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5 3 Standard EDTA tltrant, 0 02 N Place 3 723 g analytical reagent grade disodIUm ethylenedlammetetraacetatedIhydrate,Na2H2ClQH120gN2-2H20 mallItervolumetnc flask and dIlute to the mark wIth dIstIlled water Check wIth standard calcIUm solutIon (5 3 1) by tItratIOn (5 3 5) Store m polyethylene Check penodICally becallse of gradual detenoratIon 5 3 1 Standard calcIUm solution, 0 02 N Place 1 000 g anhydrous calcIUm carbonate (pnmaly standard low m heavy metals, alkalIes and magnesIUm) m a 500 ml flask Add,alIttleatatIme1+1HCI(532)untIlalloftheCaC03hasdIssolved Add 200 ml dlstllled water BOll f~ra few mmutes to expel CO2 Cool Add a few drops of methyl red mdlcator (533) and adjust to mtermedIate orange color by addmg 3N NH40H (5 3 4) or I + 1 HCI (5 3 2) as reqUIred Quantitatively transfer to a I lIter volumetnc flask and dIlute to mark with dIstilled water 5 3 2 Hydroch10nc aCId solutIon, 1 + 1 5.33 Methyl red mdlcator DIssolve 0 10 g methyl red m dIstilled water m a 100 ml volumetnc flask. and dIlute to mark 5 3 4 Ammomum hydrOXide solutIOn, 3 N 535 StandardIZatIOn tltratlon procedure Place 10 ml standard calcIUm solutIOn 536 5 3 7 5 3 8 6 Procedure (53 1) m a vessel contammg about 50 ml dIstIlled water Add 1 ml buffer solutlon (53 6) Add 1-2 drops mdICator (5 3 7) or small scoop of dry mdlcator (5 3 7) TItrate slowly wIth contmuous stIrnng untIl the last reddIsh tmge dIsappears, addmg last few drops at 3-5 second mtervals At end pomt the color IS blue Total tItratIonduratIOnshouldbe =::;;5mmutesfromthetImeofbufferaddItIOn 02 N of EDTA = - - - - ml EDTA Buffer solutIOn DIssolve 169 g ammomum chlonde m 143 ml conc ammomum hydroxIde m a 250 ml volumetnc flask Add 1 25 g of magnesIUm salt of EDTA (5 3 8) and dilute to the mark wIth dIstilled water Store m tIghtly stoppered plastIC bottle IndIcator CommerCIally available Enochrome Black T IS used m one of the three methodsdescnbed AIlgraduallydetenorate 6 1 6 2 5 3 7 1 MIX 0 5 g dye wIth 4 5 g hydroxylamme hydrochlonde DIssolve m 100 ml of95% ethanol or Isopropanol Place 0 5-1 0 g dye m 100 g of tnethanolamme or 2-methoxyethanol MIX 0 5 g dye and 100 g NaCI for dry formulatIOn Pretreatment 6 1 1 For dnnkmg waters, surface waters, salIne waters, and dIlutIOns thereof, no pretreatment steps are necessary Proceed to 6 2 6 1 2 For most wastewaters and hIghly polluted waters, the sample must be dIgested as gIven m the AtomIC AbsorptIOn Methods sectIOn of thIS manual, paragraphs 4 1 3 and 4 1 4 Followmg thIS dIgestIOn, proceed to 6 2 Sample PreparatIon 62 1 The calCIUm content of the 50 ml alIquot to be tItrated should be 5-10 mg, therefore dilutIon should be used for hIgh calCIUm concentratIons 5 3 72 5 3 7 3 EDTA MagnesIUm Salt CommerCIally available 2152-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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