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PHOSPHORUS, TOTAL Method 365.4 (Colorimetric, Automated, Block Digest()r AA II) STORET NO. 00665 1 Scope and ApplicatlOn 1 1 ThIs method covers the determmatlOn of tOial phosphorus m drInkmg water, surface water and domestIc and mdustnal wastes The applicable range ofthis method IS 0 01 to 20 mgP/1 2 Summary of Method 21 ThesampleISheatedmthepresenceofsulfuricaCId,K2S04 andHgS04 fortwoandone half hours The resIdue IS cooled, dIluted to 25 ml and placed on the AutoAnalyzer for phosphorus determmatlOn 3 Sample HandlIng and PreservatlOn 3 1 Sample contamers may be of plastIc material, such as a cubitamer, Qr of Pyrex glass 3 2 If the analysIs cannot be performed the day of collectlOn, the sample should be preserved by the addItion of2 m1 ofconc H2S04 per lIter and refrIgeratlOn at 4°C 4 Apparatus 4 1 Block Digestor BD-40 42 Techmcon Method No 327-74W for Phosphorus 5 Reagents 51 52 53 54 55 56 57 MerCUriC sulfate DIssolve 8 g red merCUriC oXIde (HgO) m 50 ml of 1 4 sulfurIc aCId (10 conc H2S04 40 ml dIStilled water) and dIlute to 100 ml wIth dIstIlled water DigestlOn solution (SulfUriC aCId-mercuriC sulfate-potassmm sulfate solutlOn) DIssolve 133 g of K2S04 m 600 ml of dIstIlled water and 200 ml of conc H2S04 Add 25 ml of mercunc st'lfate SOl1,ltlOn (5 1) and dIlute to 1 lIter SulfuncaCldsolutlOn(0 72N) Add 20 ml ofconc sulfuncaCldt08000fdIstI1ledwater, mIX and dIlute to 1 lIter Molybdate/antimony solutlOn DIssolve 8 g of ammomum molybdate and 0 2 g of antImony potassmm tartrate m about 800 ml of dIstIlled water and dIlute to 1 lIter AscorbIc aCId solutlOn DIssolve 60 g of ascorbIc aCId m about 600 ml of dIstIlled water Add 2 ml ofacetone and dIlute to 1lIter DIluent water DIssolve 40 g of NaCl m about 600 ml of dIstIlled water and dIlute to 1 lIter Sulfuric aCId solutlOn, 4% Add 40 ml of conc sulfuric aCId to 800 ml of ammoma-free dIstIlled water, cool and dIlute to 1 lIter 6 Procedure Digestion 6 1 To 20 or 25 ml ofsample, add 5 ml ofdigestlOn SolutIon and mIX (Use a vortex mIxer) 6 2 Add 4--8 Teflon boIlmg chips Too many boIlmg ChIpS WIll cause the sample to boll over Pendmg approval for NPDES and Section 304(h), CW A Issued 1974 3654-1PDF Image | Methods for Chemical Analysis of Water and Wastes
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