ASTM D6805-2002(2008) 952 Standard Practice for Infrared (IR) Procedure for Determination of Aromatic Aliphatic Ratio of Bituminous Emulsions《测定沥青乳液芳香剂 脂肪比的红外法的标准实施规程》.pdf

1、Designation: D 6805 02 (Reapproved 2008)Standard Practice forInfrared (IR) Procedure for Determination of Aromatic/Aliphatic Ratio of Bituminous Emulsions1This standard is issued under the fixed designation D 6805; the number immediately following the designation indicates the year oforiginal adopti

2、on 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. Scope1.1 This practice uses infrared analytical techniques toqualitatively determin

3、e in the laboratory a ratio of aromaticabsorbance to aliphatic absorbance. This practice may be usedto determine if the bitumen in the emulsion is predominantlyaromatic or aliphatic in nature.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included

4、in thisstandard.1.3 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 determine the applica-bility of regulatory limitations prior to use

5、.2. Referenced Documents2.1 ASTM Standards:2D 2939 Test Methods for Emulsified Bitumens Used asProtective Coatings3. Terminology3.1 Definitions:3.1.1 aliphatica group of organic compounds character-ized by straight- or branched-chain arrangements of the con-stituent carbon atoms. Examples of aliphat

6、ic compounds in-clude paraffins (alkanes), olefins (alkenes), and acetylenes(alkynes). These compounds are primarily found in petroleumsources. Hawleys Condensed Chemical Dictionary33.1.2 aromatica group of organic compounds made up ofunsaturated cyclic hydrocarbons containing one or more rings,an e

7、xample of which is benzene. Large numbers of thesecompounds are derived from petroleum and coal tar, and areclassified as “aromatics” because of their strong and notunpleasant odor characteristics.Hawleys Condensed Chemical Dictionary33.1.3 infrared absorbancethe range of wavelengths in theinfrared

8、that are absorbed by a specimen and identify itsmolecular components and compound structures. The infraredregion of the electromagnetic spectrum includes wavelengthsfrom 0.70 m to approximately 300 m, that is, longer thanvisible light and shorter than microwave.Hawleys Condensed Chemical Dictionary3

9、4. Summary of Practice4.1 A sample of bituminous emulsion from which the waterhas been removed using Na2SO4is dissolved in carbondisulfide (CS2), and the infrared (IR) absorbance from 2.5 to4.2 m is determined. The absorbance at 3.27 m (aromatic) isdivided by the absorbance at 3.40 m (aliphatic) to

10、obtain theIR ratio.5. Significance and Use5.1 The results of this practice may be used to distinguishtar-based emulsion from an asphalt-based emulsion for speci-fication compliance purposes.6. Apparatus6.1 Infrared Spectrophotometer.6.2 Sealed Sodium Chloride (NaCl) IR Cell, with 0.1 to 1mm path len

11、gth.6.3 IR Cell Cleaner.6.4 Vacuum Pump and Dry-Ice Trap, to protect pump.6.5 Syringe, glass, 10 mL.6.6 Mechanical Shaker.6.7 Sieves, No. 40 (425 m opening) and No. 100 (150 m).6.8 Balance, capable of weighing to 0.001 g.6.9 Pipet, 10 mL and rubber bulb.7. Reagents and Materials7.1 Disposable “Medic

12、ine” Dropper.7.2 Vial, 20 mL, with cork-backed metal foil liner.7.3 Filter Paper, rapid flow rate, 12.5 cm.7.4 Glass Funnel, for above filter paper.7.5 Carbon Disulfide (CS2), spectroscopy grade.1This practice is under the jurisdiction ofASTM Committee D08 on Roofing andWaterproofing and is the dire

13、ct responsibility of Subcommittee D08.09 on Bitumi-nous Emulsions.Current edition approved Dec. 1, 2008. Published December 2008. Originallyapproved in 2002. Last previous edition approved in 2002 as D 6805 021.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cust

14、omer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Lewis, R. J., Sr., Hawleys Condensed Chemical Dictionary, ThirteenthEdition, New York, Van Nostrand Reinhold, 1997.1Copyright ASTM International, 100

15、 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.6 Sodium Sulfate (Na2SO4), anhydrous.8. Hazards8.1 Carbon disulfide (CS2) is a hazardous material and mustbe handled properly. Before using CS2, read and understand theCS2Material Safety Data Sheet and the label on th

16、e CS2bottle.Use appropriate precautions, including safety equipment, whenhandling CS2. Be sure to work in a properly operating hoodand wear appropriate gloves.9. Sampling, Test Specimens, and Preparation9.1 Every effort should be taken to ensure that a represen-tative sample is taken. Follow Section

17、 4 from Test MethodsD 2939 for sampling.10. Dehydration of Sample10.1 Dehydration is not necessary since a drying agent(Na2SO4) will be added in a later step.11. Preparation of Working Sample11.1 Stir thoroughly to obtain representative sample.11.2 Dissolution in Solvent (CS2):11.2.1 Weigh 0.2 6 0.0

18、1 g of bituminous emulsion into avial using a disposable “medicine” dropper and add about 1 gof anhydrous Na2SO4. Using a 10 mL pipet and rubber bulb,add 10 mL of CS2to the vial, bituminous emulsion, andNa2SO4. Cap vial and mix on mechanical shaker for 15 min.Then filter quickly (to minimize CS2evap

19、oration) through fastfilter paper into another clean vial; save filtrate.NOTE 1CS2is preferred, as any hydrogen-containing solvent willcause interference during the IR analysis.12. Preparation of Apparatus12.1 Remove any previous solution of CS2and bituminousemulsion from the IR cell using a cell cl

20、eaner (blowing thesolution out) or by using a vacuum source and an appropriatedry-ice trap. Clean the cell with fresh CS2; the cell should befilled with fresh CS2at least 3 times.12.2 Because the moisture in the air easily etches the NaClcell, store sodium chloride (NaCl) cell in a desiccator.13. Pr

21、ocedure13.1 Determination of IR Spectrum:13.1.1 Determine spectrum within1hofextraction withCS2.13.1.2 Fill the IR reference cell, using a dropper or syringe,with the CS2solvent.13.1.3 Fill the IR sample cell, using a dropper or syringe,with the CS2/bituminous emulsion filtered solution.NOTE 2Follow

22、 the filling directions supplied by the cell(s) manufac-turer.13.1.4 Referring to the instructions supplied with the par-ticular IR instrument being used, determine the IR spectrumfrom 2.5 to 4.2 m in the absorbance mode. Linearly ruledchart paper is used in the absorbance mode; however, if theinstr

23、ument can only be operated in the Transmittance mode,use logarithmically ruled chart paper (if log paper is notavailable, follow Transmittance mode for linear paper calcula-tion procedure).13.1.5 Record the following information on the chart paper:13.1.5.1 Sample number,13.1.5.2 Sample identificatio

24、n,13.1.5.3 Date of analysis,13.1.5.4 Analysts name,13.1.5.5 Cell used (NaCl), and13.1.5.6 Solvent used (CS2).13.1.6 Draw a baseline from 2.7 to 4.0 m.14. Calculation of Results14.1 The determination of absorbance (A) is dependent onthe operational mode of the IR instrument and the chart paperused. R

25、ecord aromatic as A(aromatic). Record aliphatic absor-bance as A(aliphatic). The various methods are explained below:14.1.1 Absorbance Mode (Linear Paper)Determine ab-sorbance at 3.27 m (aromatic) and at 3.40 m (aliphatic).Absorbance can be determined by recording the value of thepeak on the chart a

26、nd subtracting the value of the baselineunder the peak. Estimate values to the nearest tenth (0.1). SeeAbsorbance Graph in Appendix X2 (Fig. X2.2).14.1.2 Transmittance Mode (Log Paper)The procedure isessentially the same as in 14.1.1 except the peak direction isreversed.14.1.3 Transmittance Mode (Li

27、near Paper)Read valuesas in 14.1.2, except divide the peak value by the baseline valueto obtain the Transmittance Percentage (T). See TransmittanceGraph in Appendix X2 (Fig. X2.1). Calculate Absorbance (A)according to the equations below:Aaromatic!5 log1Taromatic!52log Taromatic!(1)Aaliphatic!5 log1

28、Taliphatic!52log Taliphatic!(2)14.2 The IR ratio is calculated as follows:IR ratio 5Aaromatic!Aaliphatic!(3)15. Report15.1 Report aromatic/aliphatic IR ratio to nearest hundredth(0.01).16. Precision and Bias16.1 Precision:16.1.1 The repeatability standard deviation of the IR ratiohas been determined

29、 to be 0.10 absolute.16.1.2 The reproducibility of this practice is being deter-mined and will be available in 2005.17. Keywords17.1 absorbance; aliphatic; aromatic; asphalt; bituminous;coal tar; emulsion; infrared; sealerD 6805 02 (2008)2APPENDIXES(Nonmandatory Information)X1. TYPICAL AROMATICITY I

30、NDICES (Ia) OF VARIOUS MATERIALSSample IaAsphalt (aliphatic) Emulsion 0.03Coal Tar (aromatic) Emulsion 2.2350/50 Asphalt/Coal Tar Emulsion 0.09Typical Aromatic Emulsion BlendA1.94AContains aromatic coal tar and aromatic petroleum compounds.D 6805 02 (2008)3X2. ABSORBANCE AND TRANSMITTANCE GRAPHS USE

31、D IN CALCULATING AN AROMATIC INDEX (Ia)FIG. X2.1 Absorbance GraphD 6805 02 (2008)4ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the v

32、alidity of any such patent rights, and the riskof 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 andif not revised, either reapproved or withdrawn. Your c

33、omments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments ha

34、ve not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).FIG. X2.2 Transmittance GraphD 6805 02 (2008)5