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Page 2 <br /> CRA MEMORANDUM <br /> SAMPLE HOLDING TIME AND PRESERVATION <br /> The sample holding time criteria for the analyses are summarized in Table 2. Sample chain of custody <br /> documents and analytical reports were used to determine sample holding times. All samples were <br /> prepared and analyzed within the required holding times. <br /> All samples were properly preserved and delivered on ice and stored by the laboratory at the required <br /> temperature(0-6°C). <br /> GAS CHROMATOGRAPHY/MASS SPECTROMETER(GC/MS)-TUNING AND MASS CALIBRATION <br /> (INSTRUMENT PERFORMANCE CHECK) -VOLATILE ORGANIC COMPOUNDS(VOCS) <br /> GC MS <br /> Prior to analysis,GC/MS instrumentation is tuned to ensure optimization over the mass range of interest. <br /> To evaluate instrument tuning,the volatile method requires the analysis of the specific tuning compound <br /> bromofluorobenzene(BFB). The resulting spectra must meet the criteria cited in the methods before <br /> analysis is initiated. Analysis of the tuning compound must then be repeated every 12 hours throughout <br /> sample analysis to ensure the continued optimization of the instrument. <br /> Tuning compounds were analyzed at the required frequency throughout the volatile analysis periods. All <br /> tuning criteria were met;indicating that proper optimization of the instrumentation was achieved. <br /> GC/MS INITIAL CALIBRATION-VOCS <br /> To quantify compounds of interest in samples,calibration of the GC/MS over a specific concentration range <br /> must be performed. Initially,a five-point calibration curve containing all compounds of interest is analyzed <br /> to characterize instrument response for each analyte over a specific concentration range. Linearity of the <br /> calibration curve and instrument sensitivity are evaluated against the following criteria: <br /> i) All relative response factors(RRFs)must be greater than or equal to 0.05 <br /> ii) The percent relative standard deviation(RSD)values must not exceed 30.0 percent or a <br /> minimum coefficient of determination of 0.99 if quadratic equation calibration curves are <br /> used <br /> The initial calibration data for VOCs was reviewed. All compounds met the above criteria for sensitivity <br /> and linearity. <br /> GC/MS CONTINUING CALIBRATION-VOCS <br /> To ensure that instrument calibration is acceptable throughout the sample analysis period,continuing <br /> calibration standards must be analyzed and compared to the initial calibration curve every 12 hours. <br /> The following criteria were employed to evaluate continuing calibration data: <br /> i) All RRF values must be greater than or equal to 0.05 <br /> ii) Percent difference(%D)values must not exceed 25 percent <br />