Methods for Chemical Analysis of Water and Wastes

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Methods for Chemical Analysis of Water and Wastes ( methods-chemical-analysis-water-and-wastes )

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dryness, strong heatmg reoxIdIzes the chromnim Add 0 5 m1 concentrated HN03 and agam evaporate to dryness to destroy any excess sulfite Take up m im i concentrated HN03 wIth warmIng and dIlute to 200 0 m1 wIth demmeralIzed water 55 Trivalent chromIUm workIng solutIOn, 10 m1 = 0 005 ~g Cr~3 ImmedIately before use, dIlute 250 m1 of tnvalent chromIUm stock solutIOn (54) to 1000 m1 wIth demmeralIzed water 56 PotassIUm permanganate, 0 1 N DIssolve 0 3 2 g potassIUm permanganate m 100 m1 demIneralIzed water 57 SodIUm aZIde, 0 1 % DIssolve 100 mg sodIum aZIde m demineralIzed water and dIlute to 100m1 58 Methyl Isobutyl ketone (MIBK) 59 SodIUm hydroxIde SolutIon, 1 M DIssolve 40 g NaOH m demmeralIzed water and dIlute to 1lIter 5.10 Sulfunc aCId, 0 12 M Slowly add 65 m1 concentrated H2S04 (sp gr 1 84) to demIneralIzed water and dIlute to 1 lIter 6. Procedure PIpet a volume ofsample contaImg less than 2 5 ug chromIUm (100 m1 maxImum) mto a 200 m1 volumetnc flask, and adjust the volume to approxImately 100 m1 The pH must be 2 0 or less Add concentrated HN03 Ifnecessary ACIdIfy a lIter of demmeralIzed water wIth 1 5 m1 concentrated HN03 Prepare a blank and suffiCIent standards usmg tnvalent chromIUm and adjust volumes to approxImately 100 m1 wIth the aCIdIfied demmeralIzed water Add 0 1 N KMn04 dropwise to both standards and samples untIl a famt pInk color persIsts Heat on a steam bath for 20 mmutes If the color dIsappears, add addItIOnal KMn04 solutIon dropwise to maIntam a slIght excess WhIlestIllonthesteambath,addsodIUmaZIdesolutIOndropwiseuntIltheKMn04color Justdisappears Heatforabout2mmbetweeneachadditIonandaVOidaddmganyexcess Contmue heatmg for 5 mm after addIng the last drop ofsodIUm aZIde solutIOn Transfer the flasks to a water bath and cool to room temperature Remove from the water bath and filter (through Whatman No 40 filter paper or eqUIvalent) any sample WhICh has a browmsh preCIpItate or coloratIon whIch may mterfere wIth the pH adjustment Add 2 0 ml of I 1\1 NaOH and 2 drops bromophenol blue IndICator solutIon ContInue the addltlOn of I M NaOH dropwIse to all samples and standards In whIch the IndIcator change from yellow to blue has not occurred Add 0 12 M H2S04dropWIse untIl the blue colorJust disappears, then add 2 0 m1 m excess The pH at tills pomt Will be 24 The pH adjustment to 2 4 may also be made wIth a pH meter mstead of USIng an mdIcator Add 50 m1 APDC SolutIon and mIX The pH should then be approxImately 2 8 Add 10 0 m1 MIBK and shake vIgorously for 3 mmutes 61 62 63 64 65 6 6 67 68 6 9 completely m the neck of the flask 6.10 6 11 6 12 Allow the layers to separate and add demIneralIzed water untIl the ketone layer IS 2183-2

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