Analytical laboratory reports attachment for PCDDs and PCDFs, 2008

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BISosy’ ■I, Pace Analytical Services, Ine. 1700 Elm Street. Suite 200 weAnalyticar Minneapolis, MN 55414 Phone: 612.607.1700 www.pacelabs.coni REPORT OF: CHEMICAL ANALYSES Fax: 612.607.6444

PROJECT: PCDD/PCDF ANALYSES DATE: January 9, 2002

PAGE: 6 REPORT NO: 01-1052682

I Quality Control for PCDD/PCDF Analyses

The performance of the sample processing steps and the instrumentation are monitored on a routine basis: The procedures and criteria are summarized below.

One mimod blank and one laboratory spike sample are typically prepared with each ten samples of any ^iven matrix. Recoveries of the native PCDD/PCDF analytes in the laboratory spike samples ^ generally range from 70 to 130%. Recoveries of selected analytes outside this range do not invalidate the data but provide information, which is used by the laboratory to monitor recovery trends and to assure optimization of the method.

Internal standards are spiked into each sample prior to extraction in order to monitor the level of i recovery, which is achieved for each individual sample. Acceptable recoveries range from 40 to I 135 percent for the internal standards unless a deviation is due to variation in instrument response "" as a result of analytical interferences.

The resolution of the mass spectrometer is verified prior to each analysis to be 10,000 or greater. Hardcopies of the reference peaks are printed at the beginning and end of each analysis day. The resolving power of the DB-5MS chromatographic column is checked daily by analyzing a standard solution containing 2,3,7,8-TCDD and the adjacent TCDD isomers. The DB-225 column resolution is checked daily by analyzing a standard solution containing 2,3,7,8-TCDF and the adjacent TCDF <3 isomers. Acceptable performance is achieved when 2,3,7,8-TCDD or 2,3,7,8-TCDF is resolved y from the adjacent isomers by a valley of 25% or less. The group times for the selected-ion ­ monitoring data acquisitions are also checked daily by analyzing the column performance mix which has been modified to contain the first and last eluting isomers of each congener class. In Ji this way one is assured of collecting data representative of the total PCDD/PCDF content and that the 2,3,7,8-substituted isomers are suitably resolved.

y Initial calibrations are generated by analyzing standard solutions (see Table 4) containing target native and labeled PCDD/PCDF compounds. Response factors are calculated and averaged for g each compound. These averages are used for quantification and for comparison to the daily S continuing calibration. The relative standard deviation for each native compound must be 20% or less (30% or less for the labeled compounds) as specified in Method 8290. A continuing j calibration standard is analyzed at the beginning and end of each 12-hour shift on days when initial calibrations are not performed. The initial calibration is considered to be valid when the response factors from the continuing calibration analysis fall to within the ranges specified in Method 8290.

■ ?? REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except In full, without the written consent of Pace Analytical Services, Inc.

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