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54 SulfuncaCIdsolutIon,H2S04, 1+1 5.5 Diammomum hydrogen phosphate solutIon DIssolve 400 g (NH4)zHP04 m 800 ml dIstilled water 56 Methylene blue solutIOn I DIssolve 109 ofmethylene blue m dIstIlled water m al lIter volumetnc flask and dIlute to the mark Use U S P grade or one certIfied by the BIOlogIcal Stam CommISSIOn The dye content reported on the label should be 84% or more StandardIze (5 8) agaInst sulfide solutIOns of known strength and adjust concentratIon so that 0 05 ml (1 drop) equals 1 0 mg/l sulfide 57 Methylene blue solutIOn II DIlute 10 00 ml of adjusted methylene blue solutIOn I (5 6) to 100 ml wIth dIstilled water m a volumetnc flask 58 StandardIzatIOn ofmethylene blue I solutIOn 5 8 1 Place several grams of clean, washed crystals of sodIum sulfide NazS·9HzO m a small beaker 5 8 2 Add somewhat less than enough water to cover the crystals 5 8 3 StIr occasIOnally for a few mmutes Pour the solutIOn mto another vessel ThIS reacts slowly wIth oxygen but the change IS mSlgmficnat over a few hours Make the SolutIon daIly 5.8 4 To 1lIter ofdIstilled water add 1drop ofsolutIOn and mIX 5.8 5 ImmedIately dete11I1Ule the sulfide concentratIOn by the methylene blue procedure (6) and by the tttnmetnc IOdIde procedure (Method 376 1, thIS manual) 5 8 6 Repeat usmg more than one drop of sulfide solutIOn or less water untIl at least five tests have been made m the range of 1to 8 mg/l sulfide 587 Calculate the average percent error of the methylene blue procedure (6) as compared to the tltnmetnc IOdIde procedure (Method 376 1) 5 8 8 Adjust by dIlutIon or by addmg more dye to methylene blue solutIOn I (5 6) 6 Procedure 6 1 Color development 6.1 1 Transfer 7 5 ml of sample to each of two matched test tubes usmg a specIal WIde tIpped pIpet or fIllmg to a mark on the test tubes 6 1 2 To tube A add 0 5 ml amme-sulfurIc aCId reagent (5 2) and 0 15 ml (3 drops) FeCl3 6 1 3 6 14 6.1 5 SolutIon (5 3) MIX ImmedIately by mvertmg the tube only once To tube B add 05 mIl+1H2S04 (5 4) and 0 15 ml (3 drops) FeCl3 solutIOn (5 3) andmlX Color WIll develop m tube A m the presence of sulfide Color development IS usually complete m about 1 mmute, but a longer time IS often reqUIred for the fadmg ofthe InItIal pmk color Walt 3 to 5 mmutes Add 1 6 ml (NH4)zHP04 SolutIon (5 5) to each tube 6.16 6 1 7 6 1.8 Walt 3 to 5 mmutes and make color comparIsons If zmc acetate was used walt at least 10 mmutes before makmg comparIson 3762-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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