Page 93 - Geochemistry of Oil Field Waters
P. 93

ATOMIC ABSORPTION METHODS                                             81


            Reagents.  The necessary reagent is a standard zinc solution: obtain commer-
            cially or dissolve 0.500 g of  zinc metal in a minimum volume of  (1 +1) HC1
            and dilute to 1 liter with  1% (v/v) HCl.  1 ml  of solution contains 500 pg of
            zinc.

            Preliminary  calibration.  Prepare standard zinc solutions containing 0.2-1.0
            pg/ml using the standard zinc solution and 50-ml volumetric flasks. Aspirate
            these  standards and  a  blank  as recommended  in  the calcium  method  and
            determine the absorbance at a wavelength of  2138.6 a.


            Procedure.  Transfer  an aliquot  containing  about  10 pg  of  zinc to a 50-ml
            volumetric  flask.  Dilute  to volume and aspirate. Calculate the approximate
            sample concentration  from  the preliminary  calibration  readings  and deter-
            mine the aliquot size that will contain 10 pg of  zinc.
              Transfer  equal  aliquots  containing  about  10 pg  of  zinc  to three  50-ml
            volumetric flasks. Add  no zinc standard to the first flask,  10 pg of the zinc
            standard  to the  second  flask,  and  20 pg  to the  third.  Dilute  to volume.
            Aspirate and record the absorbance readings for each sample.

            Calculations.  See  calculations under  “Lithium”  in the flame spectrophoto-
            metric section, Fig. 3.3, or Table 3.XI:




            Precision.  In a single laboratory using oilfield water samples containing con-
            centrations of  27 and 120 mg Zn+2 /1,  the standard deviations were +1. The
            recoveries were 103.5% and 102.3%, respectively.

            Lead (1)

              Lead  is  determined  at  the  2833.1  A  wavelength  with  an air-acetylene
            flame.

            Reagents. The necessary reagent is a standard lead solution: obtain commer-
            cially  or  dissolve 1.598 g of  lead  nitrate,  Pb(N03)2, in 1 liter of  1% (v/v)
            HN03. 1 ml of solution contains 1,000 pg of lead.

            Preliminary  calibration.  Prepare  standard  lead  solutions  containing  2-10
            pg/ml using the standard lead solution and 50-ml volumetric flasks. Aspirate
            these  standards and  a  blank  as recommended  in  the calcium  method  and
            determine the absorbance at a wavelength of  2833.1 8.

            Procedure.  Transfer  an aliquot  containing  100 pg  of  lead to a 50-ml volu-
            metric  flask.  Dilute  to  volume  and  aspirate.  Calculate  the  approximate
            sample  concentration  from  the preliminary  calibration  readings  and deter-
            mine the aliquot size that will contain 100 pg of lead.
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