Draft Data Validation Plan Review Form Page 10
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29Draft Data Validation PRF-Tier II
Date: March 2, 2004
Page 10
Revision: 4.0
3.0
Volatile Organic Data Review - Internal Standards
3.1
Are area counts available to determine if the sample
Record actions taken, such as when the facility was contacted,
internal standards are within criteria as compared to the
names of facility personnel and when the information was
12-hour standard?
submitted:
Action: If the data is not present, the Data Validator should request
that the facility obtain the data from its laboratory. If the data is not
available, the Tier II Data Validator may qualify data based upon
professional judgement.
3.2
Is the area counts for the internal standards in a sample
outside of the +50% range of the area counts of the 12-
hour standard?
Action: All positive results associated with an internal standard
outside of the criteria should be qualified as “J.”
Non-detected compounds quantified using an internal standard
whose area count is greater than 100% should not be qualified.
Non-detected compounds quantified with an internal standard
whose area count is less than 50% of the associated calibration
standard should be qualified as “UJ.”
If extremely low area counts are associated with the internal
standards, qualify all associated target compounds as “R.”
3.3
Do any internal standards retention times vary by more
than 30 seconds (0.5 minutes) as compared to the 12-
hour standard?
Action:
The Tier II Data Validator should request raw data
chromatograms and assess whether false positives or negatives
exist for any target compounds associated with that internal
standard. Based upon this evaluation, the data may either be
qualified as “J” or “R” using professional judgement.
4.0
Volatile Organic Data Review - Target Compound Identification
Target Compound Identification
One of the primary goals of sample analyses is to accurately identify the presence of target compounds. The procedure used
by SW-846, Method 8260B to identify the presence of target compounds is to compare the retention time of unknown
compounds in a sample to the retention time of known compounds in the calibration standard. The Relative Retention Times
(RRT) of the compounds in the samples must be within +/- 0.06 RRT units of the RRTs of the same compound in the initial
calibration standards. In addition, the mass spectra of the standard must match within certain tolerances of the mass spectra
of the calibration standard. For example, all ions in the standard mass spectra at a relative intensity of 10% must also be
present in the sample spectrum. In addition, the relative intensities of the ions in the sample must agree within +/- 20%
between the sample and the standard spectra. Ions that are present at greater than 10% in the sample mass spectrum, but
not present in the standard spectrum, must be considered and accounted for.
4.1
Are the Relative Retention Times (RRTs) of reported
compounds within+/- 0.06 RRT units of the RRT for the
same compounds in the initial calibration?
Action: Use this information in conjunction with the mass spectral
analysis information to qualify data. If a target compound
identification is in error, qualify that compound as “R.”
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