Document evgLpwZZ0MNa1ObeKLYbnR1EG

Attached are re s u lts o f our recent Dayton Laboratory a n a ly sis of Chlorophenol Products fo r d io xin content. As you are aware, process m odifications in 1979 thru 1980 cleared a ll chlorophenol products of d io x in s. The only continuing le v e ls were found in the s t i l l pot residue which is c u rre n tly stored pending in c in e ra tio n . A continuing sampling program was in it ia t e d which consisted of accumulating various product samples and shipping these to Dayton fo r a n a ly s is on a q u a rte rly b a s is . A recent calendar of events is r e a lly necessary to put these numbers in perspective. 6/81 A n a lysis continued to show process streams below the detection lim it s (w*l ppb) 7/81 Residue in the c h lo rin e supply lin e was beginning to r e s t r ic t chlorine flow to the ch lo rin a to r. . 8/81 The c h lo rin e system was pressure je tte d and c a u stic washed to remove the resid ue without success. 11/81 Higher le v e ls o f d io xin appeared in unrefined 93% 2-4 DCP that was shipped d ir e c t ly from the c h lo rin a to r. 1/82 Refined PCP samples began showing low le v e l o f d io xins in the lower c h lo rin a tio n ranges. The re s u lts of these samples were not received u n t il J u ly o f 1982. 7/82 A new process fo r d ire c t c h lo rin a tio n of PCP to 2-4 DCP was demonstrated. Th is was the f i r s t m aterial made d ir e c t ly from the c h lo rin a to r sin ce the November 93% 2-4 DCP. Subsequent a n a ly s is showed t h is m aterial very high in d io x in . SUBJECT TO PROTECTIVE ORDER. C10263 H. W. Kilbourne Chlorophenol Trace Im purity Levels Page 2 WGK 11/1/82 8/82 The c h lo rin a to r ch lo rin e supply lin e was changed out and m o d ificatio ns made to prevent fu rth e r build-up. Subsequent a n a ly sis confirmed that the build-up m aterial was high in chlo rin ated phenol compounds, e s p e c ia lly Penta Chlorophenol and very high in d io x in . 9/82 2-4 DCP manufactured showed much lower d io xin le v e ls but s t i l l w ell above the detection le v e l. The actual sparge ring in the c h lo rin a to r was changed completely to elim in ate any p o tential fo r co n tam in atio n . 10/82 Current 2-4 DCP production shows no d io xin a t the detection lim it s o f 1 ppb. Other ion in te rfe re n ce make actual quanti fic a tio n of some c h lo rin a tio n isomers im possible since they could p o ssib ly hide d io xin peaks. For t h is reason, some re s u lts are reported as le s s than the in te rfe re n ce peak height. Summary Current chlorophenol products including 2-4 DCP are fre e of d io xin s a t the detection lim it s of the mass spec, a n a ly s is . The e a rly problems with the cu rren t 2-4 DCP production was a function o f a p h ysical problem in the c h lo rin a to r system and not o f function of the new manufacturing process. The only known continuing source of d io xin in the chlorophenol process i s the s t i l l pot residue which is being accumulated fo r fu tu re in c in e ra tio n . I f I can provide any other c la r if ic a t io n or explanation o f t h is problem, please le t me know. M. E. Whelan /bb A tt. CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. Date 1/82 2/82 3/82 4/82 7/82 8/82 8/82 9/82 10/82 Batch/Lot Name Cl Cl Cl Cl 5002 5007 5012 5022 5043 . 5044 5047 BI 105 PCP Samples PCP Lot. M PCP From F in a l D i s t i lla t io n Cut \ PCP From Tank 165 (Sto rag e) 5 2 NO ND ND ND ND ND ND ND ND ND ND NO < 2 Cl Cl Cl ND ND ND ND ND ND < 6 ND ND 4/81 6/81 8/81 11/81 2/82 9/32 9/82 10/82 10/82 10/82 10/82 7005 7006 7009 7010 61010118 1104 J101 J103 J107 J1 0 2-4 DCP A n a ly s is (U nrefined ) 93% 2-4DCP 93% 2-4 DCP 93% 2-4 DCP 93% 2-4 DCP ND ND ND ND ND < 7 96% 2-4 DCP (New Pro cess) ND ND ND ND ND ND ND . ND ND ND 2 ND <12 ND ND 14 29 18 3 61 27 44 ND 3 2116 ND C 7 ND < 2 ND 4 ND < 2 87 68 18 < 6 <17 <3 ND 14 8 2 ND 81 58 79 no 89 5 9113 62 52 ND ND ND <1 10/81 6/82 10/82 10/82 10/81 8005 8023 8026 OCP Crude OCP OCP' OCP Tank 163 OCP S t i l l Bottoms Residue ND ND f ND f ND <: 5800 5000 1200 1770 4200 3940 3140 Legend ND - None D etectable I - In te rfe re n c e Makes Val e Non Quan if ia b e C - Height o f an In te rfe re n ce Peak Whl ch Cou Id be Hiding a P o ssib le D ioxin Peak CONFIDENTIAL 010 6 i SU B JEC T TO PRO TECTIVE ORDER