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Distribution of Chlorinated Hydrocarbon Pesticides and PCBs in the ...

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Fraction 2: beta-HCH, alpha-HCH (60%), gamma-HCH, dieldr<strong>in</strong>,<br />

endr<strong>in</strong>, o,pt-DDT, o,pt-DDD <strong>and</strong> p,pt-DDD, alpha-<br />

endosulphan, heptachlor epoxide, methoxychlor,<br />

cis- <strong>and</strong> trans-chlorane.<br />

Fraction 3: methoxychlor (lo%), dieldr<strong>in</strong> (5%).<br />

Two composite pesticide st<strong>and</strong>ards <strong>and</strong> PCB st<strong>and</strong>ards<br />

(Aroclor 1254 <strong>and</strong>/or 1:l Aroclor 1254/Aroclor 1260) were run<br />

-<br />

daily to verify <strong>in</strong>strument performance, establish current<br />

retention times <strong>and</strong> determ<strong>in</strong>e current response factors.<br />

Each sample fraction was <strong>in</strong>jected <strong>in</strong> duplicate, <strong>and</strong> when<br />

necessary co-<strong>in</strong>jected with a pesticide composite st<strong>and</strong>ard<br />

mixture.<br />

Extracts from <strong>the</strong> third sampl<strong>in</strong>g trip were separated us<strong>in</strong>g<br />

<strong>the</strong> follow<strong>in</strong>g procedure as per Nordstrum <strong>and</strong> Muir (1985).<br />

A glass column (10 mm x 240 mm) was filled with hexane <strong>and</strong><br />

slurry packed with florisil (8 g 1.2% water deactivated), capped<br />

with a 10 mm layer <strong>of</strong> anhydrous sodium sulphate <strong>and</strong> flushed with<br />

40 mL hexane. Fraction 2 from <strong>the</strong> gel permeation column was<br />

quantitatively tr-ansferred to <strong>the</strong> column followed by a series <strong>of</strong><br />

r<strong>in</strong>ses with 3 x 1 mL hexane. The column was eluted with 35 mL<br />

hexane (fraction l), 34 mL 15% dichloromethane <strong>in</strong> hexane<br />

(fraction 2) <strong>and</strong> 52 mL 50% dichloromethane <strong>in</strong> hexane (fraction<br />

3). Each fraction was taken down to 2 mL by rotary evaporation<br />

for analysis by GC/ECD.<br />

Cut po<strong>in</strong>ts for this procedure gave <strong>the</strong> follow<strong>in</strong>g<br />

separation:<br />

Fraction 1:<br />

Fraction 2:<br />

hexachlorobenzene, heptachlor, aldr<strong>in</strong>, o,pt-DDE,<br />

p,pt-DDE, Mirex, decachlorobiphenyl (I.S.)<br />

alpha-, beta-, <strong>and</strong> gamma-hexachlorocyclohexane,<br />

oxychlordane, trans- <strong>and</strong> cis-chlordane, o,pf-<br />

DDD, p,pt-DDD, p,pt-DDT, cis-nonachlor

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