1、Designation: D6805 02 (Reapproved 2016)Standard Practice forInfrared (IR) Procedure for Determination of Aromatic/Aliphatic Ratio of Bituminous Emulsions1This standard is issued under the fixed designation D6805; the number immediately following the designation indicates the year oforiginal adoption
2、 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 determine
3、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 in
4、 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.2
5、. Referenced Documents2.1 ASTM Standards:2D2939 Test Methods for Emulsified Bitumens Used asProtective Coatings (Withdrawn 2012)33. 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. Exam
6、ples of aliphatic compounds in-clude paraffins (alkanes), olefins (alkenes), and acetylenes(alkynes). These compounds are primarily found in petroleumsources. Hawleys Condensed Chemical Dictionary43.1.2 aromatica group of organic compounds made up ofunsaturated cyclic hydrocarbons containing one or
7、more rings,an example 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 Dictionary43.1.3 infrared absorbancethe range of wavelengths
8、in theinfrared 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 Chemi
9、cal Dictionary44. 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
10、(aliphatic) to 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
11、to 1mm path length.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.1This practice is under the jur
12、isdiction ofASTM Committee D08 on Roofing andWaterproofing and is the direct responsibility of Subcommittee D08.09 on Bitumi-nous Emulsions.Current edition approved May 1, 2016. Published May 2016. Originallyapproved in 2002. Last previous edition approved in 2008 as D6805 02 (2008).DOI: 10.1520/D68
13、05-02R16.2For 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 website.3The last approved version of this historical standa
14、rd is referenced onwww.astm.org.4Lewis, R. J., Sr., Hawleys Condensed Chemical Dictionary, ThirteenthEdition, New York, Van Nostrand Reinhold, 1997.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Reagents and Materials7.1 Disposabl
15、e “Medicine” 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.7.6 Sodium Sulfate (Na2SO4), anhydrous.8. Hazards8.1 Carbon disulfide (CS2) is a hazardous materi
16、al and mustbe handled properly. Before using CS2, read and understand theCS2Material Safety Data Sheet and the label on the CS2bottle.Use appropriate precautions, including safety equipment, whenhandling CS2. Be sure to work in a properly operating hoodand wear appropriate gloves.9. Sampling, Test S
17、pecimens, and Preparation9.1 Every effort should be taken to ensure that a represen-tative sample is taken. Follow Section 4 from Test MethodsD2939 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 Wo
18、rking Sample11.1 Stir thoroughly to obtain representative sample.11.2 Dissolution in Solvent (CS2):11.2.1 Weigh 0.2 6 0.01 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,
19、bituminous emulsion, andNa2SO4. Cap vial and mix on mechanical shaker for 15 min.Then filter quickly (to minimize CS2evaporation) through fastfilter paper into another clean vial; save filtrate.NOTE 1CS2is preferred, as any hydrogen-containing solvent willcause interference during the IR analysis.12
20、. Preparation of Apparatus12.1 Remove any previous solution of CS2and bituminousemulsion from the IR cell using a cell cleaner (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.
21、12.2 Because the moisture in the air easily etches the NaClcell, store sodium chloride (NaCl) cell in a desiccator.13. Procedure13.1 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.1
22、3.1.3 Fill the IR sample cell, using a dropper or syringe,with the CS2/bituminous emulsion filtered solution.NOTE 2Follow 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 spectru
23、mfrom 2.5 to 4.2 m in the absorbance mode. Linearly ruledchart paper is used in the absorbance mode; however, if theinstrument 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 p
24、rocedure).13.1.5 Record the following information on the chart paper:13.1.5.1 Sample number,13.1.5.2 Sample identification,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.
25、1 The determination of absorbance (A) is dependent onthe operational mode of the IR instrument and the chart paperused. Record 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
26、3.27 m (aromatic) and at 3.40 m (aliphatic).Absorbance can be determined by recording the value of thepeak on the chart and 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 P
27、aper)The procedure isessentially the same as in 14.1.1 except the peak direction isreversed.14.1.3 Transmittance Mode (Linear Paper)Read values asin 14.1.2, except divide the peak value by the baseline value toobtain the Transmittance Percentage (T). See TransmittanceGraph in Appendix X2 (Fig. X2.1)
28、. Calculate Absorbance (A)according to the equations below:Aaromatic!5 log1Taromatic!52logTaromatic!(1)Aaliphatic!5 log1Taliphatic!52logTaliphatic!(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.
29、01).16. Precision and Bias16.1 Precision:16.1.1 The repeatability standard deviation of the IR ratiohas been determined to be 0.10 absolute.16.1.2 The reproducibility of this practice is being deter-mined and will be available in 2005.D6805 02 (2016)217. Keywords17.1 absorbance; aliphatic; aromatic;
30、 asphalt; bituminous;coal tar; emulsion; infrared; sealerAPPENDIXES(Nonmandatory Information)X1. TYPICAL AROMATICITY INDICES (Ia) OF VARIOUS MATERIALSX2. ABSORBANCE AND TRANSMITTANCE GRAPHS USED IN CALCULATING AN AROMATIC INDEX (Ia)Sample IaAsphalt (aliphatic) Emulsion 0.03Coal Tar (aromatic) Emulsi
31、on 2.2350/50 Asphalt/Coal Tar Emulsion 0.09Typical Aromatic Emulsion BlendA1.94AContains aromatic coal tar and aromatic petroleum compounds.FIG. X2.1 Absorbance GraphD6805 02 (2016)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item
32、 mentionedin this standard. Users of this standard are expressly advised that determination of the validity 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 commi
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34、eting of theresponsible technical committee, which you may attend. If you feel that your comments have 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,
35、 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ X2.2 Transmittance GraphD6805 02 (2016)4
