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9.215 9216 9217 9218 9.219 92110 92 111 Add a second portion of 5 ml PDCA-chloroform reagent (771) and shake vigorously for 2 mmutes Allow the phases to separate and combme the chloroform phase With that obtamed m step (9 2 1 4) Determine the pH ofthe aqueous phase and adjust to 4 5 Repeat step (9 2 1 4) agam combmmg the solvent extracts Readjust the pH to 5 5, and extract a fourth tlme Combme all extracts and evaporate to dryness on a steam bath Hold the beaker at a 45 degree angle, and slowly add 2 ml of conc dlstl1led mtnc aCid, rotatmg the beaker to effect thorough contact of the aCld With the residue Place the beaker on a low temperature hotplate or steam bath and evaporateJust to dryness Add 2 m1 ofmtnc aCid (1 1) to the beaker and heat for 1 mmute Cool, quantitatively transfer the solutlOn to a 10 ml volumetnc flask and bnng to volume With dlstl1led water The sample IS now ready for analySIS 9.22 Prepare a callbratlOn curve by plottmg absorbance versus the concentratlOn of the metal standard (ug/l) m the 200 ml extracted standard solutlOn To calculate sample concentratlOn read the metal value m ug/l from the callbratlOn curve or directly from the readout system of the mstrument If dl1utlOn of the sample was requITed use the followmg equatlOn (C+B) mg/l metal m sample = Z C where Z = B = C = ug/l ofmetal m dl1uted allquot from callbration curve ml ofdelOmzed distilled water used for dl1utlon ml ofsample allquot 93 Furnace Procedure Furnace deVlces (flameless atomlzatlOn) are a most useful means of extendmg detection llmlts Because of differences between vanous makes and models of satisfactory mstruments, no detal1ed operatmg mstuctlOns can be given for each mstrument Instead, the analyst should follow the mstructlOns provided by the manufacturer of hiS particular mstrument and use as a gUIde the temperature settmgs and other mstrument conditions llsted on the mdivldual analYSIS sheets which are recommendedforthePerkin-ElmerHGA-2100 Inaddition,thefollowmgpomtsmaybe helpful 93 1 With flameless atomization, background correctlOn becomes of high Importance especially below 350 nm Tills IS because certam samples, when atomized, may absorb or scatter llght from the hollow cathode lamp It can be caused by the presence of gaseous molecular speCies, salt partlCules, or smoke m the sample MET ALS-16PDF Image | Methods for Chemical Analysis of Water and Wastes
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