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Appendix D
Discussion of Laboratory Analyses of PCDDs and PCDFs
-------
-------
Appendix D
Laboratory Contamination Problems for Dioxin Analyses
Conducted by Midwest Research Institute
Midwest Research Institute (MRI) extracted and analyzed 32 water samples,
4 spiked tap water samples, and 4 method blanks for tetra-, octa-, CODs and COFs
and for 2378-TCDD and 2378-TCDF isomer specific. The samples, spikes, and blanks
were extracted with hexane and taken through a two-part column. The first part
contained sulfuric acid, treated silica gel, and untreated silica gel. The
second part contained acidic alumina. This cleanup procedure is described in
i the USEPA dioxin analysis protocol for soil and sediment and is an optional
iprocedure in the removal of readily oxidizable organic compounds. Samples with
''high levels of organic material required further cleanup with a Carbopak C/
Celite column. The method blanks were not carried through the Carbopak/Celite
cleanup step by MRI. Referring to Table D-l, method blank (MB) 1-3 and all other
samples had positive results for two TCDD isomers. These isomers had peak
maximums at scans 1046 and 1054 and were consistent throughout the analysis. The
2378-TCDD peak maximum occurred at scan 1100. MB4 reported total TCDD and ND
(not detectable) with a detection limit of 10 pg/liter (ppq). OCDF was found
in MB4 and 31 pg/1, less than the contract required detection limit of 90 pg/1.
HXCDD, HpCDD, and OCDF were reported in MB2. MRI stated that this was apparently
carry-over from a previous injection of spiked tap water which contained these
compounds. A request was made for reanalysis of MB2. Verbal results from MRI
indicate the presence of the two TCDD peaks and OCDD, which were found in all
samples and blanks.
MRI initiated an investigation into the source of the TCDD isomer contami-
nation. They have found that these two isomers correspond to 1368-TCDD and
1379-TCDD. MRI was unable to trace these isomers back to the solvents or
spiking solutions used in the analyses. However, MRI has found evidence
that the acidic alumina column used in the extract cleanup procedure may be
responsible. According to MRI, it appears that the contribution of these
isomers resulted from the prolonged activation of acidic alumina in a specific
oven in the laboratory. Accordingly, Region V does not consider the data for
PCDDs and PCDFs, other than 2378-TCDD, to be valid data.
-------