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i Th# raaulta of our analysis of four autoclave batches are sum m arized in tha attached graph* (Figura* 1-4). 1 believe the code ia self-explanatory with the possible i exception of D2MEO. T his re fe rs to the to tal of the dixnethoxydichlorobenzeno* and
th e xnethoxydichlorophenols. The tetrachlorodibentodioxan (TDD) concentration is
I read on the right a b scissa. Tbs TDD concentrations are based on the total of tha o th er p roducts (TCP* TCA, DXMEO)and tha TCB. W# have previously shown that th e concentrations of TDD in the TC P is approxim ately equal to *** wang^ntrerian o f TDD ia the T -acid produccd fro m th a T T c P . With this background, c ertain conclusions can be drawn V/ a com parison of Figures 1-4 and a knowledge of tbs past history of TDD production ( F igure 5). Soros of these conclusions are: *
1. During A pril, 1965, production of TDD ro se to an all-tim e high and has rem ained m uch h igher ****** the previous n o rm -c u rr ent<**50 .ppm ., norm al <*>*10 ppm .
I . T hs form ation of TDD takes place alm o st en tirely during the bold period.
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3. At the end of the hold period the TCA content accounts for 2 ,0 -2 . 5% of ths yield. About V* of th is is rem oved by azeo tropic d istillation in the m ethanol s till and
recycled with the methanol.
c4 $ 4. The TCB is essentially gone at about one hour into the hold period.
I 5. Extending th s hi*** p erio d re su lts in in creased TDD form ation (Batch 701).
The causa of ths recant in crease in TDD form ation is not obvious from ths data.
H ow ever, since TDD form ation has been relativ ely low in the p ast we feel that a
detailed lab o rato ry study of the autoclave r* -"ion has a reasonably good chance
* for s rcese. Such a study is now in th* * i
-~n stage.
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