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In-use, light-duty vehicles were recruited in Cary, North Carolina for emissions testing on a transportable dynamometer in 1999. Two hundred forty-eight vehicles were tested in as received condition using the IM240 driving cycle. The study was conducted in two phases, a summer and winter phase, with half of the vehicles recruited during each phase. Regulated emissions, PM10, carbonaceous PM, aldehydes and ketones were measured for every test. PM2.5, individual volatile hydrocarbons, polycyclic aromatic hydrocarbons, sterane and hopane emissions were measured from a subset of the vehicles. Average light-duty gasoline PM10 emission rates increased from 6.5 mg/mi for 1993-97 vehicles to 53.8 mg/mi for the pre-1985 vehicles. The recruited fleet average, hot-stabilized IM240 PM10 emission rate for gasoline vehicles was 19.0 mg/mi.

A second carbonyl round robin was conducted to enable participating laboratories doing routine analysis of carbonyls in vehicle exhaust emissions to assess their analytical capabilities. Three sets of solutions in acetonitrile containing varying number and amounts of standard DNPH-carbonyls were prepared. The parent carbonyls are known components of vehicle exhaust emissions. The samples were designed to challenge the capabilities of the participants to separate, identify and quantify all the components. The fourteen participating laboratories included automotive, contract, petroleum and regulatory organizations. All participants were able to separate and identify the C3 carbonyls; a few were not able to separate MEK from butyraldehyde and methacrolein from butyraldehyde; and many were not able to separate adequately the isomers of tolualdehyde. Inadequate separation and lack of appropriate standards resulted in a few misidentifications.

Analytical methods for determining individual aldehyde, ketone, and alcohol emissions from gasoline-, methanol-, and variable-fueled vehicles are described. These methods were used in the Auto/Oil Air Quality Improvement Research Program to provide emission data for comparison of individual reformulated fuels, individual vehicles, and for air modeling studies. The emission samples are collected in impingers which contain either 2,4-dinitrophenylhydrazine solution for the aldehydes and ketones or deionized water for the alcohols. Subsequent analyses by liquid chromatography for the aldehydes and ketones and gas chromatography for the alcohols utilize autoinjectors and computerized data systems which permit high sample throughput with minimal operator intervention. The quality control procedures developed and interlaboratory comparisons conducted as part of this program are also described.

A routine on-line reverse phase high performance liquid chromatography (HPLC)/HPLC fluorescence method has been developed which greatly simplifies the analysis of selected nitroaromatic compounds in complex matrices. Sensitivity of the method is generally in the low picogram to low nanogram levels. The method is based on on-column catalytic reduction of the non-fluorescent nitroaromatic compounds to the corresponding highly fluorescent amine derivatives. Compound selectivity is achieved by chromatographic separation, use of selective wavelengths for fluorescence detection and column switching techniques. The analytical system conveniently eliminates tedious sample clean-up. In most cases only about 25 micrograms of the crude sample is needed per analysis. For 1-nitropyrene, a precision of ± 3% at the one nanogram level is routinely obtained.