ASTM D4530-15(R2020) pdf free download

ASTM D4530-15(R2020) pdf free download.Standard Test Method for Determination of Carbon Residue (Micro Method)
1. Scope
1.1 This test method covers the determination ofthe amount of carbon residue (see Note 1) formed after evaporation and pyrolysis of petroleum materials under certain conditions and is intended to provide some indication of the relative coke forming tendency of such materials. 1.2 The test results are equivalent to the Conradson Carbon Residue test (see Test Method D189). N OTE 1—This procedure is a modification of the original method and apparatus for carbon residue of petroleum materials, where it has been demonstrated that thermogravimetry is another applicable technique. 2 However, it is the responsibility of the operator to establish operating conditions to obtain equivalent results when using thermogravimetry. 1.3 This test method is applicable to petroleum products that partially decompose on distillation at atmospheric pressure and was tested for carbon residue values of 0.10 % to 30 % (m/m). Samples expected to be below 0.10 weight % (m ⁄m) residue should be distilled to remove 90 % (V/V) of the flask charge (see Section 9). The 10 % bottoms remaining is then tested for carbon residue by this test method. 1.4 Ash-forming constituents, as defined by Test Method D482, or non-volatile additives present in the sample will add to the carbon residue value and be included as part of the total carbon residue value reported. 1.5 Also in diesel fuel, the presence ofalkyl nitrates, such as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon residue value than observed in untreated fuel, which may lead to erroneous conclusions as to the coke-forming propensity of the fuel. The presence of alkyl nitrate in the fuel may be detected by Test Method D4046. 1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.6.1 Exception—6.4 and 6.5 include inch-pound units.1.7 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been dem- onstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location. 1.8 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 appro- priate safety, health, and environmental practices and to determine the applicability of regulatory limitations prior to use. For specific warning statements, see 8.2.3 and 8.4. 1.9 This international standard was developed in accor- dance with internationally recognized principles on standard- ization established in the Decision on Principles for the Development of International Standards, Guides and Recom- mendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
8. Procedure
8.1 Sample Preparation: 8.1.1 Determine the mass of each clean sample vial being used in the sample analysis, and record the mass to nearest 0.1 mg. 8.1.2 During weighing and filling, handle vials with forceps to help minimize weighing errors. Discard the sample vials after use. 8.1.3 It is assumed that a representative sample of the stock or process has been obtained for laboratory use following Practice D4057 or similar standard. Stir the sample to be tested, first warming if necessary to reduce its viscosity. Samples that are homogeneous liquids can be transferred directly to vials using a rod, syringe, or eyedropper. Solid materials may also be heated; or frozen with liquid nitrogen, and then shattered to provide manageable pieces. 8.1.4 Transfer an appropriate mass of the sample (see Table 1) into a tared-sample vial, reweigh to nearest 0.1 mg, and record. Place the loaded sample vials into vial holder (up to twelve), noting position of each sample with respect to index mark. N OTE 2—A control sample can be included in each batch of samples being tested. This control sample should be a typical sample that has been tested at least 20 times in the same equipment in order to define an average percent carbon residue and standard deviation. Results for each batch are deemed acceptable when results for the control sample fall within the average percent carbon residue 6 three standard deviations. Control results that are outside these limits indicate problems with the procedure or the equipment. 8.2 Processing ofSamples: 8.2.1 With the oven at less than 100 °C, place the vial holder into the oven chamber and secure lid. Purge with nitrogen for at least 10 min at 600 mL ⁄min. Then decrease the purge to 150 mL ⁄min and heat the oven slowly to 500 °C at 10 °C ⁄min to 15 °C ⁄min. 8.2.2 If the sample foams or spatters, causing loss of sample, discard and repeat the test. N OTE 3—Spattering may be due to water that can be removed by prior gentle heating in a vacuum, followed by a nitrogen sweep. Alternatively, a smaller sample size can be used.