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CRA MEMORANDUM Paget <br /> The samples were properly preserved and delivered on ice and stored by the laboratory at the required <br /> temperature (0-60C). <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 Initial Calibration - Organic Analyses <br /> GC/MS <br /> To quantify VOC compounds of interest in samples, calibration of the GC/MS over a specific concentration <br /> range must be performed. Initially, a five-point calibration curve containing all compounds of interest is <br /> analyzed to characterize instrument response for each analyte over a specific concentration range. <br /> Linearity of the 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 ora minimum <br /> correlation coefficient (R) of 0.995 and minimum coefficient of determination (R2) of 0.99 if linear and <br /> quadratic equation calibration curves, respectively, are used <br /> The initial calibration data for VOCs were reviewed. All compounds met the above criteria for sensitivity <br /> and linearity. <br /> GC <br /> In order to quantify organic compounds of interest by GC, calibration of the gas chromatograph over a <br /> specific concentration range must be performed. Initially, a calibration curve consisting of a minimum of <br /> five concentration levels is analyzed for all single component compounds of interest. Linearity of the <br /> calibration curve is acceptable if all RSD values are less than or equal to 20.0 percent or if the correlation <br /> coefficient(R) is 0.995 or greater for linear regression curves. <br /> Retention time windows are also calculated from the initial calibration analyses. These windows are then <br /> used to identify all compounds of interest in subsequent analyses. <br /> EW&EMPIOVMENICPPoPiUNT'EMRMEP <br />