1、Designation: D1480 12D1480 15Standard Test Method forDensity and Relative Density (Specific Gravity) of ViscousMaterials by Bingham Pycnometer1This standard is issued under the fixed designation D1480; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 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. Scope*1.1 This test method covers two procedures for the measurement of the density of materials
3、 which are fluid at the desired testtemperature. Its application is restricted to liquids of vapor pressures below 600 mm Hg (80 kPa) 80 kPa (600 mm Hg) andviscosities below 40 000 cSt (mm40 000 mm2/s) /s (cSt) at the test temperature. The method is designed for use at any temperaturebetween 2020 C
4、and 100C.100 C. It can be used at higher temperatures; however, in this case the precision section does notapply.NOTE 1For the determination of density of materials which are fluid at normal temperatures, see Test Method D1217.1.2 This test method provides a calculation procedure for converting dens
5、ity to specific gravity.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause centralnervous system, kidney and liver dama
6、ge. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional info
7、rmation. Users should be awarethat selling mercury and/or mercury containing products intoin your state or country may be prohibited by law.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard
8、to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham PycnometerD4052 Test Method for Density, R
9、elative Density, and API Gravity of Liquids by Digital Density MeterE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 density, nmass per unit volume at a specified temperature. D40523.1.2 relative density, nthe ratio of the density of a material at a stated te
10、mperature to the density of water at a statedtemperature. D40524. Summary of Test Method4.1 The liquid sample is introduced into the pycnometer, equilibrated to the desired temperature, and weighed. The density orspecific gravity is then calculated from this weight and the previously determined cali
11、bration factor, and a correction is applied forthe buoyancy of air.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.04.0D on Physical and Chemical Methods.Current edition approved
12、 Nov. 1, 2012Dec. 1, 2015. Published December 2012February 2016. Originally approved in 1957. Last previous edition approved in 20072012as D148007.12. DOI: 10.1520/D1480-12.10.1520/D1480-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at servic
13、eastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Be
14、causeit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section app
15、ears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Significance and Use5.1 Density is a fundamental physical property that can be used in conjunction with other properties to characterize both thelight
16、and heavy fractions of petroleum and to assess the quality of crude oils.5.2 Determination of the density or relative density of petroleum and its products is necessary for the conversion of measuredvolumes to volumes at the standard temperatures of 15C.15 C.5.3 The determination of densities at the
17、 elevated temperatures of 4040 C and 100C100 C is particularly useful in providingthe data needed for the conversion of kinematic viscosities in centistokes (mmmm2/s) /s (centistokes) to the corresponding dynamicviscosities in centipoises (mPas).mPas (centipoises).6. Apparatus6.1 Pycnometer,3Bingham
18、-type of 10-mL 10 mL capacity (as shown in Fig. 1), constructed of heat-resistant4 glass.NOTE 2Pycnometers having capacities of 2 mL to 25 mL are available but have not been cooperatively evaluated.6.2 Constant-Temperature Bath, provided with suitable pycnometer holders and means for maintaining tem
19、peratures constantto 60.01C6 0.01 C in the desired range. Water-glycerin mixtures can be used for temperatures up to 100C.100 C.6.3 Bath Thermometer, graduated in 0.1C0.1 C subdivisions and standardized for the range of use to the nearest0.01C0.01 C (ASTM Saybolt Viscosity Thermometers 17C17 C to 22
20、C,22 C, conforming to the requirements in SpecificationE1, are recommended). For most hydrocarbons the density coefficient is about 0.00080.0008 units units/C, and C, and thereforean error of 60.013C6 0.013 C would cause an error of 60.00001 6 0.00001 g/mL in density. A standardized platinumresistan
21、ce thermometer may also be used, and it offers the best means for observing temperature changes in the bath.6.4 Thermal Shields, as shown in Fig. 2, to hold the pycnometer and syringe during the filling procedure, constructed of twoaluminum shells with suitably spaced viewing ports, the upper bored
22、to hold a 30-mL 30 mL hypodermic syringe and the lowerbored to hold a 25-mL 25 mL Bingham pycnometer.Awinding of No. 26 Chromel “A” wire, insulated from the shields with mica,covered with insulating tape, and having resistances connected in series of 25 on the upper shield and 35 on the lowerproduce
23、s controlled heat to the shields by means of a variable transformer. A stand is necessary to support the shields in such amanner that the center of the wells may be aligned, and the upper shield raised 180180 mm to 200 mm and swung through 45.6.5 Hypodermic Syringes, 2 to 30-mL 2 mL to 30 mL capacit
24、y, of chemically resistant glass, equipped with a 170-mm, 16-gage170 mm, 16 gauge (0.065 in.) filling needle made from stainless-steel tubing, as shown in Fig. 3.3 There is more than one supplier. If you cannot find a supplier, then contact Subcommittee D02.04.0D on Physical and Chemical Methods for
25、 possible suppliers.4 Borosilicate glass has been found satisfactory for this purpose.FIG. 1 Bingham-Type PycnometerD1480 1526.6 Draw-off Needle, made of stainless-steel tubing, as shown in Fig. 3.6.7 Solvent Cleaning Assembly, as shown in Fig. 4.6.8 Chromic Acid Cleaning Apparatus, similar to that
26、shown in Fig. 5.6.9 Balance, capable of reproducing weighings within 0.1 mg 0.1 mg when carrying a load of 30 g. 30 g. The balance shall belocated in a room shielded from drafts and fumes and in which the temperature changes between related weighings (empty andfilled pycnometer) do not cause a signi
27、ficant change in the ratio of the balance arms. The same balance shall be used for all relatedweighings.6.10 Weights, whose relative values are known to the nearest 0.05 mg or better. Use the same set of weights for the calibrationof the pycnometer and the determination of densities.7. Reagents and
28、Materials7.1 Acetone(WarningExtremely flammable. Use adequate ventilation.)7.2 Isopentane(WarningExtremely flammable. Avoid build up of vapors and remove all sources of ignition, especiallynon-explosion proof electrical apparatus.)7.3 Chromic Acid (Potassium Dichromate/Conc. Sulfuric Acid)(WarningCa
29、uses severe burns. A recognized carcinogen.Do not get in eyes, on skin, or on clothing.)Metric Equivalentsin. mm in. mm in. mm in. mm18 3.2 58 15.9 114 31.8 4 10214 6.4 34 19.1 1716 36.5 434 121716 11.1 1132 26.2 178 47.6 538 13612 12.7 118 28.6 2 50.8 638 162714 184NOTE 1Cover shields with mica or
30、insulating cement. Wind with No. 26 gagegauge Chromel “A” wire: Upper block 60 in. (1.52 m) (25.4), lowerblock 85 in. (2.16 m) (35.0)1.52 m (60 in.) (25.4 ), lower block 2.16 m (85 in.) (35.0 ) wound vertically. Cover with insulating tape or insulatingcement and connect heaters in series. Insulate s
31、hields from stand with 14-in. in. Transite.FIG. 2 Details of Thermal Shields for 30-mL 30 mL Syringe and 25-mL 25 mL PycnometerD1480 1538. Preparation of Apparatus8.1 Clean the pycnometer thoroughly with hot chromic acid cleaning solution by means of the assembly shown in Fig. 5(WarningSee 7.3.) Chr
32、omic acid solution is the most effective cleansing agent. However, surfactant cleansing fluids have alsobeen used successfully. Mount the apparatus firmly and connect the trap to the vacuum. Warm the necessary amount of cleaningacid in the beaker, place the pycnometer on the ground joint, and evacua
33、te by opening the stopcock to vacuum. Fill the pycnometerwith acid by turning the stop-cock, and either repeat several times, or remove the filled pycnometer and allow it to stand for severalhours at 50 to 60C. at 50 C to 60 C. Remove the acid from the pycnometer by evacuation, empty the acid from t
34、he trap, andflush the pycnometer with distilled water. Clean in this manner whenever the pycnometer is to be calibrated or whenever liquidfails to drain cleanly from the walls of the pycnometer or its capillary. Ordinarily, the pycnometer may be cleaned betweendeterminations by washing with a suitab
35、le solvent, rinsing with pure, dry acetone, followed by isopentane, and vacuum drying.(WarningSee 7.1 and 7.2.)FIG. 3 Accessories for Bingham-Type PycnometerD1480 1548.2 Transfer the pycnometer to the cleaner assembly shown in Fig. 4, with vacuum line and trap attached to the side tube asindicated.
36、Place the pycnometer on the cleaner with the upper hypodermic needle extending upward into the pycnometer, and pressthe edge of the ground joint on the rubber stopper until the vacuum holds it in place. Draw out all the liquid or sample. Immersethe lower end of the hypodermic tube in a suitable solv
37、ent and draw 20 to 25 mL to 25 mL through the pycnometer. Leaving thepycnometer in place, draw air through it until it is dry. Clean the hypodermic syringe with the same apparatus.FIG. 4 Cleaner Assembly for Bingham-Type PycnometerFIG. 5 All-Glass Pycnometer Cleaner Assembly for Use with Hot Chromic
38、 Acid Cleaning SolutionD1480 1559. Calibration of Pycnometers9.1 Weigh the clean, dry pycnometer to 0.1 mg and record the weight.NOTE 3It is convenient to use the lightest of a set of pycnometers as a tare. For best results the treatment and environment of both pycnometer andtare should be identical
39、 for some time prior to weighing.9.2 With a syringe of suitable size, transfer freshly boiled and cooled distilled water to the pycnometer through the filling needle(Note 6). Avoid trapping air bubbles in the bulb or capillary of the pycnometer, removing bubbles, as they form, with the syringe,when
40、possible. Also remove any water above the calibration mark and dry the overflow chamber and capillary with a cotton-fiberpipe cleaner or cotton swab which has been moistened slightly with acetone. Do not touch the plunger of the syringe or hypodermicneedle with fingers as minute quantities of oil tr
41、ansferred this way would cause faulty drainage in the capillary neck of thepycnometer.9.3 Close the pycnometer with the glass stopper and immerse it to a point above the calibration mark in the constant-temperaturebath adjusted to a constancy of 60.01C6 0.01 C at the desired temperature (Note 4). Pe
42、riodically, or before the liquid expandsinto the overflow chamber, remove the stopper, raise the pycnometer sufficiently to expose the calibration mark to view, andreadjust the liquid level to the mark by withdrawing liquid through the steel draw-off needle until expansion has stopped, indicatingtha
43、t the liquid has reached the temperature of the thermostat. To minimize errors caused by faulty drainage, do not allow the liquidto expand more than 10 mm above the calibration mark at any time. Allow the contents to equilibrate an additional 10 min anddraw the level down exactly to the calibration
44、line, avoiding parallax and using a magnifier, if necessary, to obtain good visibility.Remove any liquid adhering to the walls above the calibration mark, with the draw-off needle or pipe cleaner, depending upon thevolatility of the sample. Portions in the overflow bulb can be removed with a cotton
45、swab moistened with acetone.NOTE 4For temperatures above 80C80 C calculate the volume from the coefficient of expansion of the glass observed from calibrations made at60, 70,60 C, 70 C, and 80C.80 C.9.4 Replace the glass stopper, remove the pycnometer from the bath, wash the outside surface with ace
46、tone, and dry thoroughlywith a chemically clean, lint-free, slightly damp cloth. Place the pycnometer in or near the balance case for 20 min 20 min andweigh to the nearest 0.1 mg.NOTE 5In atmospheres of low humidity (60 % or lower), drying the pycnometer by rubbing with a dry cotton cloth will induc
47、e static chargesequivalent to a loss of about 1 mg in the weight of the pycnometer. This charge may not be completely dissipated in less than 30 min. The use of about0.1 mg of radium bromide- or polonium-coated foil in the balance case, or maintaining the relative humidity at 60 percent 60 % or high
48、er, aids in reducingweighing difficulties due to static charges.9.5 Calculate the pycnometer calibration factor, Ft, from the equation:Ft 5density of water at tC!/ (1)weight of water in pycnometer at tC!See Table 2 for the density of water between 00 C and 100C.100 C.TABLE 1 Vacuum Corrections to be
49、 Applied to DensitiesObserved in Air of Various DensitiesNOTE 1Interpolate linearly for intermediate sample densities.NOTE 2For air densities outside this table the vacuum correction shallbe calculated from the equation C = da 1 (FtWt), da being the densityof the air in the balance case in grams per millilitre. See Section 10 of TestMethod D1217 for calculating the air density.ObservedDensityAir Density g/mL0.00116 0.00118 0.00120 0.00122Corrections to be Added0.60 0.00046 0.00047