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611 Sampler 6 1 2 Mamfold (AAI) or AnalytIcal Cartndge (AAII) 6 1 3 ProportlOnmg pump 6 1 4 Heatmg bath, 50°C 6.1 5 Colonmeter equIpped wIth 15 or 50 mm tubular flow cell 6 1 6 650-660 or 880 nm filter 6 1 7 Recorder 6 1 8 DIgital pnnter for A A II (optlOnal) 62 Hot plate or autoclave 6.3 ACId-washed glassware All glassware used m the determmation should be washed wIth hot 1 1 HCI and nnsed wIth dIstilled water The aCId-washed glassware should be filled wIth dIstIlled water and treated wIth all the reagents to remove the last traces of phosphorus that mIght be adsorbed on the glassware Preferably, thIS glassware should be used only for the determmation of phosphorus and after use It should be rmsed wIth dtstilledwaterandkeptcovereduntilneededagam IfthISISdone,thetreatmentwIth11 HCI and reagents IS only reqUlred occaslOnally CommercIal detergent should never be used 7 Reagents 7 1 72 73 74 7.5 Sulfunc aCId solutlOn, 5N Slowly add 70 ml of conc H2S04to approxImately 400 ml of dIstilled water Cool to room temperature and dIlute to 500 ml wIth dIstilled water Antimony potassmm tartrate SolutIon WeIgh 03 g K(SbO)C4H40 6-1/2H20, dIssolve m 50 ml dIStilled water m 100 ml volumetnc flask, dilute to volume Store at 4°C m a dark, glass-stoppered bottle Ammomum molybdate SolutIon DIssolve 4 g (NH4)6Mo7024-4H20 m 100 ml dIstilled water Store m a plastIc bottle at 4°C AscorbIc aCId, 0 1M DIssolve 1 8 g of ascorbIC aCId m 100 ml of dIstilled water The solution IS stable for about a week If prepared wIth water contammg no more than trace amounts ofheavy metals and stored at 4°C Combmed reagent (AAI) MIX the above reagents m the followmg proportions for 100 ml of the IDlXed reagent 50 ml of 5N H2S04 (7 1), 5 ml of antimony potassmm tartrate solution (7 2), 15 ml of ammomum molybdate solutlOn (7 3), and 30 ml of ascorbIC aCId solution (7 4) MIX after addItIon of each reagent All reagents must reach room temperature before they are mIxed and must be mIxed m the order gIven If turbIdIty forms m the combmed reagent, shake and let stand for a few mmutes untIl the turbIdIty dIsappears before processmg ThIS volume IS suffiCIent for 4 hours operatlOn Smce the stabIhty of thIS solutlOn IS hmited, It must be freshly prepared for each run. NOTE 1: A stable solutlOn can be prepared by not mcludmg the ascorbIC aCId m the combmed reagent If thIS 18 done, the mIxed reagent (molybdate, tartrate, and aCId) IS pumped through the dIstilled water hne and the ascorbIC aCId solutlOn (30 ml of 7 4 dtluted to 100 ml wIth dIstIlled water) through the ongmal mIXed reagent hne Sulfunc aCId solutlOn, 11 N Slowly add 310 ml conc H2S04to 600 ml dIstIlled water When cool, dIlute to 1hter 7 6 365 1-4PDF Image | Methods for Chemical Analysis of Water and Wastes
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