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SULFIDE Method 376.2 (Colorimetric, Methylene Blue) STORET NO. Total 00745 Dissolved 00746 1 Scope and ApphcatIOn 11 ThIS method IS apphcable to the measurement of total and dIssolved sulfides m dnnkmg, surface and sahne waters, domestIc and mdustnal wastes 12 ACId msoluble sulfides are not measured by thIS method Copper sulfide IS the only common sulfide m thIs class 13 The method IS sUitable for the measurement of sulfide m concentratIOns up to 20 mg/1 2 Summary of Method 2 1 Sulfide reacts wIth dimethyl-p-phenylenediamme (p-ammodimethyl amhne) m the presence of fernc chlonde to produce methylene blue, a dye WhICh IS measured at a wavelength maXImum of625 nm, 3 Comments 3 1 32 33 Samples must be taken wIth a mmimum of aeratIOn Sulfide may be volatIhzed by aeratIOn and any oxygen madvertently added to the sample may convert the sulfide to an unmeasurable form DIssolved oxygen should not be present m any water used to dilute standards The analysIs must be started ImmedIately Color and turbIdIty may mterfere wIth observatIons of color or wIth photometnc readmgs 4 Apparatus ° 41 Matched test tubes, approXImately 125 mm long and 15 mm 42 Droppers, dehvenng 20 drops/ml To obtam umform drops, hold dropper m vertiCal posItIOn and allow drops to form slowly 43 Photometer, use eIther 4 3 1 or 4 3 2 4 3 1 Spectrophotometer, for use at 625 nm wIth cells of 1 cm and 10 cm hght path 4 3 2 Filter photometer, wIth filter provIdmg transmIttance near 625 nm 5 Reagents 5 1 52 53 Ammo-sulfunc aCId stock solutIOn DIssolve 27 g N,N-dimethyl-p-phenyienediamme oxalate (p-ammodimethylamhne) m a cold mIxture of 50 ml conc H2S04 and 20 ml dIstilled water m a 100 ml volumetnc flask Cool and dilute to the mark If dark dIscard andpurchasefreshreagent Storemdarkglassbottle Ammo-sulfunc aCId reagent DIssolve 25 ml ammo-sulfunc aCId stock solutIOn (5 1) wIth 975 ml of 1+1H2S04 (5 4) Store m a dark glass bottle ThIS SolutIon should be clear Fernc ch10nde solutIOn DiSsolve 100 g FeCl3-6H20 in 40 ml dIstilled water Approved for NPDES Issued 1978 3762-1 DPDF Image | Methods for Chemical Analysis of Water and Wastes
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