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7.3.6 Replicate analyses are performed regularly. <br />7.3.6.1 A duplicate analysis is performed on at least one sample <br />each day. <br />Method <br />102 Revision 1 <br />centrations and 4 replicate runs for each concentra- <br />tion. The concentrations must bracket the anticipate) <br />range of sample concentrations. <br />7.3.3.2 <br />The mean -square error due to lack of fit about the <br />regression line is compared to the total mean -square <br />error of the independent replicates about their <br />individual means. The calibration is accepted if the <br />F -ratio is less than the 95% rejection limit. <br />7.3.3.3 <br />Any region of concentration that deviates more than <br />b% from the least square line is considered nonlinear. <br />7.3.3.4 <br />Samples must be analyzed only in the linear range. <br />7.3.4 <br />Limits of detection must be established. <br />7.3.4.1 <br />The limit of detection (LOD) is based on three standard <br />deviations (SD) of runs near the LOD (within 10 SD <br />of the LOD, Winefordner and Long, 1983). <br />7.3.4.2 <br />The LOD should be determined at least on an annual <br />basis. <br />7.3.4.3 <br />If the benzene calibration factor changes by more than <br />10%, The instrument must be checked and the LOD <br />redetermined. <br />7.3.4.4 <br />The presence in a sample of a compound producing in <br />the chart display very large adjacent peaks will <br />often raise the LOD in that sample. <br />7.3.5 <br />GC column condition parameters should be checked and <br />documented. <br />7.3.5.1 <br />All GC accessible parameters should be logged when <br />a column is first installed. These parameters should <br />be checked daily and recorded on integrator reports. <br />7.3.5.2 <br />The efficiency and resolution of th-' column should <br />be checked every thirty days. If the tests show <br />more than a 10% ch&nge the column needs replacement. <br />7.3.5.3 <br />If the headpressure required to inaintain a specified <br />flow through the column increases by more than 100%, <br />the column needs replacement. <br />7.3.5.4 <br />If the drift of retention t-imei: of the peaks results <br />in peak misidentification, all instrument parameters <br />need to be checkEi. <br />7.3.6 Replicate analyses are performed regularly. <br />7.3.6.1 A duplicate analysis is performed on at least one sample <br />each day. <br />