Draft Data Validation Plan Review Form (Page 20 of 29) in pdf

Draft Data Validation PRF-Tier II

Date: March 2, 2004

Page 20

Revision: 4.0

4.0

Semi-Volatile 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 8270C to identify the presence of target compounds is to compare the retention time of unknown

compounds in a sample to the retention time of knowncompounds in the calibration standard. The Relative Retention Time

(RRT) of the compound in the sample must be within +/- 0.06 units of the RRT of the initial calibration standards. In addition,

the mass spectra of the standard must match the mass spectra of the calibration standard within certain tolerances . 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. Results for unknown compounds in samples are compared to an electronic ”library”

of compounds to determine if all results (retention time and mass spectra) match within specified tolerances to a library

compound (or at least to a certain type of compound of specific size).

4.1

Are the RRTs of reported compounds in the ICV within

+/- 0.06 RRT units (minutes) of the RRT for the initial

calibration?

Action: Use this information in conjunction with the mass spectral

analysis information to qualify data. If target compound

identification is in error, qualify that compound as “R.”

4.2

Check the sample compound spectra against spectral

data of the standard. All ions in the standard mass

spectra at a relative intensity of 10% must also be in the

identified sample compound.

Action: Use this information in conjunction with the mass spectral

analysis information to qualify data. If target compound

identification is in error, qualify that compound as “R.”

4.3

Check the sample compound spectra against spectral

data of the standard. The relative intensity of the ions in

the sample must agree within +/- 20% of the value

obtained from the standard spectrum.

Action: Use this information in conjunction with the mass spectral

analysis information to qualify data. If target compound

identification is in error, qualify that compound as “R.”

Draft Data Validation Plan Review Form Page 20