ASTM D4294-21 PDF
Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
- Статус документа:
- Действующий
- Формат:
- Электронный (PDF)
- Количество страниц:
- 9
- Дата публикации:
- 1 декабря 2021 г.
- Издание:
- D4294
- ICS:
- 75.080
SIGNIFICANCE AND USE 5.1 This test method provides rapid and precise measurement of total sulfur in petroleum and petroleum products with a minimum of sample preparation. A typical analysis time is 1 min to 5 min per sample. 5.2 The quality of many petroleum products is related to the amount of sulfur present. Knowledge of sulfur concentration is necessary for processing purposes. There are also regulations promulgated in federal, state, and local agencies that restrict the amount of sulfur present in some fuels. 5.3 This test method provides a means of determining whether the sulfur content of petroleum or a petroleum product meets specification or regulatory limits. 5.4 When this test method is applied to petroleum materials with matrices significantly different from the calibration materials specified in 10.1, the cautions and recommendations in Section 6 should be observed when interpreting results. SCOPE 1.1 This test method covers the determination of total sulfur in petroleum and petroleum products that are single-phase and either liquid at ambient conditions, liquefiable with moderate heat, or soluble in hydrocarbon solvents. These materials can include diesel fuel, jet fuel, kerosine, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, gasoline-ethanol blends, biodiesel (see Note 2), and similar petroleum products. Note 1: Oxygenated fuels with ethanol or methanol contents exceeding the limits given in Table 1 can be dealt with using this test method, but the precision and bias statements do not apply (see Appendix X3). Note 2: For samples with high oxygen contents (>3 % by weight) sample dilution as described in 1.3 or matrix matching must be performed to assure accurate results. 1.2 Interlaboratory studies on precision revealed the scope to be 17 mg/kg to 4.6 % by mass. An estimate of this test method’s pooled limit of quantitation (PLOQ) is 16.0 mg/kg as calculated by the procedures in Practice D6259. However, because instrumentation covered by this test method can vary in sensitivity, the applicability of the test method at sulfur concentrations below approximately 20 mg/kg must be determined on an individual basis. An estimate of the limit of detection is three times the reproducibility standard deviation, and an estimate of the limit of quantitation2 is ten times the reproducibility standard deviation. 1.3 Samples containing more than 4.6 % by mass sulfur can be diluted to bring the sulfur concentration of the diluted material within the scope of this test method. Samples that are diluted can have higher errors than indicated in Section 17 than non-diluted samples. 1.4 Volatile samples (such as high vapor pressure gasolines or light hydrocarbons) may not meet the stated precision because of selective loss of light materials during the analysis. 1.5 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 6.2). Matrix mismatch can be caused by C/H ratio differences between samples and standards (see Section 6) or by the presence of other heteroatoms. 1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.7 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.8 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.
Abstract
Overview
ASTM D4294-21, titled Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry, is a standard developed by ASTM International. This method specifies procedures for determining total sulfur content in petroleum and petroleum products using energy dispersive X-ray fluorescence (EDXRF) spectrometry. The standard encompasses a wide array of liquid petroleum products, including diesel fuel, gasoline, jet fuel, kerosine, crude oil, lubricating oils, and biodiesel blends.
This technique is widely adopted due to its rapid analysis time-typically 1 to 5 minutes per sample-and minimal sample preparation. The EDXRF method enables reliable measurement of sulfur concentrations, catering to industrial needs and ensuring compliance with regulatory and specification limits.
Key Topics
-
Scope of Application
- Suitable for single-phase petroleum and petroleum products that are liquid at ambient conditions, can be liquefied by moderate heat, or are soluble in hydrocarbon solvents.
- Applicable matrices include distillate oils, naphtha, residual oils, unleaded gasoline, gasoline-ethanol blends, and hydraulic oils, among others.
- For fuels with significant oxygen content (>3% by weight), sample dilution or matrix matching is required for accurate sulfur determination.
-
Analytical Range and Limitations
- The method’s typical measurement range is from 17 mg/kg to 4.6% by mass of sulfur.
- Pooled limit of quantitation (PLOQ) is approximately 16 mg/kg.
- For sulfur levels above 4.6% by mass, samples can be diluted to fall within the test method's scope.
- Measurement precision may be reduced for volatile samples, such as light hydrocarbons, due to possible material loss during testing.
-
Sample and Calibration Considerations
- Matrix matching is vital; calibration standards should closely resemble the sample matrix to avoid measurement bias.
- Interferences from elements like phosphorus, zinc, barium, calcium, chlorine, ethanol, methanol, and others must be considered and compensated for during analysis.
- Regular use of quality control samples and drift correction standards is recommended for maintaining analytical performance.
-
Reporting and Quality Control
- Results are reported in mg/kg or mass percent, following the requirements for significant figures.
- Laboratories are encouraged to use statistical quality assurance practices and regular calibration checks to ensure reliability.
Applications
- Regulatory Compliance: The quality and environmental acceptability of fuels are often judged by sulfur content. This test method supports compliance with federal, state, and local sulfur regulations for fuels and petroleum products.
- Quality Control in Refining and Blending: Refineries and fuel distributors utilize ASTM D4294-21 to monitor and adjust sulfur concentrations in fuels, maintaining consistent product quality.
- Routine Analysis: The minimal sample preparation and rapid analysis make EDXRF ideal for routine laboratory and process control environments.
- Product Specification Verification: ASTM D4294-21 provides a practical tool for determining if petroleum products meet internal specifications or customer requirements for sulfur content.
Related Standards
- ASTM D4057 - Practice for Manual Sampling of Petroleum and Petroleum Products
- ASTM D4177 - Practice for Automatic Sampling of Petroleum and Petroleum Products
- ASTM D6259 - Pooled Limit of Quantitation for a Test Method
- ASTM D6299 - Statistical Quality Assurance and Control Charting
- ASTM D7343 - Optimization and Validation of X-ray Fluorescence Methods for Petroleum Products
- ASTM E29 - Use of Significant Digits in Test Data
These related standards enhance guidance on sampling, calibration, data analysis, and statistical quality assurance, ensuring best practices when applying ASTM D4294-21 for sulfur analysis.
Keywords: ASTM D4294-21, sulfur determination, petroleum products, energy dispersive X-ray fluorescence, EDXRF, sulfur content, fuel analysis, regulatory compliance, sulfur in fuels, petroleum testing standard
Технические детали
- Технический комитет
- D02 - Petroleum Products, Liquid Fuels, and Lubricants
- SKU
- ASTM D4294-21
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