Quality Assurance Project Plan Including Sampling And Analysis Plan (Page 40 of 67) in pdf

Hunters Point Shipyard Parcel F ESTCP Demonstration Plan

Appendix A: Quality Assurance Project Plan

The analytical method chosen for BDO measurements was selected to meet the ecological benchmark and

is based on the National Oceanic and Atmospheric Administration (NOAA) National Status and Trends

(NS&T) program. The critical data compound list of PCB congeners in Table A-7, with required

reporting limits and detection limits, will be used if the archived sample splits are analyzed. Table A-8

provides a list of applicable laboratory SOPs.

A.3.4.4.1 Analysis of PCB Congeners in Archived Sample Splits

If it is determined that critical data is to be obtained from the archived tissue sample splits, BDO will

perform the analysis of PCBs congeners according to low-level methods developed for the NOAA Status

and Trends Program (Lauenstein and Cantillo, 1993). These procedures are detailed in BDO SOPs 5-190

and 5-128. Ideally, 30 g of sample tissue is homogenized by macerating the tissue using a tissuemizer and

75 mL of dichloromethane until a uniform slurry is attained with no visible non-uniform “chunks.” This

procedure is repeated once and the extracts decanted between tissumizing steps. A third extract is

accomplished by adding 50 mL of dichloromethane to the tissue in the extraction vessel and shaking for

0.5 hours. The extract is purified and concentrated under nitrogen to a pre-injection volume of

approximately 1.0 mL. Extracts for PCB congener analysis are solvent exchanged into hexane prior to

analysis. Masses of tissue as low as 1 g can be extracted using this procedure; if less than 30 g is available

then the entire sample will be extracted and the detection limits adjusted accordingly.

Laboratory analyses must be performed using instruments and columns that are capable of achieving the

sensitivity and separation to achieve the reporting limits defined for PCB congeners.

•

Samples are quantified using the method of internal standards.

•

PCB compounds are analyzed by using a GC/ECD with a confirmatory column to

qualitatively verify peak identification.

•

Only PCB peaks confirmed on both columns will be considered “hits.”

•

Sample data will not be surrogate corrected.

•

No data will be blank-corrected.

Manual integrations are also a key element of low-level organic compounds analyses and are

implemented routinely for low-level GC/ECD data to separate data system baseline integration features

from peaks that can be distinguished at greater than 3:1 signal:noise ratio. Manual integration:

•

Will not be used preferentially for QC samples and must not be used to satisfy QC criteria

requirements;

•

Must be identified, and must be signed and dated by the analyst; and,

•

Must be justified in each data package and in the case narratives. Due to constraints of the

software acquisition software, each manually integrated value is not flagged.

Sample cleanup is a critical component of low-level organic compounds analyses; therefore, a variety of

cleanup options may be employed to purify the sample extracts. Sample cleanup options are incorporated

into the sample processing SOPs; all sample cleanup procedures will be documented. Sample cleanup

procedures will be implemented on a batch-wide basis to ensure comparability of results and to assess

cleanup effects on QC samples.

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Quality Assurance Project Plan Including Sampling And Analysis Plan Page 40

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