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6 Reagents 6 1 Standard potasslUm dIchromate solutIon, (025 N) DIssolve 122588 g of K 2Cr20 7, pnmary standard grade, prevIously dned for 2 hours at 103°C In water and dIlute to 1000 ml 62 Sulfunc aCId reagent Conc H2S04containing 235 g sIlver sulfate, Ag2S04, per 4 09kg bottle (WIth continuous stirnng, the sIlver sulfate may be dIssolved In about 30 minutes ) 63 Standard ferrous ammOnIum sulfate, 0 250 N DIssolve 98 g of Fe(NH4)iS04)2-6H20 In dIStilled water Add 20 ml of conc H2S04, (67), cool and dIlute to 1 lIter ThIS solutIOn must be standardIzed against the standard potasslUm dIchromate solutIOn (6 1) dally 6 3 1 StandardIzatIon DIlute 25 0 ml ofstandard dIchromate solutIOn (6 1) to about 250 ml wIth dIstIlled water Add 20 ml conc sulfunc aCId (6 7) Cool, then tItrate WIth ferrous ammomum sulfate titrant (6 3), usmg 10 drops offerroIn indIcator (6 5) 64 Mercunc sulfate Powdered HgS04 65 PhenanthrolIne ferrous sulfate (ferroIn) indIcator SolutIon DIssolve 148 g of 1-10- (ortho) phenanthrolme monohydrate, together wIth 0 70 g of FeS04-7H20 In 100 ml of water ThISindIcatormaybepurchasedalreadyprepared 66 SIlver sulfate Powdered Ag2S04 67 SulfuncaCId(sp gr 184) ConcentratedH2S04 Procedure 7. 71 PIpet a 500 ml alIquot of sample not to exceed 800 mg/1 of COD Into a 500 ml, flat bottom, Erlenmeyer flask Add HgS04(6 4) In the ratIo of 10 mg to 1mg chlonde, based upon the mg of chlonde In the sample alIquot and 5 ml of sulfunc aCId (6 7) SWIrl until allthemercuncsulfatehasdIssolved Add250m1of025NK2Cr207(61) Carefullyadd 70 ml of sulfunc aCId-sIlver sulfate solutIOn (62) and gently SWIrl untIl the SolutIon IS thoroughly mIxed Glass beads should be added to the reflux mIxture to prevent bumping, WhICh can be severe and dangerous CautIon The reflux mIxture must be thoroughly mIxed before heat IS applIed If thIS IS not done, local heating occurs In the bottom of the flask, and the mIxture may be blown out ofthe condenser 7 1 1 If volatIle orgamcs are present In the sample, use an AllIhn condenser and add the sulfunc aCId-sI1ver sulfate solutIon through the condenser, whIle coolIng the flask, to reduce loss by volatIlIzation Attach the flask to the condenser and reflux the mIxture for two hours Cool, and wash down the interIor of the condenser WIth 25 ml of dIstilled water DIsconnect the condenser and wash the flask and condenser JOint WIth 25 ml of dIstIlled watersothatthetotalvolumeIS350ml Cooltoroomtemperature 7 2 7 3 4103-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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