More D A typical analysis time is 1 min to 5 min per sample. 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. Scope 1. 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.
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A number in parentheses indicates the year of last reapproval. A superscript epsilon e indicates an editorial change since the last revision or reapproval. Scope 4. Significance and Use 1.
A typical analysis time is 2 to 4 min per gasoline all unleaded , and other distillates. In addition, sulfur sample. Knowledge of sulfur concentration is 0. There are also regulations 1.
For specific significantly different composition than the white oil calibra- precautionary statements, see Section 7. Referenced Documents interpreting the results. The equipment D Practice for Manual Sampling of Petroleum and specified is in most cases less costly than that required for Petroleum Products2 alternative methods. Interferences Determine Conformance with Specifications 3 5.
Summary of Test Method resolve from sulfur X-ray emission. As a result, the lines 3. Spectral source. Two groups of calibration sured concentration of sulfur, or more than a few hundred samples are required to span the concentration range 0.
These variations directly influence I This test method is under the jurisdiction of Committee D-2 on Petroleum X-ray absorption and change the measured intensity of each Products and Lubricants and is the direct responsibility of Subcommittee D For example, performance enhancing additives, such Current edition approved Apr.
Published October Originally as oxygenates in gasoline, can affect the apparent sulfur published as D Last previous edition D ". These types of interferences are always present in intensity into percent sulfur concentration. X-ray fluorescence analysis and are completely unrelated to 6. Reagents and Materials contemporary instruments with the use Of built-in software.
Unless otherwise indicated, it is intended that to time and that the software corrections offered by the all reagents conform to the specifications of the Committee on manufacturer not be accepted at face value. Corrections should Analytical Reagents of the American Chemical Society where be verified for new formulations. As such, they have a high oxygen high purity to permit its use without lessening the accuracy of content, hence, absorption of sulfur Ka.
Such fuels the determination. Use the certified sulfur the sample. There may be a loss of sensitivity and precision. Thus, a gasoline may be simulated by 7. Standards 7. Films found to be suitable are polyester, NOTE I-In the case of petroleum materials that contain suspended polypropylene, polycarbonate, and polyimide films.
The ester and polycarbonate films. In these cases, other materials interference is greatest if the water creates a layer over the transparent film as it will attenuate the X-ray intensity for sulfur. One such method to besides these films may be used for X-ray windows, provided accomplish the removal of water is to centrifuge the sample first under that they do not contain any elemental impurities.
An optional ambient sealed conditions, taking care that the sample integrity is not window material is polyimide foil. Although polyimide foil compromised. Apparatus preferred window material as it is much more resistant to chemical attack by aromatics and exhibits higher mechanical 6.
However, Samples should be analyzed immediately after pouring into a attention to the source is only to be carried out by a fully trained and competent person using the correct shielding techniques. Disposable sample cells are not to be reused.
A new piece 6. Avoid touching the inside of the sample film window. Oil from resolution value not to exceed eV. A gas filled proportional fingerprints can affect the reading when analyzing for low counter has been found to be suitable to use. Chemi- 6. Pharmacopeial Convention, Inc. Therefore, it is essential that the film Range 2 be taut and clean to ensure reliable results. Std 2 0. Therefore, the Std 6 0.
Std 7 0. Calibration and Standardization 9. Hence, the matrix diluent should be as close to the which are certified by a national standards organization, may form of the matrix being analyzed as possible.
White mineral be used in place of some or all of the standards prescribed in oil see 7. Such 9. The calculated to four decimal places. Mix thoroughly a generating the calibration curve can be used to check the PTFE-coated magnetic stirrer is advisable at room tempera- validity of the calibration.
Calibration check standards may be ture. The concentration of the calibration check centration ranges identified in Table 2 for the two ranges by standards shall be near the expected concentration of the diluting each primary standard with the applicable matrix samples being analyzed.
As soon as any sedlffient or Method D or any other equivalent low level sulfur change of concentration is observed, discard the standard. Preparation of Apparatus mended mass to the nearest 0. It is important that the actual mass is known; thus, the actual concentration of the Whenever possible, the instrument should for calibration purposes. The concentration of sulfur can be remain energized to maintain optimum stability.
Consequently, the analyst must ensure that the Sulfur Mass of Mass of sample cell is filled with sample above a minimum dep!
Generally speaking, filling the sample cup to at 5. Provide a vent hole in the top to prevent bowing. It is recognized that QC procedures , - are the. L1 For tlw.
Typically, the calibration procedure in- they were uriknownproduction samples. Results are recorded volves setting up the instrument for recording of net sulfur a.
Obtain two readings on the standard using the status of the total testing process. Aliy out of control data shall recommended counting time for the instrument according to trigger investigation for root cause s. The outcome of the Table 3. Depending prepared cells and fresh portions of the standard. It is recom- analyzed four times. Immediately, lipon completion of the mended that at least one type of quality control sample be calibration, determine the sulfur concentration of one or mote analyzed that is representative of samples routinely analyzed of the calibration: check..
Obtain the average Report Request RR:D0. Quality Control. SRM SRM 3,0. Keywords Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn: Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.
ASTM D4294 - 10
Scope LA This test method covers the determination of total sulfur in petroleum and petroleum products that are single-phase and. These materials can include diesel fuel, jet fuel, Kerosine, other distillate oi, naphtha residual oi, lubricating base oll, hydraulic oil, crude cil, unleaded gasoline, gusohol, biodiesel see Note 2 , and similar petroleum products. Nove —Onypenaed ful with ethanol or methanol contents excct- ing tel given fa Tble Len be deat dh ung his west method, bat the precision and bias atements donot apply see Appedix X3. A minimum of three groups of calibration samples are required to span the concentration range: 0. See Practice D
EDXRF / XRF for Petroleum & Petrochem