1065.1107 Sample media and sample system preparation; sample system assembly.§ 1065.1107 Sample media and sample system preparation; sample system assembly.
This section describes the appropriate types of sample media and the cleaning procedure required to prepare the media and wetted sample surfaces for sampling.
(a) Sample media. The sampling system uses two types of sample media in series: The first to simultaneously capture the PM and associated particle phase SVOCs, and a second to capture SVOCs that remain in the gas phase, as follows:
(1) For capturing PM, we recommend using pure quartz filters with no binder if you are not analyzing separately for SVOCs in gas and particle phases. If you are analyzing separately, you must use polytetrafluoroethylene (PTFE) filters with PTFE support. Select the filter diameter to minimize filter change intervals, accounting for the expected PM emission rate, sample flow rate. Note that when repeating test cycles to increase sample mass, you may replace the filter without replacing the sorbent or otherwise disassembling the batch sampler. In those cases, include all filters in the extraction.
(2) For capturing gaseous SVOCs, utilize XAD-2 resin with or without PUF plugs. Note that two PUF plugs are typically used to contain the XAD-2 resin in the sorbent module.
(b) Sample media and sampler preparation. Prepare pre-cleaned PM filters and pre-cleaned PUF plugs/XAD-2 as needed. Store sample media in containers protected from light and ambient air if you do not use them immediately after cleaning. Use the following preparation procedure, or an analogous procedure with different solvents and extraction times:
(1) Pre-clean the filters via Soxhlet extraction with methylene chloride for 24 hours and dry over dry nitrogen in a low-temperature vacuum oven.
(2) Pre-clean PUF and XAD-2 with a series of Soxhlet extractions: 8 hours with water, 22 hours with methanol, 22 hours with methylene chloride, and 22 hours with toluene, followed by drying with nitrogen.
(3) Clean sampler components, including the probe, filter holder, condenser, sorbent module, and condensate collection vessel by rinsing three times with methylene chloride and then three times with toluene. Prepare pre-cleaned aluminum foil for capping the probe inlet of the sampler after the sampling system has been assembled.
(c) Sorbent spiking. Use good engineering judgment to verify the extent to which your extraction methods recover SVOCs absorbed on the sample media. We recommend spiking the XAD-2 resin with a surrogate standard before testing with a carbon-13 or hydrogen-2 isotopically labeled standard for each of the class of analytes targeted for analysis. Perform this spiking as follows:
(1) Insert the lower PUF plug into the bottom of the sorbent module.
(2) Add half of one portion of XAD-2 resin to the module and spike the XAD-2 in the module with the standard.
(3) Wait 1 hour for the solvent from the standard(s) to evaporate, add the remaining 20 g of the XAD-2 resin to the module, and then insert a PUF plug in the top of the sorbent module.
(4) Cover the inlet and outlet of the sorbent module with pre-cleaned aluminum foil.
(d) Sampling system assembly. After preparing the sample media and the sampler, assemble the condensate trap, cooling coil, filter holder with filter, sample probe, and sorbent module, then lower the assembly into the reservoir. Cover the probe inlet with pre-cleaned aluminum foil.[79 FR 23820, Apr. 28, 2014, as amended at 81 FR 74195, Oct. 25, 2016]