Norma Astm D 1552 - 08

Designation: D 1552 – 08

An American National Standard

Standard Test Method for

Sulfur in Petroleum Products (High-Temperature Method)1
This standard is issued under the fixed designation D 1552; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the Department of Defense.

1. Scope* 1.1 This test method covers three procedures for the determination of total sulfur in petroleum products including lubricating oils containing additives, and in additive concentrates. This testmethod is applicable to samples boiling above 177°C (350°F) and containing not less than 0.06 mass % sulfur. Two of the three procedures use iodate detection; one employing an induction furnace for pyrolysis, the other a resistance furnace. The third procedure uses IR detection following pyrolysis in a resistance furnace. 1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed. 1.3 Thevalues stated in SI units are to be regarded as the standard. The values given in parentheses are for information only. 1.4 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 touse. 2. Referenced Documents 2.1 ASTM Standards:2 D 1193 Specification for Reagent Water D 1266 Test Method for Sulfur in Petroleum Products (Lamp Method) D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products D 6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance

D 6792 Practice forQuality System in Petroleum Products and Lubricants Testing Laboratories 3. Summary of Test Method 3.1 Iodate Detection System—The sample is burned in a stream of oxygen at a sufficiently high temperature to convert about 97 % of the sulfur to sulfur dioxide. A standardization factor is employed to obtain accurate results. The combustion products are passed into an absorber containing an acid solutionof potassium iodide and starch indicator. A faint blue color is developed in the absorber solution by the addition of standard potassium iodate solution. As combustion proceeds, bleaching the blue color, more iodate is added. The amount of standard iodate consumed during the combustion is a measure of the sulfur content of the sample. 3.2 IR Detection System—The sample is weighed into a specialceramic boat which is then placed into a combustion furnace at 1371°C (2500°F) in an oxygen atmosphere. Most sulfur present is combusted to SO2 which is then measured with an infrared detector after moisture and dust are removed by traps. A microprocessor calculates the mass percent sulfur from the sample weight, the integrated detector signal and a predetermined calibration factor. Both the sampleidentification number and mass percent sulfur are then printed out. The calibration factor is determined using standards approximating the material to be analyzed. 4. Significance and Use 4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This knowledge can be used to predict performance, handling, or processing properties. In some casesthe presence of sulfur compounds is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of sulfur compounds is detrimental to the processing or use of the product. 5. Interferences 5.1 For the iodate systems, chlorine in concentrations less than 1 mass % does not interfere. The IR system can tolerate somewhat higher...