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

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Table 3.13 Replicate analyses <strong>of</strong> St<strong>and</strong>ard Reference Material CS-7<br />

Compound<br />

-- ----- -- -<br />

Repl icate<br />

1 2 3 4 5 6 Mean S.D.<br />

Aroclor 1254 0.77 0.76 0.76 0.73 0.81 0.65 0.75 jt0.05<br />

HCB 0.059 0.056 0.049 0.063 0.066 0.065 0.063 10.006<br />

p,pl-DDE 0 ,I 3 0.13 0.11 0.11 0.19 0.10 0.13 10.03<br />

alpha-HCH 0.088 0.084 0.062 0.077 0.070 0.070 0.075 t0.01<br />

gamma- HCH 0.054 0.05 0.05 0.076 0.075 0.060 0.061 10.06<br />

heptachlor epoxide 0.050 0.048 0.018 0.031 0.038 0.057 0.040 20.02<br />

When samples were retrieved, silver filters were removed<br />

by forceps, stored <strong>in</strong> disposable plastic Petri dishes <strong>and</strong> kept<br />

frozen until analysis (with<strong>in</strong> two months). Filters were fumed<br />

(30 m<strong>in</strong>) over concentrated HC1 prior to dry<strong>in</strong>g (80°C overnight)<br />

to remove carbonates. Dry weight <strong>of</strong> filters was compared with<br />

orig<strong>in</strong>al filter weight to measure total dry mass <strong>of</strong> particles<br />

collected. Filters were combusted <strong>in</strong> a Perk<strong>in</strong> Elmer Elemental<br />

Analyzer (Model 240) for determ<strong>in</strong>ation <strong>of</strong> organic carbon <strong>and</strong><br />

nitrogen. Absolute sensitivity (twice blank value) was<br />

approximately 5 pg for carbon <strong>and</strong> nitrogen.<br />

3.4 Lipids<br />

Lipids were extracted from 100 mg <strong>of</strong> <strong>the</strong> pulverized dry<br />

.a,<br />

tissue by homogenisation with 80 ml <strong>of</strong> 2:l chlor<strong>of</strong>orm:methanol <strong>in</strong><br />

a Virtis homogenizer for five m<strong>in</strong>utes (Barnes <strong>and</strong> Blackstock,<br />

1973) . The solution was ma<strong>in</strong>ta<strong>in</strong>ed at 55°C for ten m<strong>in</strong>utes <strong>and</strong><br />

<strong>the</strong>n filtered through a No. 1 chlor<strong>of</strong>orm:methanol washed Whatman<br />

filter <strong>in</strong>to a 100 ml volumetric flask. The solid residue was<br />

washed with small aliquots <strong>of</strong> which chlor<strong>of</strong>orm/methanol. On <strong>the</strong><br />

f<strong>in</strong>al wash<strong>in</strong>g it was poured <strong>in</strong>to <strong>the</strong> filter. The solution was<br />

made up to 100 mL <strong>and</strong> <strong>the</strong>n transferred to a 250 mL separatory

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