Draft Data Validation Plan Review Form Page 27
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29Draft Data Validation PRF-Tier II
Date: March 2, 2004
Page 27
Revision: 4.0
2.0
ICP Metals Data Review - Interference Check Samples (ICS)
2.6
Are concentrations of Al, Ca, Fe and Mg in the samples
greater than in the ICS, or are other elements present
in the sample at greater than 10 ppm?
Action: Estimate the concentration produced by an interfering
element. If the estimate is greater than 2X the element’s
detection limit and greater than 10% of the reported
concentration of the affected element, qualify the affected results
as “J.”
3.0
Cold Vapor AA Method for Mercury Data Review
Calibration and Instrument Runs
SW-846, Method 7470 is used for liquid samples including the TCLP extract. Method 7471A is used for solid samples and
for sludges. The methods are subject to significant interferences from chlorides, and a pre-treatment step using
potassium permanganate is required to remove these interferences.
3.1
Was potassium permanganate solution added to
eliminate interferences (typical interferences are from
sulfide, copper, chlorides, and certain VOCs that absorb
the 253.7 nm wave length absorbed by mercury vapor)?
Note: Method 7471A states that up to 25mL of 5%
permanganate solution can be used. The amount of added
permanganate should be recorded. The same amount of
permanganate solution should be added to blanks and
calibration standards.
Action: If permanganate solution was not added, qualify all positive
results as “J” and all non-detected results as “UJ.”
3.2
Was a working standard (Continuing Calibration
Standard) of 0.1 µg/mL concentration prepared each
day?
Action: If a working standard was not prepared daily, qualify all
positive results as “J” and all undetected results as “UJ.”
3.3
Was the instrument calibrated daily (or each time the
instrument was set up) per manufacturer’s instructions,
and at SOP specified levels?
Note:
Daily
calibration
with
standards
of
varying
concentration defines the reliable “working range” of the
analysis.
Note: The Contract Lab Program requires from five to eight
calibration standards and a blank for calibration (typically,
0.0002 ppm, 0.0005 ppm, 0.001 ppm, 0.005 ppm and 0.010
ppm).
SW-846, Method 7471A requires three calibration
standards and a blank be used. The correlation coefficient for
calibration must be > 0.995 to demonstrate linearity.
Action: If the specified number of calibration standards were not
used or if the instrument was not calibrated daily, qualify all data
as “R.”
3.4
Was at least 1 blank analyzed before the calibration
standards used to establish the curve?
Action: If a blank was not analyzed qualify, all associated data as
“J.”
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