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Methods for Chemical Analysis of Water and Wastes

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Methods for Chemical Analysis of Water and Wastes ( methods-chemical-analysis-water-and-wastes )

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OXYGEN, DISSOLVED Method 360.2 (Modified Winklei', Full-Bottle Technique) STORET NO. 00300 1 Scope and ApplIcatiOn 11 This method is applIcable for use with most wastewaters and streams that contam mtrate mtrogen and not more than 1mg/l offerrous iron Other reducmg Of oXidlZlng matenals should be absent If 1 ml of fluonde solutiOn IS added before aCidifymg the sample and there is no delay m titratiOn, the method is also applIcable m the presence of 100-200 mg/l fernc iron 12 The Dissolved Oxygen (DO) Probe techmque gives comparable results on all samples types 13 The aZide modificatiOn is not applIcable under the followmg conditiOns (a) samples contammg sulfite, thiOsulfate, polythiOnate, appreCiable quantities of free chlorme or hypochlonte, (b) samples high m suspended solIds, (c) samples contammg orgamc substances which are readl1y oXidized m a highly alkalme solutiOn, or which are oXidized by free iOdme m an aCid solutiOn, (d) untreated domestic sewage, (e) biOloglCal flocs, and (f) where sample color mterferes with endpomt detectiOn In mstances where the aZide modificatiOn is not apphcable, the DO probe should be used 2 Summary of Method 21 The sample is treated with manganous sulfate, potasslUm hydrOXide, and potasslUm iOdide (the latter two reagents combmed m one solutiOn) and finally sulfunc aCid The mitial preCipitate of manganous hydrOXide, Mn(OH)2' combmes with the dissolved oxygen m the sample to form a brown preCipitate, manganic hydrOXide, MnO(OH)2 Upon aCidificatiOn, the mangamc hydrOXide forms mangamc sulfate which acts as an oXidizmg agent to release free iOdme from the potasslUm iOdide The iOdme, which is stOlchiOmetncally eqUlvalent to the dissolved oxygen m the sample is then titrated with sodlUm thiOsulfate or phenylarsme oXide (PAO) 3 Interferences 31 32 3 3 There are a number ofmterferences to the dIssolved oxygen test, mcludmg oXldlzmg and reducmg agents, mtrate iOn, ferrous iron, and orgamc matter V anous modificatiOns of the ongmal Wmkler procedure for dissolved oxygen have been developed to compensate for or elImmate mterferences The Alsterberg modification is commonly used to successfully elImmate the mtnte mterference, the Rideal-Stewart modificatiOn is deSigned to elImmate ferrous iron mterference, and the Thenault procedure is used to compensate for high concentratiOn oforgamc matenals Most of the common mterferences m the Wmkler procedure may be overcome by use of the dissolved oxygen probe Approved for NPDES Issued 1971 3602-1

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