1065.1103 General provisions for SVOC measurement.§ 1065.1103 General provisions for SVOC measurement.
The provisions of §§ 1065.1103 through 1065.1111 specify procedures for measuring semi-volatile organic compounds (SVOC) along with PM. These sections specify how to collect a sample of the SVOCs during exhaust emission testing, as well as how to use wet chemistry techniques to extract SVOCs from the sample media for analysis. Note that the precise method you use will depend on the category of SVOCs being measured. For example, the method used to measure polynuclear aromatic hydrocarbons (PAHs) will differ slightly from the method used to measure dioxins. Follow standard analytic chemistry methods for any aspects of the analysis that are not specified.
(a) Laboratory cleanliness is especially important throughout SVOC testing. Thoroughly clean all sampling system components and glassware before testing to avoid sample contamination. For the purposes of this subpart, the sampling system is defined as sample pathway from the sample probe inlet to the downstream most point where the sample is captured (in this case the condensate trap).
(b) We recommend that media blanks be analyzed for each batch of sample media (sorbent, filters, etc.) prepared for testing. Blank sorbent modules (i.e., field blanks) should be stored in a sealed environment and should periodically accompany the test sampling system throughout the course of a test, including sampling system and sorbent module disassembly, sample packaging, and storage. Use good engineering judgment to determine the frequency with which you should generate field blanks. The field blank sample should be close to the sampler during testing.
(c) We recommend the use of isotope dilution techniques, including the use of isotopically labeled surrogate, internal, alternate, and injection standards.
(d) If your target analytes degrade when exposed to ultraviolet radiation, such as nitropolynuclear aromatic hydrocarbons (nPAHs), perform these procedures in the dark or with ultraviolet filters installed over the lights.
(e) The following definitions and abbreviations apply for SVOC measurements:
(1) Soxhlet extraction means the extraction method invented by Franz von Soxhlet, in which the sample is placed in a thimble and rinsed repeatedly with a recycle of the extraction solvent.
(2) XAD-2 means a hydrophobic crosslinked polystyrene copolymer resin adsorbent known commercially as Amberlite® XAD®-2, or an equivalent adsorbent like XAD-4.
(3) Semi-volatile organic compound (SVOC) means an organic compound that is sufficiently volatile to exist in vapor form in engine exhaust, but that readily condenses to liquid or solid form under atmospheric conditions. Most SVOCs have at least 14 carbon atoms per molecule or they have a boiling point between (240 and 400) °C. SVOCs include dioxin, quinone, and nitro-PAH compounds. They may be a natural byproduct of combustion or they may be created post-combustion. Note that SVOCs may be included in measured values of hydrocarbons and/or PM using the procedures specified in this part.
(4) Kuderna-Danish concentrator means laboratory glassware known by this name that consists of an air-cooled condenser on top of an extraction bulb.
(5) Dean-Stark trap means laboratory glassware known by this name that uses a reflux condenser to collect water from samples extracted under reflux.
(6) PUF means polyurethane foam.
(7) Isotopically labeled means relating to a compound in which either all the hydrogen atoms are replaced with the atomic isotope hydrogen-2 (deuterium) or one of the carbon atoms at a defined position in the molecule is replaced with the atomic isotope carbon-13.