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Analyzing Be (in HNO3 and HF) by GFAAS

Currently our lab owns an AA800 Graphite Furnace.  We anlayze various trace metals by EPA Method 29, which requires a filter digestion using HNO3 and HF.  We have found that when we use the recommended conditions for the different steps in the analysis program, we receive a 0% spike recovery and a lower than usual concentration on a known concentration.

Is there anyone out there using an AA800 and have had difficulty analyzing Be in a HNO3/HF solution?  Not sure what the drying, pyrolysis, and atomization should be in the method.  The recommended conditions do not work.

I currently have:

Temp:          Ramp:          Hold:

100               5                    50

120               30                  10

1500             1                    5

2400             0                    5

2500             1                    5

Sample at 10µl,  Diluent at 14µl

Matrix modifier at 5µl Mg(NO3)2

Thank you.

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