ASTM D7757 Standard Test Method for Silicon in Gasoline and Related Products by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry
1. Scope
1.1 This test method covers the determination of total silicon by monochromatic, wavelength-dispersive X-ray fluorescence (MWDXRF) spectrometry in naphthas, gasoline, gasoline-ethanol blends, reformulated gasoline (RFG), ethanol and ethanol-fuel blends, and toluene at concentrations of 3 mg/kg to 100 mg/kg. The precision of this test method was determined by an interlaboratory study using representative samples of the liquids described in 1.1 and 1.2. The pooled limit of quantitation (PLOQ) was estimated to be 3 mg/kg.
NOTE 1 - Volatile samples such as high-vapor-pressure gasolines or light hydrocarbons might not meet the stated precision because of the evaporation of light components during the analysis.
NOTE 2 - Aromatic compounds such as toluene are under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals. However, toluene can be a contributor to silicon contamination in gasoline (see 4.4), thus its inclusion in this test method.
1.2 Gasoline samples containing ethanol and other oxygenates may be analyzed with this test method provided the matrix of the calibration standards is either matched to the sample matrices or the matrix correction described in Annex A1 is applied to the results. The conditions for matrix matching and matrix correction are provided Section 5, Interferences.
1.3 Samples with silicon concentrations above 100 mg/kg can be analyzed after dilution with appropriate solvent. The precision and bias of silicon determinations on diluted samples have not been determined and may not be the same as shown for neat samples (Section 16).
1.4 A fundamental assumption in this test method is that the standard and sample matrices are well matched, or that the matrix differences are accounted for (see 13.5). Matrix mismatch can be caused by C/H ratio differences between samples and standards or by the presence of other interfering heteroatoms; observe the cautions and recommendations in Section 5.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4806 Specification for Denatured Fuel Ethanol for Blending with Gasolines for Use as Automotive Spark-Ignition Engine Fuel
D5798 Specification for Ethanol Fuel Blends for Flexible-Fuel Automotive Spark-Ignition Engines
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
D7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants
