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4. Sample Handlmg and Preservation 5. 6 samphng Apparatus 51 Sample bottles-300 ml ±3 ml capacity BOD 1Ocubatlon bottles With tapered ground glass pomted stoppers and flared mouths 5.2 Pipets-with elongated tiPS capable ofdehvermg 2 0 ml ±O 10 ml ofreagent Reagents 61 Manganous sulfate solution Dissolve 480 g manganous sulfate (MnS04-4H20 m distilled water and dtlute to 1 hter 6 I 1 Alternatively, use 400 g of MnS04-2H20 or 364 g of MnS04-H20 per hter When uncertamty eXists regardmg the water of crystalhzatlOn, a solutlOn of eqUIvalent strength may be obtamed by adJustmg the speCific gravity of the solutlOn to 1 270 at20°C 62 Alkalme lOdlde-azlde solution Dissolve 500 g of sodmm hydrOXide (NaOH) or 700 g of potassIUm hydrOXide (KOH) and 135 g of sodmm lOdlde (Nat) or 150 g of potassmm Iodide (KI) 10 distilled water and dtlute to 1 hter To thiS solutlOn add 10 g of solutlOn aZide(NaN3) dissolvedm40mlofdistilledwater 4 1 42 4 3 4.4 4.5 Where possible, collect the sample m a 300 ml BOD mcubatlon bottle Special precautions are reqUIred to aVOld entramment or solution of atmosphenc oxygen or loss ofdissolved oxygen Wheresamplesarecollectedfromshallowdepths(lessthan5feet),useofanAPHA-type sampler IS recommended Use of a Kemmerer type sampler IS recommended for samples collected from depths ofgreater than 5 feet When a Kemmerer sampler IS used, the BOD sample bottle should be filled to overflowmg (overflow for approximately 10 seconds) Outlet tube of Kemmerer should be mserted to bottom of BOD bottle Care must be taken to prevent turbulence and the formation ofbubbles when ftI1mg bottle At time ofsamplmg, the sample temperature should be recorded as preCisely as reqUIred Do not delay the determmatlOn of dissolved oxygen m samples havmg an appreCiable lodme demand or contammg ferrous Iron I f samples must be preserved either method (45 1) or (452) below, may be employed 4.5 1 Add 2 ml ofmanganous sulfate solution (6 1) and then 2 ml ofalkahne lOdlde-azlde solution (62) to the sample contamed m the BOD bottle Both reagents must be addedwellbelowthesurfaceofthehqUld StopperthebottleImmediatelyandmix the contents thoroughly The sample should be stored at the temperature of the collection water, or water sealed and kept at a temperature of 10 to 20°C, 10 the dark Complete the procedure by addmg 2 ml H2S04(see 7 1) at time ofanalYSIS 4.52 Add 0 7 ml ofconc H2S04(6 3) and 1ml sodmm aZide solution (2 g NaN3 10 100 ml dlsttlled water) to sample 10 the BOD bottle Store sample as 10 (45 1) Complete the procedure us10g 2 ml of manganous sulfate solutlOn (6 1), 3 ml alkahne Iodide-azide solution (62), and 2 ml of conc H2S04 (63) at time of analYSIS Ifeither preservation techmque IS employed, complete the analySIS wlthm 4-8 hours after 4 6 3602-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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