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52 SIlver sulfate, Ag2S04 crystals 53 Stock fluonde solutlOn DIssolve 0221 g anhydrous sodIUm fluonde, NaP, m dIstIlled water In a I-lIter volumetnc flask and dIlute to the mark WIth dIstIlled water, 100 ml = oImgF 54 Standard fluonde solutlOn Place 100 ml stock fluorIde solutlOn (53) In a 1 lIter volumetnc flask and dIlute to the mark WIth dIstIlled water, 1 00 ml = 0 010 mg F 55 SPADNS solutIon DIssolve 0958 g SPADNS, sodIUm 2-(parasulfophenylazo)-1,8- dlhydroxy-3,6-naphthalene dlsulfonate, In dIstIlled water In a 500 ml volumetrIC flask anddIlutetothemark StablemdefimtelyIfprotectedfromdIrectsunlIght 56 Zirconyl-acid reagent DIssolve 0 133 g zIrconyl chlonde octahydrate, ZrOCI2-8H20 In approXimately 25 ml distIlled water m a 500 ml volumetnc flask Add 350 ml conc HCI and dIlute to the mark WIth dIstIlled water 5.7 ACld-Zlrconyl-SPADNS reagent MIX equal volumes of SPADNS solutlOn (55) and zirconyl-acid reagent (5 6) The combIned reagent IS stable for at least 2 years 58 Reference solutlOn Add 10 ml SP ADNS solutlOn (5 5) to 100 ml dIstIlled water DIlute 7 ml conc HCI to 10 ml and add to the dIlute SPADNS solutlOn ThIS solutlOn IS used for zeromg the spectrophotometer or photometer It IS stable and may be used Indefimtely 59 SodIUm arsemte solutlOn Dissolve 50 g NaAs02 In dIstIlled water In a I-lIter volumetnc flask and dIlute to the mark WIth dIstIlled water (CAUTION TOXIc-avoid IngestlOn) 6 Procedure 61 PrelImmary dlstIllatlOn 6 1 1 Place 400 ml distIlled water m the distIllmg flask 6 2 Colonmetnc DetermInatlOn 6 2 1 Prepare fluonde standards In the range 0 to 1 40 mg/l by dIlutIng appropnate quantitIes ofstandard fluonde solutlOn (54) to 50 ml WIth dIstIlled water 6 1 2 6 1 3 6 14 6 1 5 6 1 6 6 1 7 61 8 6 1 9 Carefully add 200 ml conc H2S04 and SWIrl untIl contents are homogeneous Add 25 to 35 glass beads, connect the apparatus (FIgure 1) makmg sure all Jomts are tIght Heat slowly at first, then as rapIdly as the effiCIency of the condenser wIll permIt (dIstIllate must be cool) untIl the temperature of the flask contents reaches exactly 180·C Discard the dIstIllate ThiS process removes fluonde contammatlOn and adjusts the aCId-water ratlO for subsequent dlstillatlOns Cool to 120·C or below Add 300 ml sample, mIX thoroughly, dIstIll as In 6 1 4 untIl temperature reaches 180·C Do not heat above 180·C to prevent sulfate carryover Add Ag2S04 (5 2) at a rate of 5 mg/mg CI when hIgh chlonde samples are dIstIlled Use the sulfunc aCid solutlOn m the flask repeatedly untIl the contamInants from the samples accumulate to such an extent that recovery IS affected or mterferences appear In the distIllate Check penodically by distIllIng standard fluonde samples High fluonde samples may reqUIre that the stIll be flushed by using dIstIlled water and combInIng dIstIllates 340 1-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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