 3 1 22.00 min 100 uL 6.21 Quantitation method Svstem number Vial Total injections Sample rate Mode Quantitation version FLUOR GPC BUSaO THF 1 ML/MIN; 2 50A COLUMNS, 35C UV ABSORPTION 235, FLUORESCENCE EXCIT-233, EMIT-S70nm LAB 2 * 1 1.00 per Analysis 6.21 IN MEOH Chromatogram of SPA 1000 mV sae 600 460 G0 A Peak Name Ret time Area Height Type Amount Intercept No Peaks, Try Again. Total Area or Height is zero. No Peaks, Try Again. Slope Response UEU-145154 805 1-Feb--9O 1V:26:56 Tinted on 2-Feb"2G at 2:41:46 Acquisition method Units Channel *nject*on Run time Injection volume Acquisition version LAS 2 22.00 min 100 uL 6.21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version LAS 2 3 1 2,00 per sec Analysis 6.21 UV235 GPC BUSS9 THF 1 ML/MIN; 2 50A COLUMNS, 35C UV ABSORPTION 235, FLUORESCENCE EXCIT-233, EMIT-370nm A Chromatogram of 605 300 mV 50 280 15 10 5 a Peak Nane Ret time Area Heicftt Type Amount InterceptSlone Response No Peaks, Try Again. Total Area or Height is zero. No Peaks, Try Again. VEV-145155 302 iO 17sQ2:04 .'iated on 2-Feb-90 it 5:38s36 Acquisition method Jm's Channel --ejection Sun time Injection volume Acquisition version LAB 2 22.00 min 100 uL 6.21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version LAS 2 2A 2.00 per sec Analysis 6.21 1*7 225 2rC ausao TH? 1 ML/MIN; 2 50A COLUMNS, 35C JV ABSORPTION 225, FLUORESCENCE EXCIT-233, EMIT-370nm Chromatogram ox 602 39 mV 250 269 150 100 50 0 V reak Kane Ret tine Area Height Tvse Amount InterceptSlone Response No Peaks, Cry Again. Total Area or Height is zero. No Peaks, Try Again. gEV-145156 SPA l-F#b-90 16 s 37 : 06 listed on 2-Feb-90 at 9 :55 Acquisition method Units Channel Innujnectitmioen Injection volume Acquisition version LAB 2 22.00 min 100 uL 6.21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version LAB 2 2.DO per sec Analysis 6.21 UV235 GPC BUSS0 THF 1 ML/MIN; 2 50A COLUMNS, 35C UV ABSORPTION 225, FLUORESCENCE EXCIT-233, EMIT-370nm SPIKE\A IN MEOH WIT* St f+6 BUS Chromatogram of SPA 300 mV 5 200 150 180 50 0 4 Peak MaceRet tise._ Area_ Height.Type Amount InterceptSlope Response So Peaks, Try Again. Total Area or Height is zero. No Peaks, Try Again. VEU-145157 3 Q4CON 1 --Faste 90 1 S s X 6 : 44 inted on 2-Feb-SO st 9:50:25 Acquisition method Units Channel Injection Sun time Injection volume Acquisition version LAE *w5 1 22.00 min 100 uL 6.21 Quantitation method System number Vial Total inject! ons Sample rate Mode Quantitation version FLUOR GPC 3US80 THF 1 ML/MIN; 2 50A COLUMNS, 35C UV ABSORPTION 235, FLUORESCENCE EXCIT-233, EMIT-370n LAB 5 1 1.00 per Analysis 8.21 20-4 10X C0NC2N IN THF/UNTREATED Chromatogram of S04CCN 1000 Ch mV @00 600 400 08 A reak Naae xer, tineArea Height Type Amount Intercept No Peaks, Try Again. Octal Area or Height is zero. No Peaks, Try Again. No Slope Sesronse VV~M5158 SP3CON 1-Fb-SO 19:31 22 ,inted on 2-Feb-90 at 10 s 01:30 Acquisition method Units Channel Injection Sun time Injection volume Acquisition version FLUOR LAB 3 22.00 min 100 uL .21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version LAE 2 e i 1.00 per sec Analysis 6.21 CPC BUSoC THF 1 ML/MIN; 2 50A COLUMNS, 35C UV ABSORPTION 235, FLUORESCENCE EXCIT-233, EMIT-370nm OX CONCEN Chromatogram of 5PBC0N 1000 mV S00 600 400 200 Peak Name Ret tine Area Height Type Amount Intercept `Jo Peaks, Try Again. Total Area or Height is zero. So Peaks, Try Again. Slope Response ^EU-145160 3 O 4 CON l-F*b-90 X B s X 6 : 44 ringed on 2-Feb-SO at 3:43:28 Acquisition method Units Channel Injection Run time Injection volume Acquisition version LAB 2 1 22.00 min 100 uL 6.21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version LAB 2 5 1 2.00 per sec Analysis 6.21 UV235 GPC BUS80 THF 1 ML/MIN? 2 50A COLUMNS, 35C UV ABSORPTION 225, FLUORESCENCE EXCIT-233, EMI?-370nm 80-4 10X CONCEN IN THF Chromatogram of 804CON 300 rr,V 50 00 150 100 50 0 A Peak Name Ret tineArea Height Type Amount InterceptSlcne _ Response No Peaks, Try Again. Total Area or Height is zero. Mo Peaks, Try Again. VEV-145161 801CON 1-Feb- 90 18:41 : 38 rinted on Z-Feb-90 at 9:52:51 Acquisition method Units Channel Injection Run time Injection volume Acquisition version LAE 2 1 22.00 min 100 uL 6.21 Quantitation method System number Vial Total inject ions Sample rate Mode Quantitation version LAE 2 S 1 2.GO per Analysis 6.21 sec UV235 G?C BUS80 THF 1 ML/MINj 2 50A COLUMNS, 35C UV ABSORPTION 235, FLUORESCENCE EXCIT-253, EMI?-370nm BO-1 10X CONCEN IN THF Chromatogram of 801CON see mV 250 00 15 100 50 0 A Peak NameRet timeArea Height Type Amount InterceptSlsoe Response No Peaks, Try Again. Total Area or Height is zero. No Peaks, Try Again. yB,_145162 SPBCON l-Feb-SO 19:31:22 .Tinted on 2-Feb-90 at 10:00:02 Acquisition method Units Channel Injection Run time Injection volume Acquisition version LAB 2 22.00 min 100 uL 6.21 Quantitation method System number Vial Total injections Sample rate Mode Quantitation version LAB 2 8 1 2.00 per sec Analysis 6.21 UV235 GFC 3US80 THF 1 ML/MXN; 2 50A COLUMNS, 35C UV ABSORPTION 235, FLUORESCENCE EXCIT-233, EMIT-370nm [SPIKE\B 10X CONCEN 'A'lTv4 5DPPB so Chromatogram of SPBCON A Peak NameRet tine Area___ Height Tyne Amount InterceptSlone ,, Response No Peaks, Try Again. Total Area or Height is zero. No Peaks, Try Again. vEV-i45i63