Draft Data Validation Plan Review Form (Page 3 of 29) in pdf

Draft Data Validation PRF-Tier II

Date: March 2, 2004

Page 3

Revision: 4.0

1.0

Volatile Organic Data Review

Initial Calibration

Organic methods rely on an Initial Calibration in which 5-9 different concentrations of all target analytes are analyzed to

establish a “working range” for sample analysis. The results of this initial calibration may be used for a period of weeks in

which Initial Calibration Verification (ICV) Quality Control (QC) samples and Continuing Calibration Verification (CCV) QC

samples will be analyzed to confirm the system is still operating as it was during the Initial Calibration. Problems with the Gas

Chromatograph (GC) column (e.g., organic “junk” accumulating in the end) may require that the end of the column be clipped

off. As the retention time data is modified from this action, the need for a new initial calibration will be triggered. Samples

from this point on must all refer back to this new initial calibration date.

1.1

Is the GC/MS system hardware-tuned to meet the

Provide details on which ion abundance is out of compliance. In

criteria for 5-50 ng injection or purging of

addition, list all affected sample IDs:

4-bromofluorobenzene (BFB) prior to sample analysis?

Note: The ion abundance criteria used in this checklist is from

SW-846, Method 8260B. The U.S. EPA’s National Functional

Guidelines have different criteria.

m/z

Ion Abundance Criteria

15% to 45% of mass 95

30% to 60% of mass 95

Base peak, 100% relative abundance

5% to 9% of mass 95

173

0% to <2% of mass 174

174

>50% of mass 95

175

5% to 9% of mass 174

176

>95% but <101% of mass 174

177

5% to 9% of mass 176

Action: If the initial tune was not performed correctly, all data

generated using this initial calibration should be qualified “R.”

1.2

Has the GC/MS system hardware been tuned to meet

BFB tuning criteria within 12 hours prior to sample

analysis?

Note: Tuning is valid up to 12 hours after tuning analysis.

Assess whether the laboratory tuned the instrument at the

required time. If necessary, obtain a run log chart from the

laboratory to confirm the time of tuning.

Action: If the tune was not performed at the required time, the Data

Validator may qualify all data as “R” or “J.”

1.3

Was the initial calibration performed with a minimum of

Calibration Date:

five concentration levels for each target analyte?

Instrument ID:

Note: An additional data source on calibration procedures is

the laboratory’s QAP.

Sample ID:

Action: If the initial calibration did not include at least five different

Calibration Concentrations:

concentration levels, require that the laboratory provide an

explanation. The Data Validator may, at his or her discretion,

qualify the data as “J” or “R,” depending on the number and

concentration range of the calibration standards. This information

should be included in the bench sheets provided by the laboratory.

If it is not, the laboratory should be notified and information

submitted to the agency.

Draft Data Validation Plan Review Form Page 3

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