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6. 54 StIvermtrate-mtncaCidreagent Dissolve85gAgN03and05mlconc HN03m500ml distilled water Procedure 7 Calculation 6 1 Removalofslhca IfslhcaconcentratiOnISgreaterthan25mg/l 6 1 1 Evaporate sample nearly to dryness m a platmum dish on a steam bath 6 1 2 Add 1 ml HCI solutiOn (5 2), tilt dish and rotate unttI acid contacts all of the residue 6 1 3 ContInue evaporatiOn to dryness 6 1 4 Complete drymg m an oven at 180°C 6 1 5 Iforgamc matter present, char over a flame 6 1 6 MOisten with 2 ml dlsttlled water and 1 ml HCI solutiOn (5 2) 6 1 7 Evaporate to dryness on a steam bath 6 18 Add2mlHCIsolutiOn(5 2) 6.1 9 Take up soluble residue m hot dlsttIled water and filter 6 1 10 Wash the msoluble stIlca With several small portiOns ofhot dlsttIled water 6.1 11 Combme filtrate and washmgs PreCipitation ofbanurn sulfate 6 2 6 3 FtItratiOn and Welghmg 62 1 62 2 6 2 3 6 2 4 6.2 5 62.6 627 6 2 8 Ifnecessary, treat clanfied sample to remove mterfenng agents Adjust to contam approximately 50 mg S04iOn m a 250 ml volume Adjust aCidity With HCI solutiOn (5 2) to pH 4 5 to 5 0, usmg pH meter or orange colorofmethylredmdlcator(5 1) Add an addltiOnall to 2 ml HCI solutiOn (5 2) For lower concentratiOns ofsulfate Ion fix the total volume at 150 ml Heat to botImg and, whtIe stIrnng gently, add warm BaCl2 solutiOn (5 3) slowly, unttI precipitatiOn appears to be complete, then add approximately 2 ml m excess Ifamount ofprecipitate IS small, add a total of5 ml BaCl2 solutiOn (53) Digest the precipitate at 80 to 90°C preferably overnight but for not less than 2 hours 63 1 63 2 6 3 3 634 6 3 5 MiX a httle ashless filter paper pulp w1th the BaS04 and filter at room temperature Wash the precipitate With small portiOns of warm dlstllied water untll the washmgs are free of chlonde as mdiCated by testmg With sliver mtrate-mtnc aCid reagent (5 4) Dry the filter and precipitate Igmteat800°Cfor1hour DONOTLETTHEFILTERPAPERFLAME Cool m a deSiCcator and weigh mg/lS04= mgBaS04 x4115 ml sample 3753-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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