Analytical laboratory reports attachment for PCDDs and PCDFs, 2008

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a Paee Analytical Services, Im. 1700 Elm Street, Suite 200 weAnalyticar iimw.pacBlabs.com REPORT OF: CHEMICAL ANALYSES Minneapolis, MN 55414 Phone: 612.607.1700 Fax: 612.607.6444

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

PAGE: 2 REPORT NO: 01-1052682

I PCDD/PCDF Analyte Enrichment 3 The extraction .procedure often removes a variety of compounds, in addition to the PCDDs and PCDFs, from the sample matrix. Some of these compounds can directly interfere with the analyses while others can overload the capillary column causing degradation in chromatographic resolution si or sensitivity. The analyte enrichment steps described below are used to remove interferences from the extracts.

Each extract was diluted to 100 mL with hexane, transferred to a separatory funnel, and washed „ with IN sodium hydroxide, concentrated sulfuric acid, and aqueous sodium chloride (5% w/v) as ■J needed. The hexane extract was quantitatively transferred to a liquid chromatography column containing alternating layers of silica gel, 40% concentrated sulfuric acid on silica gel, and 33% 1 _ N sodium hydroxide on silica gel. The column was eluted with 90 mL of hexane and the entire Hh eluate was collected and concentrated, under ambient conditions, to a volume of 1 mL.

, Each extract was then fractionated on a liquid chromatography column containing 4 g of activated alumina. The column was eluted with 20 mL of hexane followed by 15 mL of 60% methylene chloride/hexane. The 60% methylene chloride/hexane fraction was concentrated to 1 mL under a r stream of dry nitrogen and applied to the top of a chromatography column containing 1 g of 5% AX-21 activated carbon in silica gel. The column was eluted with two 2-mL portions of hexane, 2 mL of cyclohexane/methylene chloride (50:50 v/v) and cyclohexane/methanol/toluene (75:20:5 v/v) in the forward direction, and then with toluene in the reverse direction. The toluene fraction is was collected, concentrated, spiked with recovery standards (1,2,3,4-TCDD-’5Ci2 and 1,2,3,7,8,9- HxCDD-’^Cij) and taken to a final volume of 20 uL.

PCDD/PCDF Analyses a B Each sample extract was analyzed for the presence of PCDDs and PCDFs using combined capillary column gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The Q instrumentation consisted of a Hewlett Packard Model 6890 gas chromatograph interfaced to a 0 Micromass Ultima high-resolution mass spectrometer. The capillary column was interfaced directly into the ion source of the mass spectrometer, thus providing the highest possible ■ sensitivity while minimizing degradation of the chromatographic resolution.

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

npfer CONFIDENTIAL, CITY_21MC100_0 03432695 SUBJECT TO PROTECTIVE ORDER NO. 2, SEPT. 2008

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