ASTM D1552-2008 Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)《石油产品中硫的试验方法(高温法)标准试验方法》.pdf
《ASTM D1552-2008 Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)《石油产品中硫的试验方法(高温法)标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D1552-2008 Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)《石油产品中硫的试验方法(高温法)标准试验方法》.pdf(7页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 1552 08An 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 () 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 proc
4、edures 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 and
6、 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 Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD 6792 Practice for Quality System in Petroleum Productsand Lubricants Testing Laboratories3. Summary of Test Method3.1 Iodate Detection SystemThe sample is burned in astream
8、 of oxygen at a sufficiently 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 bluecolo
9、r is developed in the 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
10、sample is weighed into 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
11、 percent sulfurfrom 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
12、 and Use4.1 This test 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 thed
13、epletion of sulfur can 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 high
14、er concentrations. Nitrogen when present in1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved Dec. 1, 2008. Published December 2008. Originallyappr
15、oved in 1958. Last previous edition approved in 2007 as D 155207.2For referenced ASTM 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 webs
16、ite.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.excess of 0.1 mass % may interfere with the iodate systems; theextent of such interference may be dependent on the
17、type ofnitrogen compound as well as the combustion conditions.Nitrogen does not interfere with the IR system. The alkali andalkaline earth metals, 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
18、types are available, the pri-mary difference being the manner in which the necessary hightemperatures are obtained. These two types are as follows: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 temp
19、erature of at least1482C (2700F) in the sample combustion zone, under theconditions set forth in 9.1 and shall be equipped with anadditional induction 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 minim
20、um 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 between 350 and450 mA. (WarningThis type of furnace is capable ofinflicting high frequency burns and high-voltage shocks. Inaddition to other precautions, maintai
21、n all guards properly.)(WarningDisconnect the furnace from the power line when-ever electrical repairs or adjustments are made.)6.1.1.3 Resistance 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
22、 either type of furnace is anautomatic titrator, specifically designed for iodometry. This combines thefunctions of absorption and titration to a predetermined end point.6.1.3 Buret, standard 25-mL or automatic types availablefrom the manufacturers of the specific combustion units, aresuitable (Note
23、 1).6.2 Combustion and IR Detection System, comprised ofautomatic balance, oxygen flow controls, drying tubes, com-bustion furnace, infrared detector and microprocessor. Thefurnace shall be capable of maintaining a nominal operatingtemperature of 1350C (2460F).36.3 Miscellaneous ApparatusSpecific co
24、mbustion assem-blies require additional equipment such as crucibles, combus-tion boats, crucible lids, boat pushers, separator disks, com-bustion tubes, sample inserters, oxygen flow indicator, andoxygen drying trains. The additional equipment required isdependent on the type of furnace used and is
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