Draft Data Validation Plan Review Form (Page 13 of 29) in pdf

Draft Data Validation Plan Review Form Page 13

Draft Data Validation PRF-Tier II

Date: March 2, 2004

Page 13

Revision: 4.0

1.0

Semi-Volatile Data Review - Initial Calibration

Initial Calibration

Semi-volatile 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 the initial calibration will be confirmed by Continuing Calibration Verification (CCV) Quality Control (QC)

samples. 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 must be triggered. Samples from this point on may all refer back to this new initial calibration date.

1.1

Is the Gas Chromatograph/Mass Spectrometer (GC/MS)

Indicate samples affected and qualification of sample results:

system tuned to meet the criteria for 50 ng injection of

Decafluorotriphenylphosphine (DFTPP) prior to sample

analysis?

Note: The ion abundance criteria used in this checklist is

from SW-846, Method 8270C. U.S. EPA’s National Functional

Guidelines have slightly different criteria.

Mass

Ion Abundance Criteria

30% to 80% of mass 198

<2% of mass 69

127

25% to 75% of mass 198

197

<1% of mass 198

198

Base peak, 100% relative abundance

199

5% to 9% of mass 198

275

10% to 30% of mass 198

365

>0.75% of mass 198

441

Present but less than mass 443

442

>40-110% of mass 198

443

15% to 24% of mass 442

Note: All ion abundances must be normalized to m/z 198

(except the ones that are normalized to m/z 69, as noted

above).

Action: If a base peak, other than m/z 198 is used for

normalization, then qualify all associated data as “R.”

If the ion abundance criteria is not met then judgement should be

used to qualify associated data as “J” or “R.”

1.2

Has the GC/MS system hardware been tuned to meet

DFTPP 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(s). 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.”

Draft Data Validation Plan Review Form Page 13

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