ASTM D2007-2003(2008) Standard Test Method for Characteristic Groups in Rubber Extender and Processing Oils and Other Petroleum-Derived Oils by the Clay-Gel Absorption Chromatograp.pdf

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1、Designation: D 2007 03 (Reapproved 2008)An American National StandardStandard Test Method forCharacteristic Groups in Rubber Extender and ProcessingOils and Other Petroleum-Derived Oils by the Clay-GelAbsorption Chromatographic Method1This standard is issued under the fixed designation D 2007; the n

2、umber immediately following the designation indicates the year oforiginal adoption or, in the case of revision, 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.1. Sco

3、pe1.1 This test method covers a procedure for classifying oilsamples of initial boiling point of at least 260C (500F) intothe hydrocarbon types of polar compounds, aromatics andsaturates, and recovery of representative fractions of thesetypes. This classification is used for specification purposes i

4、nrubber extender and processing oils.NOTE 1See Test Method D 2226.1.2 This test method is not directly applicable to oils ofgreater than 0.1 mass % pentane insolubles. Such oils can beanalyzed after removal of these materials, but precision isdegraded (see Appendix X1).1.3 The values stated in SI un

5、its are to 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 pr

6、actices and determine the applica-bility of regulatory limitations prior to use. Specific warningstatements are given in 6.1, Section 7, A1.4.1, and A1.5.5.2. Referenced Documents2.1 ASTM Standards:2D 2226 Classification for Various Types of Petroleum Oilsfor Rubber Compounding UseD 5309 Specificati

7、on for Cyclohexane 999E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 The following terms refer to the hydrocarbon typesand structural groups as measured by this test method:3.1.2

8、aromaticsmaterial that, on percolation, passesthrough a column of adsorbent clay in a n-pentane eluent butadsorbs on silica gel under the conditions specified.3.1.3 asphaltenes, or n-pentane insolublesinsoluble mat-ter that precipitates from a solution of oil in n-pentane underthe specified conditio

9、ns.3.1.4 polar aromaticssynonym for polar compounds.3.1.5 polar compoundsmaterial retained on adsorbentclay after percolation of the sample in n-pentane eluent underthe conditions specified.3.1.6 saturatesmaterial that, on percolation in a n-pentaneeluent, is not adsorbed on either the clay or silic

10、a gel under theconditions specified.4. Summary of Test Method4.1 The sample is diluted with solvent and charged to aglass percolation column containing clay in the upper sectionand silica gel plus clay in the lower section. n-pentane is thencharged to the double column until a definite quantity ofef

11、fluent has been collected. The upper (clay) section is removedfrom the lower section and washed further with n-pentane. Atoluene-acetone mixture 50 to 50 by volume is then charged tothe clay section for desorption and a specified volume ofeffluent collected. The lower (gel) column may be desorbed by

12、recirculation of toluene.4.2 The solvents are completely removed from the recov-ered n-pentane and the toluene-acetone fractions and theresidues are weighed and calculated as saturate and polarcompounds contents. Aromatics may be calculated by differ-ence, or measured following evaporation of the to

13、luene usedfor desorption of the gel column.4.3 When the sample contains more than 0.1 mass % ofn-pentane insolubles, this test method cannot be used directly.The insoluble matter must be removed from the sample prior tocharging to the column. A method for this removal is given asan appendix.4.4 Alte

14、rnative methods are provided (1) for recovery ofaromatics from the gel column, and (2) for analysis of oil withhigh-polar content.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.04.0C on Liquid

15、Chromatography.Current edition approved Dec. 1, 2008. Published February 2009. Originallyapproved in 1968. Last previous edition approved in 2003 as D 2007031.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of

16、ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 The composition of the oil included in rubber com-pounds has

17、 a large effect on the characteristics and uses of thecompounds. The determination of the saturates, aromatics, andpolar compounds is a key analysis of this composition.5.2 The determination of the saturates, aromatics, and polarcompounds and further analysis of the fractions produced isoften used a

18、s a research method to aid understanding of oileffects in rubber and other uses.6. Apparatus6.1 Beakers, Anticreep, 150-mL capacity, as illustrated inFig. 1.(WarningBeakers should be examined for sharpedges and fire polished, if necessary.)6.2 Clay-Gel Column, constructed as illustrated in Fig. 2.6.

19、3 Conical Flasks, (Erlenmeyer), 250-mL capacity.6.4 Solvent Receiver, capable of collecting solvent, withoutsplashing or loss of material during the analysis. A wide-mouth, graduated, 500-mL capacity Erlenmeyer flask is onesuch example that has been found suitable to use.6.5 Filter Funnel, long stem

20、, 125-mm diameter; for use with185 mm ready folded, fine-texture, rapid filter paper.6.6 Separatory Funnel, 500 mL.6.7 Hot Plate, explosion proof, controlled to a surfacetemperature of 100 to 105C.NOTE 2Temperatures should be uniform on the top of the hot plate.Some laboratory hot plates benefit by

21、the inclusion of an aluminum plate,approximately 6-mm thick, included under or on top of regular plate top.6.8 Round Bottom Flask, 3-necked, borosilicate, 500-mLcapacity (Fig. 3).6.9 Condenser, borosilicate (Fig. 3).6.10 Adapter Tube with Vigreux column (Fig. 3).3,46.11 Flexible Joint, TFE-fluorocar

22、bon and borosilicate,24/40 TSground glass joints on each end.4,57. Reagents and Materials7.1 Purity of Reagents, Reagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the commit-tee on Analytical Reagents

23、 of the American Chemical Society,where such specifications are available.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Acetone, reagent grade, minimum purity. (Warnin

24、gAcetone is extremely flammable.)7.3 Calcium Chloride, anhydrous granules.7.4 Clay Adsorbent, 500 to 250 m (30 to 60 mesh)Attapulgus.4,7Clay quality may be determined using theazobenzene equivalence test shown in Annex A1. The azoben-zene activity test measures the adsorptive characteristics of thec

25、lay. Azobenzene equivalence value should be 30 to 35. Clayoutside of these limits should be discarded.7.5 Cyclohexane, conforming to Specification D 5309. (Op-tional, see 8.1.9.) (WarningCyclohexane is extremely flam-mable. Harmful if inhaled.)7.6 Pentane,4,8reagent grade minimum purity.(Warningn-Pe

26、ntane is extremely flammable. Harmful ifinhaled.)7.7 Silica Gel, activated, conforming to the following in-spections:4,9Sieve analysis 30 sieve size, 5 % (mass) maximum;50 sieve size, 45 % (mass) min100 sieve size, 80 % (mass) min200 sieve size, 94 % (mass) min7.7.1 Gel should be activated for4hinan

27、airoven at 190Cin a shallow pan.7.8 Toluene, reagent grade minimum purity. (WarningToluene is flammable. Vapor harmful.)3The sole source of supply of the adapter tube known to the committee at thistime is Owens Glass Apparatus, Inc., 128 River Road, Channelview, TX 77530This item can be fabricated a

28、t any scientific glassblowing shop.4If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee1, which you may attend.5Cole Parmer No. 6675-40 has

29、been found suitable for this purpose.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U

30、.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.7The sole source of supply of clay adsorbent known to the committee at this timeis Forcoven Products, 22010 East Martin Dr., Porter, TX 77365. Packaged inmoisture resistant twinned

31、 packets of 50 and 100 g (sufficient for one determina-tion). These packets are packed 50 sets per case. It is important that extremes oftemperature be avoided on stored clay samples.8The sole source of supply of pentane known to the committee at this time isSpecial Products Div., Phillips Petroleum

32、 Co., Bartlesville, OK.9The sole source of supply of silica gel meeting these specifications known tothe committee at this time is Forcoven Products, 22010 East Martin Dr., Porter, TX77365, packaged in 200 g moisture resistant packets. Sieve analysis should bechecked on other sources of gel.FIG. 1 A

33、nticreep BeakerD 2007 03 (2008)27.9 Toluene-Acetone Mixture (50 to 50 by volume), mixequal volumes of toluene and acetone.7.10 In order to obtain results that are consistent with thoseobtained elsewhere, it is very important that only the reagentsand materials described in this section be used.8. Pr

34、ocedure8.1 Fractionation:8.1.1 Prepare the adsorption column (Fig. 2) by placing 100g of clay adsorbent in the upper section of the column and 200g of silica gel plus 50 g of clay on top of the gel in the lowersection (Note 5). Place a piece of glass wool (of about 25-mmloose thickness) over the top

35、 surface of the clay in the uppercolumn to prevent agitation of the clay while charging theeluent solvents. Join the columns (clay over gel) after lubri-cating the joint with hydrocarbon-insoluble grease. It is impor-tant that the adsorbents in each column be packed to a constantlevel. A minimum of

36、ten taps with a soft rubber hammer atdifferent points up and down and 25 taps on top of each columnshould be employed to achieve constant level. A suitablerubber hammer may be assembled by fastening two No. 7 or 8rubber stoppers on one end of a small rod about 200-mm long.Use fresh adsorbents for ea

37、ch determination.8.1.2 If n-pentane insolubles were not determined, select theappropriate sample size in accordance with the following polarcontent ranges, if the proper range can be anticipated; other-wise, use a 10 6 0.5 g sample.Polar Content Range,mass percent Sample Size, g020 10 6 0.5Above 20

38、5 6 0.28.1.3 Dilute with 25 mL of n-pentane solvent and mix wellto ensure a uniform solution of the sample. The sample shouldnot display precipitate or flocculate at this point. If a precipitateis present asphaltenes may be removed by the procedure ofAppendix X1, however, the precision statement no

39、longerapplies. It is important that the polar content result obtained benot greater than that for the sample size as specified above,since the capacity of the clay for retaining polar constituentsbecomes limited at these concentrations. If results exceed thisNOTECheck to ascertain ID is 44 mm.FIG. 2

40、 Clay-Gel Percolating ColumnD 2007 03 (2008)3specification, repeat the test using a smaller sample. Partition-ing between aromatics and polar compounds is affected bysample size. Results using different sample size may not beequivalent.NOTE 3For viscous oils, dilutions of the sample with 25 mL ofcyc

41、lohexane is more convenient and does not affect the results. Cyclo-hexane used in this manner will not detect small quantities of asphaltenes,however.8.1.4 Add 25 mL of n-pentane to the top of the clay portionof the assembled column and allow to percolate into the clay.As soon as nearly all of the n

42、-pentane has entered the clay,charge to the column the diluted sample of 8.1.3. Wash thesample beaker (or flask) with n-pentane and add the washingsto the column. After nearly all of this material has entered theclay, wash the walls of the column above the clay free ofsample with n-pentane. The samp

43、le and eluent solvent can beadded to the column through a 65-mm diameter, wide-stemfunnel (the funnel can be left on top of the column). At no timeduring the run should air be allowed to enter the clay bed.8.1.5 When nearly all of the washings have entered the clay,charge n-pentane to the column and

44、 maintain a head level wellabove the clay beds (Note 4) to wash the saturate portion of thesample from the adsorbents. Recover 280 6 10 mL of the firstn-pentane effluent from the column in a graduated, 500-mLwide-mouth conical flask.NOTE 4Columns may be briefly separated, if necessary, to give asolv

45、ent head 5- to 10-mm deep in the second (lower) column. Loss of thehead will give channeling in the lower column, with inaccurate results.NOTE 5With long use, the frits in the absorption columns becomeprogressively less porous. If the time for percolation doubles over that fora new column, the slow

46、columns are to be discarded.NOTE 6If only saturates are to be determined, proceed to 8.3 andsubsequent calculation of saturates.8.1.6 Disconnect the two sections. Allow the lower sectionto drain into a receiver. Continue washing the upper claysection with n-pentane. Maintain a moderate liquid head l

47、evelabove the clay during this wash and adjust n-pentane additionsso that the level is about 25 mm when 150 mL have beencollected in the receiver. Discontinue additions at this point andallow the liquid to essentially drain from the column. Thequantity in the receiver should then be about 200 mL. Th

48、en-pentane from this step and from the draining of the lowercolumn should be discarded if aromatics are to be determinedby difference. This n-pentane should be added to the aromaticssolution from the gel column during solvent evaporation (8.3)if aromatics are to be recovered.NOTE 7This extra n-penta

49、ne washing of the clay section is necessaryin order to ensure complete removal of aromatics from the clay.8.1.7 After n-pentane effluent has essentially drained fromthe column, charge a 50 to 50 volume mixture of tolueneac-etone. Collect the effluent in a 500-mL separatory funnel.Collect 250 mLof the toluene-acetone (plus n-pentane) effluentor until the effluent is practically colorless (only in exceptionalcases will more than 300 mL of effluent be required).8.1.8 Stopper the separatory funnel containing the toluene-acetone fraction and swirl it a few time