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7. 6 1 7 Flve-gallon Carboy fume-trap 6 1 880°C Heatmg bath 6 1 9 Colonmeter eqUlpped wlth 50 mm tubular flow cell and 630 nm filters 6 1 10 Recorder eqUlpped wlth range expander 6111 Vacuumpump Reagents 7 1 72 73 74 7S 7.6 77 78 79 710 7 11 Dlstl1led water Speclal precautlOn must be taken to msure that dlstl1led water IS free of ammOnIa Such water IS prepared by passage of dlstl1led water through an lOn exchange column compnsed of a mlxture of both strongly aCldlC cation and strongly baSiC anIon exchange resms Furthermore, smce organIC contammatlOn may mterfere with thlS analysls, use of the resm Dowex XE-75 or eqUlvalent whlCh also tends to remove organIc ImpuntiesISadvlsed TheregeneratlOnofthe10nexchangecolumnshouldbecarnedout accordmg to the mstructlOn of the manufacturer NOTE 1: All solutlOns must be made usmg ammonIa-free water Sulfunc aCid As It readl1y absorbs ammOnIa, special precautlOn must also be taken wlth respecttoItSuse DonotstorebottlesreservedforthlsdetermmatlOnmareasofpotential ammOnIa contammatlOn EDT A (2% solutlOn) Dlssolve 20 g dlsodiUm ethylenedlamme tetraacetate m 1 hter of distilled water Adjust pH to 10 5-11 wlth NaOH (74) SodiUm hydrOXide (30% solutlOn) Dlssolve 300 g NaOH m 1hter ofdlstilled water NOTE 2: The 30% sodiUm hydroxlde should be sufficlent to neutrahze the dlgestate In rare cases It may be necessary to mcrease the concentratlOn of sodiUm hydroxlde m thlS solutlOn to msure neutrahzatlOn of the dlgested sample m the manIfold at the water Jacketed mlxmg colI SodiUm nItroprusslde, (005% solutlOn) Dlssolve 0 5 g Na2Fe(CN)sN0-2H20 m 1 hter dlstllled water Alkahne phenol reagent Pour 550 ml hqUld phenol (88-90%) slowly wlth mlxmg mto 1 hterof40%(400gperhter)NaOH Coolanddlluteto2hterswlthdistl1ledwater Sodmm hypochlonte (1 % solutlOn) Dl1ute commercial "Clorox"-200 ml to 1 hter wlth dlstilled water Avallable chlonne level should be approxlmately 1% Due to the mstab111ty ofthls product, storage over an extended penod should be aVOlded Dlgestant mlxture Place 2 g red HgO m a 2 hter contamer Slowly add, wlth stirnng, 300 ml ofacld water (100 ml H2S04 + 200 ml H20) and stir untl1 cool Add 100 mllO% (10 g per 100 ml) K2S04 Dl1ute to 2 hters wlth conc sulfunc aCld (approxlmately 500 ml at a time, allowmg time for coolmg) Allow 4 hours for the preclpitate to settle or filter through glass fiber filter Stock solution Dlssolve 4 7193 g of pre-dned (1 hour at 105°C) ammOnIum sulfate m dlstl1ledwateranddl1uteto10htermavolumetncflask 10ml= 10mgN StandardsolutlOn Dl1ute100mlofstocksolutlOn(79)to1000milOml= 001mgN Usmg the standard solutlOn (7 10), prepare the followmg standards m 100 ml volumetnc flasks 351 1-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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