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6.2 6 1 4 CommercIally avaIlable "odorless buffers" WhICh are more stable, may be used InhIbItors For most waters InhIbItors are not necessary If Interfenng Ions are present use one ofthe follOWIng 62 1 InhIbItor I NaCN powder (CautIon extremely pOIsonous) Flush solutIons or sample contaImng thIs down draIn USIng large quantItIes of water Make sure no aCIds are present whIch mIght lIberate HCN gas 6.22 InhIbItor II DIssolve 50 g Na2S-9 H20 or 3 7 g Na2S·5 H20 In 100 ml dIStilled water Exclude aIr WIth tIghtly fitted rubber stopper ThIS gIves sulfide preCIpItates whIch may obscure the end POInt If large quantIties of heavy metals are present Detenorates rapIdly throllgh aIr oXIdatIOn 623 InhIbItor III DIssolve 45 g hydroxylamIne hydrochlonde m 100 m1 of 95% ethanol or Isopropanol IndIcator Use a commercIally avaIlable IndIcator such as Calmaglte IndIcator (Mallmckrodt) or one ofthe formulatIOns descnbed below (63 1-6 3 3) 6.3 I MIX 0 5 g Enochrome Black T WIth 4 5 g hydroxylamIne hydrochlonde DIssolve In 100 m1 of95% ethanol or Isopropanol 6 3 2 DIssolve 0 5 to 1 0 9 Enochrome Black T m an appropnate solvent such as tnethanolammeor2-methoxyethanol StableapproxImatelyoneweek 6 3 3 MIX together 0 5 g Enochrome Black T and 100 g NaCl Standard EDTA tltrant, 002 N 'Place 3 723 g analytICal reagent grade dISodIUm ethylenedIammetetraacetatedIhydrate,Na2H2ClOH120gN2-2H20 mallItervolumetnc flask and dIlute to the mark WIth dIstIlled water Check WIth standard calCIUm solution (641) by tItratIOn (6 4 5) Store m polyethylene Check penodICally because of gradual detenoratlon 63 64 64.1 6 4 2 643 644 645 Standard calcIUm solutlon 0 02 N Place 1 000 g anhydrous calcIUm carbonate (pnmarystandardlowInmetals)Ina500mlflask Add,alIttleatatlme,1+1 HCL (642) untll all of the CaC03 has dIssolved Add 200 ml dIstllled water Boll for a few mInutes to expel CO2 Cool Add a few drops of methyl red mdicator (643) and adjust to IntermedIate orange color by addIng 3N NH40H (6 4 4) or 1 + 1 HCI (6 4 2) as reqUIred Quantltatlvely transfer to a 1 lIter volumetnc flask and dIlute to mark WIth dIstIlled water Hydrochlonc aCId solutIOn, 1+ 1 Methyl red IndIcator DIssolve 0 10 g methyl red In dIstIlled water In a 100 ml volumetnc flask and dIlute to the mark AmmOnIumhydrOXidesolutIOn,3N DIlute210mlofconc NH40Hto1hterWIth dIstIlled water StandardIZatlon tltratlon procedure Place 10 0 ml standard calcIUm solution (641) m vessel contaInIng about 50 m1 dIstIlled water Add 1 m1 buffer SolutIon (6 1) Add 1-2 drops mdICator (6 3) or small scoop of dry IndIcator (6 3 3) TItrate slowly With contmuous stIrnng untIl the last reddIsq tmge dIsappears, addmg last 1302-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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