Draft Data Validation Plan Review Form Page 25

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Draft Data Validation PRF-Tier II
Date: March 2, 2004
Page 25
Revision: 4.0
1.0
ICP Metals Data Review - Initial Calibration
Initial Calibration
The review of initial calibration data for inorganic elements is complicated because of the lack of a prescribed procedure.
SW-846 6010B requires that the instrument be calibrated according to the instrument manufacturer’s recommendations.
Several manufacturers only require that a blank and one calibration standard be used for calibration, whereas others require
up to five standards be used to establish the calibration. Whatever method is used, the laboratory should be able to
demonstrate adequate instrument response and linear range. The laboratory should be consulted as to standard operating
procedures are required to calibrate the instrument.
1.1
Was a minimum of one standard and a blank used for
the initial calibration of the ICP instrument?
Note: SW-846, Method 6010B does not describe a sole
procedure for instrument calibration. The calibration
procedure will vary by the manufacturer’s recommended
instrument calibration procedure. It may be necessary to
consult the laboratory’s QAP or contact the laboratory for the
exact calibration procedure that is used.
Action: If the minimum number of standards were not used,
qualify all results as “R.”
1.2
Was an Initial Calibration Verification (ICV), a
Calibration Blank, and a Continuing Calibration
Verification (CCV) analyzed immediately after the initial
or daily calibration? A CCV must also be analyzed after
every tenth sample or every two hours, whichever is
more frequent.
Note: This sequence must be followed and is found in
Section 7.4 of SW-846, Method 6010B. The ICV and CCV
must be from a certified standard other than that used for the
initial calibration, and must be within the calibrated range.
Action: The ICV and CCV must be within +/- 10% percent (%R
= found/true X100) of the expected value or the analysis should
have been halted and the instrument re-calibrated. If the analysis
was not halted, qualify all results as “R.”
2.0
ICP Metals Data Review - Interference Check Samples (ICS)
Interference Check Samples (ICS)
The ICS consists of two standard solutions, an A or AB solution (solution A consists of the interferents, and solution AB
consists of the analytes mixed with the interferents). The ICS solutions are used to determine if non-target analytes (e.g.,
interfering elements) are elevating or depressing results for target metals. The ICS results can be used to demonstrate that
correction for interfering elements is not necessary at the concentrations tested or to develop Inter-element Correction
Factors (IECFs), which can be applied to sample results to account for the presence of these interfering metals.
2.1
Was an Interference Check Sample (ICS) analyzed at
the beginning and end of each analytical run or at a
minium of two every eight hours?
Note: The ICS is NOT to be analyzed before the initial
calibration verification standard.
Action: Check the run log to verify that the ICS was run in the
proper order and frequency. If discrepancies exist, consult the lab
for clarification and re-submission of the data pack. If no new
information is forthcoming, qualify all positive results using best
professional judgement.

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