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' SOP TO-14A/15 <br /> Rev 4 <br /> December 2007 <br /> ' Secondary standards for TO-14A/15 analysis will be prepared and given expiration <br /> dates not to exceed the manufacturer's date of expiration on the primary standard. <br /> The lab operator should monitor response factors to determine whether standards are <br /> ' degrading. In general, response factors will vary with tuning characteristics. <br /> However,comparison to response factors from fresh standard is suggested. <br /> ' 8.0 Method Calibration <br /> In order to analyze samples the instrument must first be calibrated. The following subsections describe the <br /> ' system start-up and initial calibration procedures. <br /> 8.1 Initial System Calibration <br /> ' Prior to performing analyses, the GC-MS must be tuned and calibrated to ensure system precision and <br /> accurate results. <br /> Tuning of the GC-MS is accomplished using the Agilent Target Tune function in the BFB tune mode. The <br /> instrument automatically performs the tuning in an attempt to adjust parameters such that the spectrum of the <br /> ' compound 1,4-Bromofluorobenzene will meet the following specifications: <br /> • Mass 50 15 percent to 40 percent of mass 95 <br /> ' 0 Mass 75 30 percent to 60 percent of mass 95 <br /> • Mass 95 base peak, 100 percent relative abundance <br /> Mass 96 5 percent to 9 percent of mass 95 <br /> ' 0 Mass 173 less than 2 percent of mass 174 <br /> • Mass 174 greater than 50 percent of mass 95 <br /> • Mass 175 5 percent to 9 percent of mass 174 <br /> ' 0 Mass 176 greater than 95 percent, but less than <br /> 101 percent of mass 174 <br /> • Mass 177 5 percent to 9 percent of mass 176 <br /> ' Following tuning, 50 ng of BFB or less should be evaluated in the next blank or standard to determine the <br /> validity of the tune. Since BFB is one of the surrogate compounds that are included in every analysis, it can <br /> ' be monitored following any analysis. (See section 11.0 for details.) If the above criteria are not met,the <br /> instrument must be retuned or the problem found prior to proceeding. <br /> ' Prior to performing analyses, the GC-MS must be calibrated to ensure system precision and accurate results. <br /> To calibrate the GC-MS, standards of the analytes, along with intemal standards and surrogates are <br /> introduced into the concentrator and measured by the method. A minimum of five concentration levels <br /> should be used during calibration for EPA Method TO-14A/15. (For TO-14A, three level are required, for <br /> TO-15, five levels are used.) Each standard level is analyzed under the identical parameters as samples will <br /> be analyzed. The end result is a calibration curve for each analyte. (Note: Certain regulatory protocols i.e. <br /> LARWQCB and specific client Data Quality Objectives(DQOs)may require fewer than five initial <br /> calibration standards) <br /> ' Page 7 of 24 <br />