1、Designation: D 5006 03An American National StandardStandard Test Method forMeasurement of Fuel System Icing Inhibitors (Ether Type) inAviation Fuels1This standard is issued under the fixed designation D 5006; the number immediately following the designation indicates the year oforiginal adoption or,
2、 in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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.
3、1 This test method covers a technique for measuring theconcentration of Diethylene Glycol Monomethyl Ether (Di-EGME) in aviation fuels. The HB and Brix scale refractome-ters are specified to determine the concentration of this fuelsystem icing inhibitor (FSII) by measuring the refractive indexof a w
4、ater extract. Precision estimates have been determinedfor the DiEGME additive using specific extraction ratios witha wide variety of fuel types. The extraction ratios are highenough that portable handheld refractometers can be used, butnot so high as to sacrifice accuracy or linearity, or both, in t
5、he0.01 to 0.25 vol % range of interest.1.2 DiEGME is fully described in Specification D 4171 andin other specifications.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is
6、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. Referenced Documents2.1 ASTM Standards:2D 4171 Specification for Fuel System Icing InhibitorsE 1 Specification for ASTM Ther
7、mometersE 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 Brix scalea refractometer with a refractive indexscale calibrated to weight percent cane sugar (sucrose).3.1.2 HBa refract
8、ometer that can be used in a temperaturerange from 18 to 35C without incorporating a temperaturecorrection factor.3.2 Acronyms:3.2.1 DiEGMEDiethylene Glycol Monomethyl Ether3.2.2 FSIIfuel system icing inhibitor4. Summary of Test Method4.1 In order to determine the concentration of DiEGME inaviation
9、fuel, a measured volume of fuel is extracted with afixed ratio of water. The extraction procedure includes suffi-cient agitation and contacting time to ensure that equilibriumdistributions are attained. With the HB refractometer,3,4severaldrops of the water extract are placed on the prism face and t
10、hevolume percent DiEGME is read directly from a customgraduated scale printed on the reticule. If the Brix refractome-ter is used, a temperature correction factor is first applied to thereading, multiplied by 2 and divided by 100 to calculatevolume percent DiEGME. (WarningDiethylene glycolmonomethyl
11、 ether (DiEGME), Slightly toxic material. Thismaterial caused slight embryo-fetal toxicity (delayed develop-ment) but no increase in birth defects in laboratory animals.Consult the suppliers material safety data sheet.)NOTE 1Isopropanol is not detected because of the similarity ofisopropanol/water r
12、efractive indices, and the presence of isopropanol infuel containing other additives results in lower than true values.5. Significance and Use5.1 DiEGME is miscible with water and can be readilyextracted from the fuel by contact with water during shipping1This test method is under the jurisdiction o
13、f ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.J0 on Aviation Fuels.Current edition approved Dec. 1, 2003. Published January 2004. Originallyapproved in 1989. Last previous edition approved in 2002 as D 500602.2For referenced ASTM standar
14、ds, 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 sole source of supply of the HB refractometer known to the committee atthis time is
15、Gammon Technical Products, Inc., 2300 Hwy 34, P.O. Box 400,Manasquan, NJ 08736. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee1, whichyou
16、 may attend.4After July 1, 2003, all HB refractometers provided by Gammon TechnicalProducts will contain only the DiEGME scale on the instrument reticle.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.and in storage. Methods are ther
17、efore needed to check theadditive content in the fuel to ensure proper additive concen-tration in the aircraft.5.2 This test method is applicable to analyses performed inthe field or in a laboratory.6. Apparatus6.1 RefractometerThe HB temperature compensated, di-rect reading refractometer and the 0
18、to 30 or 0 to 16 Brix havebeen found satisfactory for use.6.2 Extraction VesselAny suitable vessel of at least 200mL with provisions for isolating a small column of waterextract. Examples are separatory funnels, (glass or plastic), orplastic dropping bottles.6.3 Measuring VesselAny vessel capable of
19、 measuring upto 160 mL of fuel to an accuracy of 62 mL, such as a 250-mLgraduated cylinder, or other calibrated container.6.4 Water Dispenser2.0-mL pipettes are preferred, butsyringes or burettes not exceeding 5.0-mL capacity that candispense 2.0 6 0.2 mL may be used. For the Brix refractome-ter, th
20、e pipette must measure 1.0 6 0.1 mL.6.5 ThermometerThe thermometer must have suitablerange to measure air and fuel temperature in the field. Accurateto 61C and meeting Specification E 1.7. Reagents and Materials.7.1 WaterDistilled or deionized water is preferred for theextraction procedure, but pota
21、ble water may be used.8. Calibration8.1 Calibration of the HB or Brix scale refractometerconsists of setting the reading obtained with water at ambienttemperature to 0.0 with the zero adjustment.8.2 The calibration step is incorporated into the procedure tominimize the effect of temperature changes
22、between the time ofcalibration and measurement. (WarningThe extraction, cali-bration, and measurement steps should be done at ambientconditions. Avoid placing the refractometer on hot or coldsurfaces, in pockets on your person, or other locations thatwould change the temperature of the instrument fr
23、om ambient.When setting zero or making a measurement, take care not toheat or cool the refractometer from ambient.)9. Procedure9.1 Extraction Procedure for the HB Refractometer (Tem-perature Compensated, Direct Reading):9.1.1 Locate the thermometer and refractometer where theywill remain at ambient
24、temperature during the test.9.1.2 Measure 160 mL of fuel to be tested into the extractionvessel.9.1.3 Measure 2.0 mL of water into the extraction vessel.9.2 Extraction Procedure for the Brix Scale Refractometer(Non-Temperature Compensated):9.2.1 Locate the thermometer and refractometer where theywil
25、l remain at ambient temperature during the test.9.2.2 Measure 80 mL of the fuel to be tested into theextraction vessel.9.2.3 Measure 1.0 mL of water into the extraction vessel.9.3 Procedure for the Determination of Fuel System IcingInhibitor:9.3.1 Shake the extraction vessel vigorously for a minimum
26、of 5 min for all fuels.9.3.1.1 Mechanical shakers may be used provided thoroughintermixing of the aqueous and fuel phases occurs, similar tothat obtained by hand shaking. (WarningFollowing theextraction procedures is most critical. Failure to extract for thespecified time or failure to provide vigor
27、ous agitation can resultin false readings. If lower than expected readings are obtained,a second test should be done with a longer extraction time.)9.3.2 Allow the extraction vessel to sit undisturbed atambient temperature for a period of at least 2 min to allow thewater to settle to the bottom. (Wa
28、rningFuel entrained in thewater causes an indistinct refractometer reading. In most casesfuel residue can be eliminated by slowly lowering the refrac-tometer cover. The surface tension of water will sweep fuel offthe prism surface.)9.3.3 Open the cover of the refractometer prism and wipe itclean wit
29、h a tissue. Place several drops of the water used forthe extraction on the prism face.9.3.4 Close the cover and view the scale through theeyepiece. Adjust the focus if necessary to bring the numberedscale into focus. Observe the position of the shadow line on thenumbered scale.9.3.5 Rotate the zero
30、adjustment knob or set screw so thatthe shadow line intersects at 0.0 on the HB or Brix scalerefractometer.9.3.6 Open the prism cover and wipe the surface clean witha tissue.9.3.7 Isolate several drops of the water extract from theextraction vessel and place on the prism face.9.3.7.1 If a separatory
31、 funnel is used, it may be necessary tocollect some extract into a smaller container, and then transferseveral drops to the prism face with a clean eyedropper, syringeor pipette.9.3.7.2 If a dropping bottle is used as an extraction vessel,place it right side up, remove the cap, squeeze slightly, and
32、replace the cap with the bottle under a slight vacuum. Invert thebottle and allow the water extract to settle to the bottom. Uncapthe bottle and squeeze it gently until several drops of extractare collected on a tissue held in the same hand as therefractometer, and then allow several drops of the wa
33、ter extractto fall onto the prism face.9.3.8 Slowly lower the prism cover into place using thesame technique described in 9.3.4. Observe and record theposition of the shadow line.9.3.9 Record the ambient temperature to the nearest degreeCentigrade using a thermometer.9.3.10 Properly dispose of test
34、fluids, wash apparatus withsoap and water, and dry all items. (WarningTreat therefractometer as an optical instrument and avoid damage to thelens and window elements. Store the refractometer in aprotective cover or case.)10. Calculation10.1 For the HB refractometer, report the reading obtainedin 9.3
35、.8 to two significant figures as the final result in volumeD5006032percent DiEGME. If multiple determinations are made, aver-age results falling within the specified repeatability and repro-ducibility tolerances. For rounding off of significant figures,Practice E 29 shall apply.NOTE 2Report the read
36、ing in volume percent from the left hand scalemarked DiEGME or M. The scale is printed on the reticule in the eyepieceof the refractometer.10.2 For the non-temperature compensated refractometerwith Brix scale, first apply the temperature correction factorfrom Table 1. Calculate the volume percent Di
37、EGME asfollows:Vol % FSII 52 3 Temperature Corrected Scale Reading100(1)11. Report11.1 Report the following information:11.1.1 The type of fuel analyzed,11.1.2 The volume percent DiEGME found, and11.1.3 The temperature (C) of the analysis.12. Precision and Bias512.1 The precision of this test method
38、 as determined bystatistical examination of interlaboratory results according toRR: D02-10076is as follows:12.1.1 RepeatabilityThe difference between two test re-sults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould in the long
39、 run, in the normal and correct operation ofthe test method, exceed the following values in only one casein twenty:HB temperature compensated refractometer:repeatability 5 0.009 volume % (2)Brix scale refractometer: repeatability 5 0.005 volume % (3)12.1.2 ReproducibilityThe difference between two s
40、ingleand independent results obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, in normal and correct operation of the testmethod, exceed the following values only in one case intwenty:HB temperature compensated refractometer:reproduc
41、ibility 5 0.018 volume % (4)Brix scale refractometer: reproducibility 5 0.021 volume % (5)NOTE 3Accuracy and precision in the field can be lower than asimilar test done under controlled laboratory conditions using a tempera-ture controlled precision refractometer.12.2 BiasThe HB temperature compensa
42、ted refractometergave results, on average, greater than the true value by 0.0018volume %. The Brix scale refractometer gave results, onaverage, less than the true value by 0.0051 volume %.13. Keywords13.1 aviation fuel; diethylene glycol monomethyl ether; fuelsystem icing inhibitor; refractometry5Su
43、pporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D02-1251.6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D021007.TABLE 1 Temperature Correction Factors for B
44、rix RefractometerReading0 5 10 15 20 25 30 35 40 45 50 55 60 65 7010 0.50 0.54 0.58 0.61 0.64 0.66 0.68 0.70 0.72 0.73 0.74 0.75 0.76 0.78 0.7911 0.46 0.46 0.53 0.55 0.58 0.60 0.62 0.64 0.63 0.66 0.67 0.68 0.64 0.70 0.7112 0.42 0.45 0.48 0.50 0.52 0.54 0.56 0.57 0.58 0.59 0.60 0.61 0.61 0.63 0.6313
45、0.37 0.40 0.42 0.44 0.46 0.48 0.49 0.50 0.51 0.52 0.53 0.54 0.54 0.53 0.5514 Deduct 0.33 0.35 0.37 0.39 0.40 0.41 0.42 0.43 0.44 0.45 0.45 0.46 0.46 0.47 0.4815 from 0.27 0.29 0.31 0.33 0.34 0.34 0.35 0.36 0.37 0.37 0.38 0.39 0.39 0.40 0.4016 reading 0.22 0.24 0.25 0.26 0.27 0.28 0.28 0.29 0.30 0.30
46、 0.30 0.31 0.31 0.32 0.3217 0.17 0.18 0.19 0.20 0.21 0.22 0.21 0.22 0.22 0.23 0.23 0.23 0.23 0.24 0.2418 0.12 0.13 0.13 0.14 0.14 0.14 0.11 0.15 0.15 0.15 0.15 0.16 0.16 0.16 0.1619 0.06 0.06 0.06 0.07 0.07 0.07 0.07 0.08 0.08 0.08 0.08 0.08 0.08 0.08 0.08TemperatureC 20 00000000000000021 0.06 0.07
47、0.07 0.07 0.07 0.08 0.08 0.08 0.08 0.08 0.08 0.08 0.08 0.08 0.0822 0.13 0.13 0.14 0.14 0.15 0.15 0.15 0.15 0.15 0.16 0.16 0.16 0.16 0.16 0.1623 0.19 0.20 0.21 0.22 0.22 0.23 0.23 0.23 0.28 0.24 0.24 0.24 0.24 0.24 0.2424 0.26 0.27 0.28 0.29 0.30 0.30 0.31 0.31 0.31 0.31 0.31 0.32 0.32 0.32 0.3225 Ad
48、d to 0.33 0.35 0.36 0.37 0.38 0.38 0.39 0.39 0.40 0.40 0.40 0.40 0.40 0.40 0.4026 reading 0.40 0.42 0.43 0.44 0.45 0.46 0.47 0.47 0.48 0.48 0.48 0.48 0.48 0.48 0.4827 0.48 0.50 0.52 0.53 0.54 0.55 0.55 0.55 0.55 0.56 0.56 0.56 0.56 0.56 0.5628 0.56 0.57 0.60 0.61 0.62 0.63 0.63 0.63 0.64 0.64 0.64 0
49、.64 0.64 0.64 0.6429 0.64 0.66 0.68 0.69 0.72 0.72 0.72 0.72 0.74 0.73 0.73 0.73 0.73 0.73 0.7330 0.71 0.74 0.77 0.78 0.79 0.80 0.80 0.81 0.81 0.81 0.81 0.81 0.81 0.81 0.81D5006033ASTM 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
