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ASTM D1094-07 (Reapproved 2013)

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ASTM D1094-07 (Reapproved 2013)

Designation D1094 − 07 Reapproved 2013 An American National StandardStandard Test Method forWater Reaction of Aviation Fuels1This standard is issued under the fixed designation D1094; the number 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the determination of the pres-ence of water-miscible components in aviation gasoline andturbine fuels, and the effect of these components on volumechange and on the fuel-water interface.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included 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. This standardinvolves the use of hazardous chemicals identified in Section 7.Before using this standard, refer to suppliers’ safety labels,Material Safety Data Sheets and other technical literature.2. Referenced Documents2.1 ASTM Standards2D381 Test Method for Gum Content in Fuels by Jet Evapo-rationD611 Test Methods for Aniline Point and Mixed AnilinePoint of Petroleum Products and Hydrocarbon SolventsD1836 Specification for Commercial HexanesD2699 Test Method for Research Octane Number of Spark-Ignition Engine FuelD2700 Test Method for Motor Octane Number of Spark-Ignition Engine FuelD3948 Test Method for Determining Water Separation Char-acteristics ofAviation Turbine Fuels by Portable Separom-eter2.2 Energy Institute Standard3IP Standard Test Methods Vol 2, Appendix B, Specificationfor Petroleum Spirits3. Terminology3.1 Definitions of Terms Specific to This Standard3.1.1 film, nthin, translucent layer that does not adhere tothe wall of the glass cylinder.3.1.2 lace, nfibers thicker than hairlike shred or of whichmore than 10 are interlocking, or both.3.1.3 loose lace or slight scum, or both Table 2, Rating 3,nan assessment that the fuel/buffer solution interface iscovered with more than 10 but less than 50 of lace orscum that does not extend into either of the two layers.3.1.4 scum, nlayer thicker than film or that adheres to thewall of the glass cylinder, or both.3.1.5 shred, nhairlike fibers of which less than 10 areinterlocking.3.1.6 shred, lace or film at interface Table 2, Rating 2,nan assessment that fuel/buffer solution interface containsmore than 50 clear bubbles or some but less than 10 shred, lace, film or both.3.1.7 tight lace or heavy scum, or both Table 2, Rating 4,nan assessment that the fuel/buffer solution interface iscovered with more than 50 of lace or scum, or both, thatextends into either of the two layers or forms an emulsion, orboth.3.1.8 water reaction interface conditions rating, na quali-tative assessment of the tendency of a mixture of water andaviation turbine fuel to form interface films or precipitates.3.1.9 water reaction separation rating, na qualitativeassessment of the tendency of insufficiently cleaned glasswareto produce emulsions or precipitates, or both, in separated fueland water layers.3.1.10 water reaction volume change, na qualitative indi-cation of the presence in aviation gasoline of water-solublecomponents.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricantsand is the direct responsibility of SubcommitteeD02.J0.05 on Fuel Cleanliness.Current edition approved May 1, 2013. Published August 2013. Originallyapproved in 1950. Last previous edition approved in 2007 as D1094–07. DOI10.1520/D1094-07R13.2For 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 standard’s Document Summary page onthe ASTM website.3Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http//www.energyinst.org.uk.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Summary of Test Method4.1 A sample of the fuel is shaken, using a standardizedtechnique, at room temperature with a phosphate buffer solu-tion in scrupulously cleaned glassware. The cleanliness of theglass cylinder is tested. The change in volume of the aqueouslayer and the appearance of the interface are taken as the waterreaction of the fuel.5. Significance and Use5.1 When applied to aviation gasoline, water reaction vol-ume change using the technique reveals the presence ofwater–soluble components such as alcohols. When applied toaviation turbine fuels, water reaction interface rating using thetechnique is not reliable in revealing the presence of surfactantswhich disarm filter-separators quickly and allow free water andparticulates to pass; but can reveal the presence of other typesof contaminants. Other tests, such as Test Method D3948, arecapable of detecting surfactants in aviation fuels.6. Apparatus6.1 Graduated Glass Cylinder, glass-stoppered, 100 mL,with 1-mL graduations. The distance between the 100-mLmark and the top of the shoulder of the cylinder must be withinthe range from 50 to 60 mm.7. Reagents7.1 Purity of ReagentsReagent 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 of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficient purity to permit its use without lessening the accu-racy of the determination.7.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean distilled water, or waterof equivalent purity.7.3 AcetoneWarningFlammable. Health hazard.7.4 Glass-Cleaning SolutionSaturate concentrated sulfu-ric acid H2SO4, sp gr 1.84 with potassium dichromateK2Cr2O7 or sodium dichromate Na2Cr2O7. WarningCorrosive. Health hazard. Oxidizing agent.7.5 n-HexaneConforming to Specification D1836 orn-heptane conforming to material used in Test Methods D611,D381, D2699, and D2700 or petroleum spirit 60/80 conform-ing to IPAppendix B Specification, or equivalent. WarningFlammable. Health hazard.7.6 Phosphate Buffer Solution pH 7Dissolve 1.15 g ofpotassium monohydrogen phosphate, anhydrous K2HPO4and 0.47 g of potassium dihydrogen phosphate, anhydrousKH2PO4 in 100 mL of water. Larger volumes of the phos-phate buffer solution may be prepared provided the concentra-tion of K2HPO4and KH2PO4in the water solution isequivalent to that described above. As an alternative, thelaboratory may use a commercially prepared solution.8. Preparation of Apparatus8.1 Clean the graduated cylinder thoroughly before carryingout this test. Only cylinders that are adequately cleaned can beused.8.1.1 Remove traces of oil from the graduated cylinder andstopper by flushing with hot tap water, brushing if necessary.Alternately, remove all traces of oil from the graduatedcylinder and stopper, using either n-hexane or n-heptane or theIPpetroleum solvent 60/80. Rinse with acetone followed by tapwater.8.1.2 Following the washing described in 8.1.1, immerse thecylinder and stopper in either 1 a non-ionic detergent clean-ing solution, or 2 glass cleaning solution described in 7.4.The type of non-ionic detergent and conditions for its use needto be established in each laboratory. The criterion for satisfac-tory cleaning shall be a matching of the quality of that obtainedwith chromic acid cleaning solution. Non-ionic detergentcleaning avoids the potential hazards and inconveniencesrelated to handling corrosive chromic acid solutions. The latterremains as the reference cleaning practice and as such mayfunction as an alternate to the preferred procedure-cleaningwith non-ionic detergent solutions. Following cleaning withnon-ionic detergent or glass cleaning solution, rinse with tapwater, then distilled water, and finally rinse with phosphatebuffer solution and drain.8.1.3 Inadequately cleaned glassware used in this test cangive misleading indications of fuel contaminants. Use onlycylinders that are adequately cleaned. Cylinders that draincleanly are adequately cleaned. Alternatively, a separationrating see Table 1 of 2 or less is indicative of adequatelycleaned glassware.9. Preparation of Samples9.1 It is desirable to take a sample of at least 100 mL toperform this test. A clean container is required.9.2 Under no circumstances shall the sample be prefilteredafter collection. Filtration media can remove surfactants, thedetection of which is one of the purposes of this test method.If the test fuel sample is contaminated with particulate matter,allow it to settle before testing.4Reagent 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.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. USPC, Rockville,MD.TABLE 1 SeparationRating Appearance1 Complete absence of all emulsions and/orprecipitates within either layer or upon the fuellayer.2 Same as 1, except small air bubbles or smallwater droplets in the fuel layer.3 Emulsions and/or precipitates within either layer orupon the fuel layer, and/or droplets in the waterlayer or adhering to the cylinder walls, excludingthe walls above the fuel layer.D1094 − 07 20132NOTE 1Test method results are known to be sensitive to tracecontamination from sampling containers.10. Procedure10.1 Measure 20 mL of phosphate buffer solution at roomtemperature into the cylinder and record the volume to thenearest 0.5 mL.Add 80 mL, at room temperature, of the fuel tobe tested and stopper the cylinder.10.2 Shake the cylinder for 2 min 6 5 s, two to three strokesper second using 5 to 10-in. 12 to 25-cm strokes.WarningTake care to avoid a swirling motion duringshaking of the cylinder since swirling action tends to break anyemulsion that might be formed.10.3 Immediately place the cylinder on a vibration-freesurface and allow the contents to settle undisturbed for 5 min.10.4 Without picking up the cylinder, record the following,viewing in diffused light10.4.1 The change in volume of the aqueous layer to thenearest 0.5 mL.10.4.2 The condition of the interface in accordance withTable 2.10.4.3 The degree of separation of the two phases inaccordance with Table 1.10.4.4 Disregard any slight cloudiness in the fuel layer thatis no longer visible when viewed against a white background.11. Report11.1 The report shall include the following11.1.1 Change in volume of the aqueous layer to the nearest0.5 mL.11.1.2 Rating of the condition of the interface see Table 2.11.1.3 Rating of the degree of separation see Table 1.12. Precision and Bias12.1 PrecisionThe change in volume of the aqueous layeris a measure of water reaction of aviation gasoline and is aqualitative indication of water–miscible components and is notsubject to a statement of precision.12.1.1 It is not practical to specify the precision of theinterface rating as a measure of the water reaction of aviationturbine fuels because results of the ratings described in Table 2are purely qualitative. Table 2 assigns a number to descriptionsof interface appearance as a convenient guide to qualitativeratings.12.2 BiasThe procedure in this test for water reaction ofaviation fuels has no bias because the value of volume changeand interface rating is defined only in terms of the test method.13. Keywords13.1 aviation gasoline; aviation turbine fuel; fuel waterinterface surfactants; water reaction; water-soluble additivesASTM 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 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 committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments 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 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, 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 websitewww.astm.org. Permission rights to photocopy the standard may also be secured from the ASTM website www.astm.org/COPYRIGHT/.TABLE 2 Interface ConditionsARating Appearance1 Clear and clean1b Clear bubbles covering not more than anestimated 50 of the interface and no shreds,lace, or film at the interface2 Shred, lace, or film at interface3 Loose lace or slight scum, or both4 Tight lace or heavy scum, or bothASection 3 contains definitions of terms used in this table.D1094 − 07 20133

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