Quality Assurance Project Plan Including Sampling And Analysis Plan (Page 39 of 67) in pdf

Hunters Point Shipyard Parcel F ESTCP Demonstration Plan

Appendix A: Quality Assurance Project Plan

univariate and/or multivariate techniques to address both spatial and temporal differences in community

structure (US EPA 1992).

A.3.4.2.3 ERDC PCB Congener Analysis

Following cleanup, extracts will be transferred to solvent-rinsed 2 mL vials, internal standards

pentachloronitrobenzene and 4,4’-dibromobiphenyl (Restek, Bellafonte, PA), will be added at a final

concentration of 50 ng/mL, and the final volume adjusted to 1 mL. Extracts will be analyzed following

EPA Method 8082 (US EPA, 1996) using a Hewlett-Packard 5890 series II gas chromatograph equipped

with electron capture detectors and dual columns using 2µl injection volume. Agilent (Wilmington, DE)

DB-5MS and Supelco (Bellefonte, PA) SPB-octyl columns, both 30 m, 0.25 mm ID, 0.25-µm-film

thickness, will be used to achieve separation. Initial oven temperature will be 130 ºC (2 minute hold

time), ramped to 255 ºC at 1.4 ºC/minute. The temperature will be then raised to 265 ºC at a rate of

18º/minute and held for 9 minutes resulting in a total run time of 100.8 minutes. Injector and detector

temperatures will be 255 and 305 ºC, respectively. The carrier gas mix will be helium (1.35 mL/minute)

and 5% methane in argon (65 mL/min) gas. Data for co-eluting peaks will be presented as a sum of

congeners. Only congeners with all data replicates above MDL will be included.

A.3.4.3 Analytical/Testing Methods for UMBC

A.3.4.3.1 Measurement of Aqueous and Suspended Particulate PCB Concentrations in Field Water

The XAD-2 resin and the glass fiber filters will be extracted in a soxhlet extraction system with a 50%

acetone and 50% hexane. The soxhlet extraction procedure will follow EPA SW846 method 3540C. The

extract will be concentrated in a Kuderna Danish evaporator and a N

blowdown apparatus. The PCB

sample will be cleaned up from organic interferences using a deactivated silica gel column following EPA

SW846 method 3630C. Sulfur interferences will be removed by contacting with activated copper

following EPA SW846 method 3660B. The PCB analysis of the resulting extracts will be performed

according to Section A.3.4.3.2.

A.3.4.3.2 PCB Desorption Characteristics of Field Sediments

PCB desorption characteristics of subsamples from a homogenate of sediment cores from each plot will

be evaluated. The desorption tests will follow previously published methods (Ghosh et al. 2003a).

A.3.4.3.3 UMBC PCB Congener Analysis

PCB congener specific analysis will be performed using a modified EPA SW846 Method 8082. An

Agilent gas chromatograph (model 6890) with a fused silica capillary column (HP-5, 60 m x 0.25 mm ID)

and a micro electron capture detector will be used for analysis. A 5-level PCB calibration table is

prepared using a known PCB mixture containing 250 µg/L of Aroclor 1232, 180 µg/L of Aroclor 1248

and 180 µg/L of Aroclor 1262 yielding a total PCB concentration of 610 µg/L. The known PCB

calibration mixture has been already obtained from the EPA's National Health and Environmental Effects

Research Laboratory in Grosse Ile, Michigan. Concentrations of individual PCB congeners in this mixture

have been obtained from Mullin (1994). Two internal standards are used: PCB 30 (2,4,6-

trichlorobiphenyl) and PCB 204 (2,2’,3,4,4’,5,6,6’-octachloro biphenyl), which are not present in

commercial Aroclor mixtures. Using this protocol, 92 PCB congeners or congener groups could be

identified and quantified. With this analytical method, there are some coeluting PCB peaks in the

analysis. Where this occurs, coeluting peaks are calibrated as sum of congeners.

A.3.4.4 Analytical/Testing Methods for BDO

Page A-

of A-67

Quality Assurance Project Plan Including Sampling And Analysis Plan Page 39

Related Articles

Related forms

Related Categories