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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must be accomplished by analyzing a second 10mL aliquot of the pH adjusted filtrate (9 1) spiked wIth Cr6+ (7 8) The amount of spIke added should double the concentration found In the original aliquot Under no cIrcumstance should the Increase be of less than 30,ug Cr6+/L To verify the absence of an Interference the spIke recovery should be between 85% and 115% 10 2 If the additIon of the spIke extends the concentratIon beyond the range of the calibratIOn curve, the analYSIS solutIon should be dIluted With blank solutIon and the calculated results adjusted accordingly 10 3 If the VerifIcatIon indIcates a suppressIve Interference, the sample should be dIluted and reanalyzed 11 Analytical Notes 11 1 Nitrogen should not be used as a purge gas because of possIble CN band Interference 11 2 The use of pyrolytlc graphIte should be avoIded when possIble Generally, pyrolytlc graphIte resulted In a more limIted analytIcal working range and In some SItuatIOns an enhancement effect 11 3 PIpet tIpS have been reported to be a possIble source of contaminatIOn (See part 5 2 9 of the AtomIC AbsorptIon Methods sectIon of thIs manual) 11 4 The method of standard addItIon should not be requIred In as 6 much as the Cr + has been separated from the original sample solutIon and redIssolved In a uniform matrix haVIng an absorptIon response cOincIdent to the calibratIon curve 11 5 Data to be entered Into STORET (No 01032) must be reported as ,ug/L 12 PrecIsion and Accuracy 12 1 In a Single laboratory (EMSL) uSing a mIxed industrial-domestIc Cr +/L and spIked WIth a concentratIon of 50,ug Cr6+/L the standard deVIatIons were ..t 1 0 and ± 27, respectIvely WIth a spike recovery of 94% 12 2 Recoveries of a 40 ,ug Cr6+/L spIke In diluted tannery and platIng waste effluents were 96% and 93%, respectIvely 12 3 USing CinCinnatI, Ohio tap water spiked at concentratIons of 5,10, and 50,ug Cr6+/L the standard deVIatIons were ± 0 7, ±O 6, and ±O 6 respectIvely SpIke rec-overy at all three levels was 102% 12 4 A 1000,ug Cr3+/L standard solutIon analyzed by thIS method YIelded a result of 8,ug Cr6+/L WIth a relatIve standard deVIatIon of 19% 12 5 The data from 5 ,ug Cr6+/L tap water spIke was used to calculate method detectIon limIt (MOL) WIth 99% confIdence as deSCribed In 'Trace Analyses for Wastewater," J Glaser, 0 Foers!, G McKee, S Quave, W Budde, EnVironmental SCIence and Technology Vol 15, Number 12, page 1426, December 1981 The calculated MOL for CinCinnati drinking water IS 2 3,ug/L waste effluent containing 22 ,ug 6 21853 Dec 1982 ,

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