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CRA MEMORANDUM Paget <br /> Two samples required identification verification when differences were observed between the COC and <br /> sample labels. Sample 1-629-5-COC had a sample time of 10:19 and the sample label 10:35; 10:35 was <br /> verified as the correct sample time by the sampler. Sample 1-B38-5 was incorrectly written as 1-1338 on the <br /> sample label, 1-B38-5 was verified as the correct sample name by the sampler. <br /> 3.0 Gas Chromatography/Mass Spectrometer (GC/MS)—Tuning and Mass Calibration <br /> (Instrument Performance Check)—Volatile Organic Compounds (VOCs) <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 /> 4.0 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 minimum <br /> coefficient of determination of 0.99 if quadratic equation calibration curves are used <br /> The initial calibration data for VOCs was reviewed. All compounds met the above criteria for sensitivity and <br /> linearity. <br /> 5.0 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 /> H. Percent difference (%D)values must not exceed 25 percent <br /> EOUN EMMOWENT OWOMNIIYEMPWWR <br />