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6.2.4 Each of the replicate spikes is extracted or digested in the same manner as samples. Routine cleanup <br /> steps shall be included. If dilutions are routinely performed for entire batches of samples (e.g., soil batches <br /> run on older ICP/MS instruments), then the same routine dilution must be applied to the MDL spikes prior to <br /> analysis. <br /> Note: It is not acceptable to spike at a high concentration prior to extraction or digestion and then <br /> dilute down to the MDL spike concentration after preparation, unless that is part of the sample <br /> preparation procedure (e.g., Methanol extractions for Method 8260) <br /> 6.2.5 If there are multiple instruments that will be assigned the same MDL, then the spikes shall be <br /> distributed across all of the instruments. A minimum of 2 spiked samples and 2 method blanks shall be <br /> analyzed on different calendar days on each instrument. Each analytical batch may contain one spiked sample <br /> and one MB run together. <br /> 6.2.6 The same prepared extract may be analyzed on multiple instruments if the minimum requirement of 7 <br /> preparations in at least 3 separate batches analyzed on 3 separate calendar dates is maintained. <br /> 6.2.7 Statistical outlier tests should not be used to remove data for the initial MDL determination because <br /> the total number of observations is small and the purpose of the MDL procedure is to capture routine method <br /> variability. However, documented instances of gross failures (e.g., instrument malfunctions, mislabeled <br /> samples, cracked vials) may be excluded from the calculations, provided that at least 7 spikes and 7 method <br /> blanks are available and the reason for excluding data is properly documented. <br /> 6.2.8 Evaluate the spiking level: If any result for any individual analyte from the spiked samples does not <br /> meet the method qualitative identification criteria or does not provide a numerical result greater than zero, <br /> then re-prepare the spiked samples at a higher concentration. Note that qualitative identification alone does <br /> not ensure that quantitative results for the analyte can be obtained. <br /> 6.2.9 Make all computations as specified in the analytical method and express the final results in the method- <br /> specified reporting units. <br /> 6.2.10 Using the following equation, calculate the standard deviation of the replicate spike measurements <br /> and the standard deviation of the method blank measurements: <br /> �quatjon 1: <br /> S — rr�_r -r)` , where <br /> x=X—X <br /> X=individual measurement <br /> rr <br /> X= Mean Measured Concentration <br /> rT <br /> n=number of sample aliquots <br /> 6.2.11 Compute the MDL based on spikes (MDLs) as follows: <br /> Equation 2; <br /> MDLs =t x Ss,where <br /> t= Student's t-value appropriate for a slingle-tailed 99"' percentile t statistic and a <br /> standard deviation estimate with n-1 degrees of freedom(see Attachment I-) <br /> Ss = sample standard deviation of the replicate spiked sample analyses determined <br /> using Equation 1 <br />