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8. Procedure 8 1 For samples wIthout sulfIde 82 For samples that contam sulfIde 83 84 85 86 87 the aIr rate occasIOnally Proceed to 8 4 IfsamplescontamNOsandorN02add2gofsulfamlcaCIdsolutIon(7 15)aftertheaIr rate IS set through the aIr mlet tube MIX for 3 mmutes pnor to addltlon of H~04 Slowly add 50 ml l8N sulfunc aCId (7 5) through the au mlet tube Rmse the tube with dIstIlled water and allow the aIrflow to mIX the flask contents for 3 mm Pour 20 ml of magnesIUm chlonde (7 14) mto the aIr mlet and wash down with a stream of water Heat the solutIon to bOIlmg Reflux for one hour Turn off heat and contmue the anflow for at least 15 mmutes After coolmg the bOIlmg flask, dIsconnect absorber and close off the vacuum source Dram the solution from the absorber mto a 250 ml volumetrIc flask Wash the absorber With dIstilled water and add the washmgs to the flask DIlute to the mark with dIstIlled water Withdraw 50 ml or less of the solution from the flask and transfer to a 100 ml volumetnc flask If less than 50 mIlS taken, dIlute to 50 ml with 0 25N sodIUm hydroXIde SolutIon (74) Add 150 ml of sodIUm phosphate solutIOn (7 6) and mix 8 I I 8 1 2 Place 500 ml of sample, or an alIquot dIluted to 500 ml m the 1 lIter bOIlmg flask PIpet 50 ml of sodIUm hydroxIde (7 1) mto the absorbmg tube If the apparatus m FIgure 1 IS used, add dIstIlled water untIl the spIral IS covered Connect the boIlmg flask, condenser, absorber and trap m the (ram (FIgure 1 or 2) Start a slow stream of aIr entenng the bOIlIng flask by adJustmg the vacuum source AdJustthevacuumsothatapproxImatelytwobubblesofaIrpersecond enters the bOIlmg flask through the aIr mlet tube Proceed to 8 4 8.2 1 822 Place 500 ml of sample, or an alIquot dIluted to 500 ml m the 1 lIter bOIlmg flask Plpet50 ml of sodIUm hydroXIde (7 1) to the absorbmg tube Add 25 ml of lead acetate (7 2) to the sulfIde scrubber Connect the boIlmg flask, condenser, scrubberandabsorberm thetram (FIgure3)Theflo~meterISconnectedtothe outlet tube of the cyamde absorber Start a stream of aIr entermg the bOIlmg flask by adJustmg the vacuum source Adjust the vacuum so that approxImately 15 lIters per mmute enters the bOIlmg flask through the aIr mlet tube The bubble rate may not remam constantwhIleheatISbemgapplIedtotheflask Itmaybenecessarytoreadjust 871 8 7 2 Pyndme-barbltunc aCId method Add 2 ml of chloramme T (7 12) and mIX See Note 1 After 1 to 2 mmutes, add 5 ml of pyndme-barbItunc aCId solution (713 1) and mIX DIlute to mark WIth dIstIlled water and mIX agam Allow 8 mmutes for color development then read absorbance at 578 nm m a l cm cell wIthm 15 mmutes Pyndme-pyrazolene method Add 0 5 ml of chloramme T (7 12) and mIX See Note 1 and 2 After 1 to 2 mmutes add 5 ml of pyndme-pyrazolone solutIOn 3352-4PDF Image | Methods for Chemical Analysis of Water and Wastes
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