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54 Hydrochlonc aCId, HCI, 1 + 1 55 Ammomum molybdate reagent Place 10 g (NH4)6M07024·4H20 m dIstilled water m a 100 ml volumetnc DIssolve by stIrnng and gently warmmg Dilute to the mark FIlter If necessary Adjust to pH 7 to 8 WIth sIhca free NH40H or NaOH Store in plastIC bottle 56 Oxahc aCId solutiOn DIssolve 10 g H2C204·2H20 m dIstilled water m a 100 ml volumetnc flask, dilute to the mark Store m plastIC 57 Stock silIca solutiOn DIssolve 4 73 g sodiUm metasilICate nonahydrate, Na2SI03·9H20, m recently boiled and cooled dIstilled water Dilute to approxImately 900 ml Analyze 100 0 ml portiOns by graVImetry (ref 1, p 484) Adjust concentratiOn to 1000 mg/1 8102 Store m tIghtly stoppered plastIC bottle 5.8 Standard slhca solutiOn DIlute 10 0 ml stock solutiOn to 1 hter WIth recently boiled and cooled dIstilled water ThIS IS 10 mg/1 S102(1 00 ml = 10 0 ug SI02) Store m a tIghtly stoppered plastIC bottle 5.9 Permanent color solutiOns 5 9 1 PotassiUm chromate solution DIssolve 630 mg K2Cr04 m dIstilled water m a l hter volumetnc flask and dilute to the mark . 592 Borax solution DIssolve 10 g sodiUm borate decahydrate, (Na2B407·lOH20) m d1stilled water m a l hter volumetnc flask and dIlute to the mark 5.10 Reducmg agent DIssolve 500 mg of 1-ammo-2-naphthol-4-sulfomc aCId and 1 g Na2S03 m 50 ml dIstIlled water WIth gentle warmIng If necessary DIssolve 30 g NaHS03m 150 m1 dIstIlled water MIX these two solutiOns FIlter mto a plastic bottle Refngerate and aVOId exposure to hght DIscard when It darkens If there IS mcomplete solubIhty or ImmedIate darkemng of the ammonaphthosulfomc aCId solutiOn do not use 6 Procedure 61 FIlter sample through a 0 45 u membrane filter 62 DIgestIon If molybdate unreactive SIlIca IS present and ItS mc1usiOn m the analySIS IS deSIred, mclude thIS step, otherWIse proceed to 6 3 62 1 622 62 3 624 Place 50 ml, or a smaller portiOn dIluted to 50 ml, offiltered (6 1) sample m a 100 ml platmum dISh Add 200 mg sIhca-free NaHC03(52) and dIgest on a steam bath for 1 hour Cool Add slowly and WIth stlrrmg 24 ml H2S04 (5 3) ImmedIately transfer to a 50 ml Nessler tube, dIlute to the mark WIth dIStilled water and proceed to 6 3 WIthout delay 63 Color development 63 1 6 3 2 Place 50 ml sample m a Nessler tube Add rapIdly 1 0 ml of 1+1 HCI (5 4) and 2 0 ml ammOnium molybdate reagent (55) MIX by mvertmg at least 6 tImes Letstand5to10mmutes Add 1 5 ml oxahc aCId solutiOn (5 6) and mIX thoroughly 6 3 3 634 63 5 636 Read color (spectrophotometncally or VIsually) after 2 mmutes but before 15 mmutes from the addItiOn of oxalIc aCid 370 1-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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