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65 66 67 68 69 NOTE 4: Hydroxylamme hydrochlonde may be used m place of hydroxylamme sulfate Potassmm Permanganate 05% solutlOn, w/v DIssolve 5 g ofpotassmm permanganate m 1 hter of dIstIlled water Potassmm Permanganate, 0 1 N DIssolve 3 16 g of potassmm permanganate m dIstIlled water and dIlute to 1 hter Potassmm Persulfate 0 5% solutlOn, WIv DIssolve 5 g potassmm persulfate m 1 hter of dIstIlled water Stock Mercury SolutlOn DIssolve 0 1354 g of mercunc chlonde in 75 ml of dIstIlled water Add 10 ml of conc mtnc aCId and adjust the volume to 1000 m IlO ml = 10 mgHg Workmg Mercury SolutlOn Make succeSSIve dIlutIons of the stock mercury SolutIon (68) to obtam a workmg standard contammg 01 ug per ml ThIS workmg standard and thedIlutIonsofthestockmercurySolutIonshouldbepreparedfreshdaIly ACIdItyofthe workmg standard should be mamtamed at 015% mtnc aCId ThIS aCId should be added to the flask as needed before the addItIon of the ahquot From thIS solutlOn prepare standards contammg 02,05, 1 0,20,50, 10 0, 150 and 20 0 ug Hg/1 AIr Scrubber SolutlOn MIX equal volumes of 0 1 N potassmm permanganate (6 6) and 10% sulfunc aCId (6 1 2) 6 10 7 Procedure 7 1 72 73 74 7 5 Set up mamfold as shown m FIgure 2 Feedmg all the reagents through the system wIth aCId wash solutIon (6 2 1) through the sample hne, adjust heatmg bath to 105°C Turn on atomIC absorptIon spectrophotometer, adjust mstrument settmgs as recommended by the manufacturer, ahgn absorptlOn cell m hght path for maXImum transmIttance and place heat lamp dIrectly over absorptlOn cell Arrange workmg mercury standards from 0 2 to 20 0 ug Hg/1 m sampler and start samphng Complete loadmg ofsample tray wIth unknown samples Prepare standard curve by plottmg peak heIght of processed standards agamst concentratIon values Determme concentratIOn of samples by comparmg sample peak heIght wIth standard curve NOTE 5: Because of the tOXIC nature of mercury vapor, precautIOn must be taken to aVOId ItS mhalatlOn Ventmg the mercury vapor mto an exhaust hood or passmg the vapor through some absorbmg medIa such as a) equal volumes of0 1N KMn04 (6 6) and 10% H2S04 (6 I 2) b) 025% Iodme m a 3% KI solutIOn, IS recommended A specIally treated charcoal that WIll adsorb mercury vapor IS also avaIlable from Barnebey and Cheney, E 8th Ave and North CaSSIdy St ,Columbus, OhIO 43219, Cat #580-13 or #580-22 After the analysIs IS complete put all hnes except the H2S04 hne m dIstIlled water to wash out system After flushmg, wash out the H2S04 hne Also flush the COlIs m the hIgh temperature heatmg bath by pumpmg stannous sulfate (63) through the sample hnes followed by dIstIlled water ThIS WIll prevent buIld-up of OXIdes of manganese 76 2452-3PDF Image | Methods for Chemical Analysis of Water and Wastes
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