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6 by means of a ground glass Jomt Any eqmvalent reflux apparatus may be substituted provided that a ground-glass connectIOn IS used between the flask and the condenser Reagents 7 65 66 67 6.8 Procedure 6 1 6 2 63 64 Distilled water Special precautions should be taken to msure that distIlled water used m this test be low m orgamc matter Standard potassIUm dichromate solutIOn (0 025 N) Dissolve 12 259 g K2Cr207, pnmary standard grade, preVIOusly dned at 103°C for two hou~s, m distIlled water and dilute to 1000 ml MIx thiS solutIOn thoroughly then dllute 100 0 ml to 1000 ml With distilled I IIIII water. Sulfunc aCid reagent Conc H2S04contamlng 23 5g sli~er~ulfate, Ag2S04> per 409kg bottle (With contmuous stlfrmg, the sIlver sulfate may be dissolved m about 30 mtnut~s ) I I II Standard ferrous ammomum sulfate (0 025 N) Dissolve 98 g of Fe(NH4)z(S04)2-6H20 m distdled water Add 20 ml ofconc H2S04(6 8), cool and dllute to 1hter Dilute 100 ml of thiS solutIOn to 1 hter With distilled water ThiS solution "Ifl:yst ~,~ stap.,Hardlzed dally agamst K2Cr207 solutIOn 64 1 Standardization To approximately 200 ml ofdistIlled water add 25 0 ml of0 025 N K2Cr207 (62) solutIOn Add 20 ml of H2S04 (68) and cool Titrate With ferrous ammomumsulfate(64)usmg3dropsofferrommdlcator(66) Thecolorchange IS sharp, gomg from blue-green to reddish-brown Mercunc sulfate Powdered HgS04 Phenanthrolme ferrous sulfate (ferrom) mdlcator solution Dissolve 148 g of 1-10 (ortho)phenanthrohne monohydrate, together With 070 g of FeS04-7H20 m 100 ml of water ThiS mdlcator may be purchased already prepared Silver sulfate Powdered Ag2S04 Sulfunc aCid (sp gr 1 84) Concentrated H2S04 Place several bOllmg stones m the reflux flask, followed by 50 0 ml of sample or an aliquot d11uted to 500 m1 and 1 g of HgS04(6 5) Add 50 ml conc H2S04(6 8), SWirl until the mercunc sulfate has dissolved Place reflux flask m an Ice bath and slowly add, With sWlrlmg, 25 0 ml of 0025 N K2Cr207 (6 2) Now add 70 ml of sulfunc aCid-sliver sulfate solution (6 3) to the cooled reflux flask, agam usmg slow addition With sWlrhng motIOn Caution Caremustbetakentoassurethatthecontentsoftheflaskarewellmixed Ifnot, superheatmg may result, and the mixture may be blown out of the open end of the condenser 7 1 4102-2 I II II I I III I I,PDF Image | Methods for Chemical Analysis of Water and Wastes
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