ASTM D1552-2007 Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)《石油产品中硫含量的标准试验方法(高温法)》.pdf
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1、Designation: D 1552 07An American National StandardStandard Test Method forSulfur in Petroleum Products (High-Temperature Method)1This standard is issued under the fixed designation D 1552; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、 covers three procedures for the deter-mination of total sulfur in petroleum products includinglubricating oils containing additives, and in additive concen-trates. This test method is applicable to samples boiling above177C (350F) and containing not less than 0.06 mass % sulfur.Two of the three pro
4、cedures use iodate detection; one employ-ing an induction furnace for pyrolysis, the other a resistancefurnace. The third procedure uses IR detection followingpyrolysis in a resistance furnace.1.2 Petroleum coke containing up to 8 mass % sulfur can beanalyzed.1.3 The values stated in SI units are to
5、 be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices an
6、d determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1266 Test Method for Sulfur in Petroleum Products(Lamp Method)D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 6299 Practice
7、 for Applying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformanceD 6792 Practice for Quality System in Petroleum Productsand Lubricants Testing Laboratories3. Summary of Test Method3.1 Iodate Detection SystemThe sample is burned in astream of oxygen at a suff
8、iciently high temperature to convertabout 97 % of the sulfur to sulfur dioxide. A standardizationfactor is employed to obtain accurate results. The combustionproducts are passed into an absorber containing an acidsolution of potassium iodide and starch indicator. A faint bluecolor is developed in th
9、e absorber solution by the addition ofstandard potassium iodate solution. As combustion proceeds,bleaching the blue color, more iodate is added. The amount ofstandard iodate consumed during the combustion is a measureof the sulfur content of the sample.3.2 IR Detection SystemThe sample is weighed in
10、to aspecial ceramic boat which is then placed into a combustionfurnace at 1371C (2500F) in an oxygen atmosphere. Mostsulfur present is combusted to SO2which is then measuredwith an infrared detector after moisture and dust are removedby traps. A microprocessor calculates the mass percent sulfurfrom
11、the sample weight, the integrated detector signal and apredetermined calibration factor. Both the sample identificationnumber and mass percent sulfur are then printed out. Thecalibration factor is determined using standards approximatingthe material to be analyzed.4. Significance and Use4.1 This tes
12、t method provides a means of monitoring thesulfur level of various petroleum products and additives. Thisknowledge can be used to predict performance, handling, orprocessing properties. In some cases the presence of sulfurcompounds is beneficial to the product and monitoring thedepletion of sulfur c
13、an provide useful information. In othercases the presence of sulfur compounds is detrimental to theprocessing or use of the product.5. Interferences5.1 For the iodate systems, chlorine in concentrations lessthan 1 mass % does not interfere. The IR system can toleratesomewhat higher concentrations. N
14、itrogen when present inexcess of 0.1 mass % may interfere with the iodate systems; theextent of such interference may be dependent on the type ofnitrogen compound as well as the combustion conditions.Nitrogen does not interfere with the IR system. The alkali and1This test method is under the jurisdi
15、ction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved Dec. 1, 2007. Published January 2008. Originallyapproved in 1958. Last previous edition approved in 2003 as D 155203.2For referenced A
16、STM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright A
17、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Copyright by ASTM Intl (all rights reserved); Wed Jul 30 22:09:32 EDT 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.alkaline earth met
18、als, as well as zinc, phosphorus, and lead, donot interfere with either system.6. Apparatus6.1 Combustion and Iodate Detection System:6.1.1 FurnacesTwo major types are available, the pri-mary difference being the manner in which the necessary hightemperatures are obtained. These two types are as fol
19、lows:6.1.1.1 Induction Type, which depends upon the high-frequency electrical induction method of heating. This assem-bly shall be capable of attaining a temperature of at least1482C (2700F) in the sample combustion zone, under theconditions set forth in 9.1 and shall be equipped with anadditional i
20、nduction coil located above the combustion zone,substantially as shown in Fig. 1.6.1.1.2 The furnace work coil should have a minimumoutput of 500 W; the minimum input rating of the furnace mustbe 1000 W. With the correct amount of iron chips, weighed to60.05 g, the maximum plate current will be betw
21、een 350 and450 mA. (WarningThis type of furnace is capable ofinflicting high frequency burns and high-voltage shocks. Inaddition to other precautions, maintain all guards properly.)(WarningDisconnect the furnace from the power line when-ever electrical repairs or adjustments are made.)6.1.1.3 Resist
22、ance Type, capable of maintaining a tempera-ture of at least 1371C (2500F).6.1.2 Absorber, as described in Test Method D 1266.NOTE 1Also suitable for use with either type of furnace is anautomatic titrator, specifically designed for iodometry. This combines thefunctions of absorption and titration t
23、o a predetermined end point.6.1.3 Buret, standard 25-mL or automatic types availablefrom the manufacturers of the specific combustion units, aresuitable (Note 1).6.2 Combustion and IR Detection System, comprised ofautomatic balance, oxygen flow controls, drying tubes, com-bustion furnace, infrared d
24、etector and microprocessor. Thefurnace shall be capable of maintaining a nominal operatingtemperature of 1350C (2460F).36.3 Miscellaneous ApparatusSpecific combustion assem-blies require additional equipment such as crucibles, combus-tion boats, crucible lids, boat pushers, separator disks, com-bust
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