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5. Apparatus 5.1 52 5 3 5.4 An all-glass distilhng apparatus wIth an 800-1000 ml flask Spectrophotometer or filter photometer for use at 425 nm and provIdIng a hght path of 1 cmormore Nessler tubes Matched Nessler tubes (APHA Standard) about 300 mm long, 17 mm InsIdedIameter,andmarkedat225mm ±15mmInsIdemeasurementfrombottom Erlenmeyer flasks The dIstillate IS collected In 500 ml glass-stoppered flasks These flasks should be marked at the 350 and the 500 ml volumes WIth such markIng, It IS not necessary to transfer the dIstIllate to volumetnc flasks 6 Reagents 61 62 6.3 64 65 66 67 68 DIstilled water should be free of ammoma Such water IS best prepared by passage through an Ion exchange column contaInIng a strongly aCIdIC catIOn exchange reSIn mIxed wIth a strongly baSIC amon exchange reSIn RegeneratIOn of the column should be earned out accordIng to the manufacturer's InstructIOns NOTE 1: All solutIOns must be made WIth ammoma-free water Ammomum chlonde, stock solutIOn 10 ml = 10 mg NH3-N DIssolve 3819 g NH4C1 In dIstilled water and bnng to volume In a 1hter volumetnc flask Ammomum chlonde, standard solutIOn 10 ml = 001 mg Dl1ute 10 0 ml of stock SolutIon (6 2) to 1 hter In a volumetnc flask Bonc aCId solutIOn (20 gil) DIssolve 20 g H3B03 In dIstIlled water and dl1ute to 1 hter MIXed IndIcator MIX 2 volumes of 0 2% methyl red In 95% ethyl alcohol WIth 1 volume of 02% methylene blue In 95% ethyl alcohol ThIS solutIOn should be prepared fresh every 30 days NOTE 2: SpeCIally denatured ethyl alcohol conformIng to Formula 3A or 30 ofthe US Bureau of Internal Revenue may be SubstItuted for 95% ethanol Nesslerreagent DIssolve100gofmercuncIOdIdeand70gofpotassmmIOdIdeInasmall amount of water Add thIS mIxture slowly, WIth stIrnng, to a cooled solutIOn of 160 g of NaOH In 500 ml ofwater Dl1ute the mIxture to 1hter IfthIs reagent IS stored In a Pyrex b o t t l e o u t o f d I r e c t s u n l I g h t , I t w111 r e m a I n s t a b l e f o r a p e n o d o f u p t o 1 y e a r NOTE 3: ThIS reagent should gIve the charactenstIc color WIth ammoma WIthIn 10 mInutes after addItIOn, and should not produce a preCIpItate WIth small amounts of ammoma (004 mg In a 50 m1 volume) Borate buffer Add 88 ml of 0 1 N NaOH solutIOn to 500 m1 of 0 025 M sodmm tetraborate solutIOn (5 0 g anhydrous Na2B40 7 or 9 5 g Na2B40 7-lOH20 per hter) and dIlute to 1 hter Sulfunc aCId, standard solutIOn (002 N, 1 ml = 028 mg NH3-N) Prepare a stock solutIon of approXimately 0 1 N aCId by dl1utIng 3 ml of conc H2S04 (sp gr 1 84) to 1 liter WIth CO2-free dIstIlled water Dl1ute 200 ml of thIS solutIOn to 1 hter WIth CO2-free dlstl1led water NOTE 4: An alternate and perhaps preferable method IS to standardIze the approxImately 0 1 N H2S04 solutIOn agaInst a 0 100 N Na2C03 solutIOn By proper dIlutIOn the 0 02 N aCId can then be prepared 3502-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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