Draft Data Validation Plan Review Form Page 15
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29Draft Data Validation PRF-Tier II
Date: March 2, 2004
Page 15
Revision: 4.0
1.0
Semi-Volatile Data Review - Initial Calibration
1.6
A. Is the %RSD for individual analytes (except CCCs, see
Additional Information: The laboratory has the option of using
Table 3 and question 1.7 ) in the initial calibration below
linear regression or quadratic calibration equations for individual
%15?
analytes that don’t meet the 15% criteria. Information concerning
B. If not, are alternate calibration equations used for
the acceptability for these alternate calibration equations must be
those analytes not meeting the 15% criteria?
supplied by the laboratory.
C. Is the average %RSD for all analytes below 15%?
The laboratory also has the option to re-analyze a particular
calibration standard if it is suspected that the standard has
Note: Reference Method 8000, Section 7.5.1.2. Method 8000
degraded. In addition, the lab may remove either the low level or
specifies a linearity criterion of 20% RSD. That criterion
high level calibration point from the %RSD analysis for up to two
pertains to GC and HPLC methods other than GC/MS. Method
individual analytes to bring the %RSD within criteria. If a low
8270C requires 15% RSD as evidence of sufficient linearity to
level standard is removed to improve the %RSD, the detection
employ an average relative response factor (Avg. RRF).
limit should be raised accordingly. If the high level standard is
removed, the linear range is shortened for that analyte.
Action: If the %RSD for each analyte is below 15% RSD, no
qualification is necessary.
If certain individual analytes have %RSDs above the criteria, but
the average of all the analytes is below 15% RSD, then the
If one or two analytes had a low level calibration point removed to
average RRF is acceptable for use.
better the %RSD calculation, and the detection limit was not
raised, qualifiy all undetected data as estimated. Positive data
Record the analytes in the initial calibration that used an
should not be qualified.
alternate calibration curve or had %RSD values greater than
15%.
If the average RSD for all calibration analytes is above 15% and
average response factors are used, qualify all positive and
undetected data for those individual analytes that exceeded the
15% RSD criteria requirement as estimated .
Additional qualification, including rejection of data, may be
warranted if other quality control criteria is not within requirements.
1.7
Do the Calibration Check Compounds (CCC) listed in
Table 3 in the initial calibration standards meet a percent
Relative Standard Deviation (%RSD) of 30% or less?
Action: If any of the CCCs have a %RSD of greater than 30%, the
system is considered too unstable for analysis. The system
should undergo corrective action.
If the analysis was not
terminated, qualify all non-detected compounds as “R” and any
associated positive results based upon the best professional
judgement of the validator.
Table 3
Calibration Check Compounds (CCC) for SW-846, Method 8270C
Base/Neutral Fraction Com pounds
Acid Fraction Com pound
Acenapthene
4-Chloro-3-methylphenol
1,4-Dichlorobenzene
2,4-Dichlorophenol
Hexachlorobutadiene
2-Nitrophenol
Diphenylamine
Phenol
Di–n -octylphthalate
Pentachlorophenol
Fluoranthene
2,4,6-Trichlorophenol
Benzo(a)pyrene
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