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instrument blank should also be analyzed whenever contamination is suspected by the analyst. <br /> The frequency of analysis will vary with the data quality objectives of the project. A <br /> manufacturer-recommended count time per source should be used for the blank analysis. No <br /> element concentrations above the method detection limits should be found in the instrument <br /> blank. If concentrations exceed these limits, then the probe window and the check sample <br /> should be checked for contamination. If contamination is not a problem, then the instrument <br /> must be "zeroed" by following the manufacturer's instructions. <br /> 9.3.2 A method blank is used to monitor for laboratory-induced contaminants or <br /> interferences. The method blank can be "clean" silica sand or lithium carbonate that <br /> undergoes the same preparation procedure as the samples. A method blank must be analyzed <br /> at least daily. The frequency of analysis will depend on the data quality objectives of the <br /> project. To be acceptable, a method blank must not contain any analyte at a concentration <br /> above its method detection limit. If an analyte's concentration exceeds its method detection <br /> limit, the cause of the problem must be identified, and all samples analyzed with the method <br /> blank must be reanalyzed. <br /> 9.4 Calibration Verification Checks: A calibration verification check sample is used to check <br /> the accuracy of the instrument and to assess the stability and consistency of the analysis for the <br /> analytes of interest. A check sample should be analyzed at the beginning of each working day, <br /> during active sample analyses, and at the end of each working day. The frequency of calibration <br /> checks during active analysis will depend on the data quality objectives of the project. The check <br /> sample should be a well characterized soil sample from the site that is representative of site samples <br /> in terms of particle size and degree of homogeneity and that contains contaminants at <br /> concentrations near the action levels. If a site-specific sample is not available, then an NIST or other <br /> SRM that contains the analytes of interest can be used to verify the accuracy of the instrument. The <br /> measured value for each target analyte should be within ±20 percent (%D) of the true value for the <br /> calibration verification check to be acceptable. If a measured value falls outside this range, then the <br /> check sample should be reanalyzed. If the value continues to fall outside the acceptance range, the <br /> instrument should be recalibrated, and the batch of samples analyzed before the unacceptable <br /> calibration verification check must be reanalyzed. <br /> 9.5 Precision Measurements: The precision of the method is monitored by analyzing a <br /> sample with low, moderate, or high concentrations of target analytes. The frequency of precision <br /> measurements will depend on the data quality objectives for the data. A minimum of one precision <br /> sample should be run per day. Each precision sample should be analyzed 7 times in replicate. It <br /> is recommended that precision measurements be obtained for samples with varying concentration <br /> ranges to assess the effect of concentration on method precision. Determining method precision <br /> for analytes at concentrations near the site action levels can be extremely important if the FPXRF <br /> results are to be used in an enforcement action; therefore, selection of at least one sample with <br /> target analyte concentrations at or near the site action levels or levels of concern is recommended. <br /> A precision sample is analyzed by the instrument for the same field analysis time as used for other <br /> project samples. The relative standard deviation (RSD) of the sample mean is used to assess <br /> method precision. For FPXRF data to be considered adequately precise, the RSD should not be <br /> greater than 20 percent with the exception of chromium. RSD values for chromium should not be <br /> greater than 30 percent. <br /> The equation for calculating RSD is as follows: <br /> RSD = (SD/Mean Concentration) x 100 <br /> CD-ROM 6200 - 11 Revision 0 <br /> January 1998 <br />