1、Designation: D 1837 02a (Reapproved 2007)An American National StandardStandard Test Method forVolatility of Liquefied Petroleum (LP) Gases1This standard is issued under the fixed designation D 1837; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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.1. Scope1.1 This test method is a measure of the relative purity ofthe various types of liquefied pet
3、roleum (LP) gases and helpsto ensure suitable volatility performance. The test results, whenproperly related to vapor pressure and density of the product,can be used to indicate the presence of butane and heaviercomponents in propane type LP-gas, and pentane and heaviercomponents in propane-butane a
4、nd butane type fuels. Thepresence of hydrocarbon compounds less volatile than those ofwhich the LP-gas is primarily composed is indicated by anincrease in the 95 % evaporated temperature.1.2 When the type and concentration of higher boilingcomponents is required, chromatographic analysis should beus
5、ed.1.3 The values stated in SI units 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
6、appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D96 Test Methods for Water and Sediment in Crude Oil byCentrifuge Method (Field Procedure)3D 1796 Test Method forWater and Sediment in Fuel Oils
7、 bythe Centrifuge Method (Laboratory Procedure)E1 Specification for ASTM Liquid-in-Glass Thermometers3. Summary of Test Method3.1 Refrigerate the sample by means of a cooling coil andcollect 100 mL of liquid in a weathering tube. Allow toevaporate (“weather”) at ambient pressure under specifiedcondi
8、tions that approximate a single plate distillation. Correctthe observed temperature, when 5 mL of liquid test portionremains, for barometric pressure and thermometer ice pointerror, and report as the 95 % evaporation temperature.4. Significance and Use4.1 Volatility, expressed in terms of the 95 % e
9、vaporatedtemperature of the product, is a measure of the amount of leastvolatile components present in the product. Coupled with avapor pressure limit, it serves to ensure essentially single-component products in the cases of commercial grades ofpropane and butane. When volatility is coupled with a
10、vaporpressure limit which has been related to density, as in the caseof the commercial PB-mixture, the combination serves toassure essentially two component mixtures for such fuels.When coupled with a proper vapor pressure limit, this mea-surement serves to assure that special-duty propane productsw
11、ill be composed chiefly of propane and propylene and thatpropane will be the major constituent.5. Apparatus5.1 Weathering TubeAcentrifuge tube, cone-shaped, con-forming to the dimensions given in Fig. 1 and made ofthoroughly annealed heat-resistant glass.4The shape of thelower tip of the tube is esp
12、ecially important. The taper shall beuniform and the bottom shall be rounded as shown in Fig. 1.The tubes shall comply in wall thickness to ASTM centrifugetube requirements (Note 1). The graduation tolerances aregiven in Table 1.NOTE 1Requirements for centrifuge tubes appear in Test MethodsD 96 and
13、D 1796.5.2 Tube SupportMeans shall be provided for supportingthe weathering tube by its neck in a vertical position.5.3 Water Bath (for use in tests on butane and propane-butane mixture types of liquefied petroleum gas only). Ashallow container filled with clean water having a maintainedtemperature
14、ranging from 15 to 21C (60 to 70F) and a depthof 38 mm (112 in.).5.4 ThermometerASTM Armored Weathering Test Ther-mometer having a range from 50 to 5C (58 to 41F) andconforming to the requirements for Thermometer 99C921This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Prod
15、ucts and Lubricants and is the direct responsibility of SubcommitteeD02.H0 on Liquefied Petroleum Gas.Current edition approved May 1, 2007. Published June 2007. Originallyapproved in 1961. Last previous edition approved in 2002 as D 1837 02a.2For referenced ASTM standards, visit the ASTM website, ww
16、w.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.3Withdrawn.4Borosilicate glass has been found satisfactory for this purpose.1Copyright ASTM International, 100 Barr Har
17、bor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.(99F86) as prescribed in Specification E1. Do not remove thearmor from the thermometer.5.5 Sampling Precooling Equipment:5.5.1 Cooling VesselAny suitable wide-mouthed metalcontainer or Dewar flask at least 64 mm (212 in.) in ins
18、idediameter by 292 mm (1112 in.) deep.5.5.2 Cooling CoilApproximately 6 m (20 ft) of 4.8-mm(316-in.) outside diameter soft copper tubing, wound around ahollow mandrel at least 54 mm (218 in.) in outside diameter,with adjacent turns touching. Run the lower end of the tube upthrough the center of the
19、mandrel before winding so that thefinished coil will fit snugly inside the cooling vessel. Whenassembled, the top of the coil shall be at least 25 mm (1 in.)below the top of the cooling vessel and the open ends of thecoil shall not be more than 100 mm (4 in.) above. Connect thedownstream end of the
20、coil to a 3.2 mm (18 in.) needle valvehaving an outlet connection not more than 76 mm (3 in.) long(see Fig. 2).5.5.3 PrecoolantThis can be the liquefied petroleum gasfrom the same container from which a sample is to be taken.Other refrigerants having a boiling point lower than the initialboiling poi
21、nt of the sample can be used. Use a nonflammableprecoolant if required.5.6 CharcoalFour grains of activated charcoal, approxi-mately 6 to 14 mesh in size, are required. The four grains shallbe similar in size (Note 2).NOTE 2Grains of charcoal are used as a boiling aid which reduces theNOTEFor gradua
22、tion tolerances see Table 1.FIG. 1 Weathering TubeTABLE 1 Weathering Tube Graduation TolerancesRange, mLScaleDivision, mLLimit ofError, mL0.0 to 0.1 0.05 0.020.1 to 0.3 0.05 0.030.3 to 0.5 0.05 0.050.5 to 1.0 0.1 0.051.0to3.0 0.1 0.13.0to5.0 0.5 0.25.0 to 25.0 1.0 0.525.0 to 100.0 1.0 1.0NOTEThe coi
23、ls in the drawing are extended for clarity.FIG. 2 Precooling EquipmentD 1837 02a (2007)2tendency for the propane or butane to overflow the weathering tube as thepropane or butane evaporates.6. Procedure6.1 Positioning the ThermometerAdd water to the 5 mLline of the weathering tube. Add two grains of
24、 charcoal. Insertthe armored thermometer as low as possible into the weather-ing tube. Observe and record the water level in the tube.Remove and discard the water and charcoal and clean and drythe weathering tube.6.2 Obtaining a Test PortionFill the cooling vessel withthe precoolant so as to cover t
25、he cooling coil. Attach the inletof the cooling coil to the source from which the sample is to betaken with a short line connection of 6.4 mm (14 in.) pipe (orlarger), having a sampling valve large enough to preventvaporization of the material due to the drop in pressure acrossthe valve seat. Purge
26、the sampling line and cooling coil byopening both the sampling valve and the 3.2 mm (18 in.)needle valve on the downstream end of the cooling coil. Fill theweathering tube with the sample flowing through the coolingcoil. Empty this first sample, add two grains of similar-sizedcharcoal as was used in
27、 6.1, and then refill the weathering tubeto the 100-mL mark with fresh liquid sample passing throughthe cooling coil.6.3 Placement of ThermometerCarefully insert the pre-cooled armored thermometer into the centrifuge tube, to thesame position as in 6.1, and center it in the tube by means ofa slotted
28、 cork. Take all 5 % residue readings at the levelestablished in 6.1.NOTE 3Inadequate precooling of the sample will result in excessivevaporization and loss of light components from the sample collected in theweathering tube. This results in proportionally more of the higher boilingcomponents in the
29、sample in order to collect 100 mLof liquid.As a result,the test is made more severe, with a higher reported 95 % evaporationtemperature, which is on the conservative side.6.4 Weathering Butane and Propane-Butane Mixture Typesof Liquefied Petroleum Gas ProductsWhen the temperatureof the sample is bel
30、ow 12C (10F), allow it to weather in theatmosphere until the temperature has reached 12C (10F).Atthis point, place the weathering tube, with the armored ther-mometer still in place, in the water bath in a vertical position,submerging it to the 112-mL mark, and allow the contents toweather.6.5 Weathe
31、ring Propane Type of Liquefied Petroleum GasProductsAllow the sample to weather in the atmosphere,taking care to disturb the frost on the tube as little as possible.An acetone or alcohol swab can be used to remove frostsufficient to permit reading of the temperature.6.6 Reading of TemperatureWhen th
32、e liquid level in theweathering tube, with the armored thermometer still in place,corresponds to the level previously determined in 6.1, read andrecord the temperature of the sample in accordance with 6.4and 6.5.6.7 Temperature CorrectionFollowing the final tempera-ture reading (6.6), remove the arm
33、ored thermometer from theweathering tube and place it in a bath of finely crushed ice upto the immersion point. Observe the reading of the thermom-eter when a constant reading is obtained. If the thermometerreading is less than 0C (32F), add the fraction of a degree itis low to the final test readin
34、g. If the thermometer reading ismore than 0 (32F), subtract the fraction of a degree that it ishigh from the final test reading. If the thermometer readingvaries more than 0.5C (1F), the test result is invalid. Repeatthe procedure using an accurate thermometer.NOTE 4A high reading of the thermometer
35、 when it is placed in iceusually indicates that there is a break in the mercury-thallium thread. Thiscan be corrected by warming the thermometer gently in a warm water bathto drive the break upward into the expansion chamber at the top of thethermometer. While the mercury-thallium is continuous in t
36、he upperchamber, tap the bottom of the thermometer on a hard, but cushionedsurface, to join the liquid into a continuous thread. A low reading in iceusually indicates that some of the liquid has remained in the expansionchamber. To correct this, allow the thermometer to warm so the liquidenters the
37、chamber and tap as previously instructed.7. Interpretation of Results7.1 Correct the thermometer at the 95 % boiling point (5 %residue) for the thermometer error (6.7).7.2 Correct the observed temperature for the thermometererror from the observed atmospheric pressure in kPa (millime-tres of mercury
38、) to a base barometric pressure of 101 kPa (760mm).7.3 In the weathering test for propane, add 0.3C (0.6F) tothe corrected temperature for each 1.3 kPa (10 mm Hg) that thetest is conducted below 101 kPa (760 mm) pressure, or subtract0.3C (0.6F) from the observed temperature for each 1.3 kPa(10 mm Hg
39、) that the test is conducted above 101 kPa (760mm).7.4 In the weathering test for butane and propane-butanemixtures, add 0.4C (0.7F) to the corrected temperature foreach 1.3 kPa (10 mm Hg) that the test is conducted below 101kPa (760 mm) pressure, or subtract 0.4C (0.7F) from theobserved temperature
40、 for each 1.3 kPa (10 mm Hg) that the testis conducted above 101 kPa (760 mm).8. Precision and Bias8.1 The following criteria should be used for judging theacceptability of results (95 % confidence):8.1.1 RepeatabilityThe difference between two test re-sults obtained by the same operator with the sa
41、me apparatusunder constant operating conditions on identical test materialswould in the normal and correct operation of the test method,exceed the following value only in one case in twenty:0.6C 1.0F! (1)8.1.2 ReproducibilityThe difference between two singleand independent results obtained by differ
42、ent operators work-ing in different laboratories on identical test material would inthe long run, in the normal and correct operation of the testmethod, exceed the following value only in one case in twenty:1.0C (1.7F) for butane and propane-butane mixtures and1.3C (2.3F) for propane.8.2 BiasThe pro
43、cedure in this test method for measuringvolatility of LP-gases has no bias because the volatility isdefined only in terms of this test method.9. Keywords9.1 butane; liquefied petroleum (LP) gases; LPG; propane;volatilityD 1837 02a (2007)3ASTM International takes no position respecting the validity o
44、f 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
45、 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.
46、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 c
47、opyrighted 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).D 1837 02a (2007)4
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