1、Designation: D1817 05 (Reapproved 2016)Standard Test Method forRubber ChemicalsDensity1This standard is issued under the fixed designation D1817; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i
2、n parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the densityof solid chemicals used as rubber additives during processingand manufacture. It is int
3、ended for determining the density ofthe rubber chemical itself and not for the determination of theeffective density of the chemical in a rubber.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 purp
4、ort 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. Referenced Documents2.1 ASTM Standards:2E1
5、Specification for ASTM Liquid-in-Glass ThermometersE300 Practice for Sampling Industrial Chemicals3. Summary of Test Method3.1 The density of the test specimen is obtained via wetpycnometry.4. Significance and Use4.1 The density of a rubber chemical is used for calculatingthe rubber compound volume,
6、 which is used to determine thecost of a rubber product. The density may also be used as a rawmaterial control tool.5. Apparatus5.1 Pycnometer, 50-cm3capacity.NOTE 1The weld type with the cap seal on the outside of the neck ofthe bottle is preferred because there is less danger of trapping air justu
7、nder the capillary tube than with types having the ground seal on theinside of the neck. The stopper may contain a thermometer. However, thecontrol of the temperature is through the adjustment of the water bathrather than by this thermometer.5.2 Water Bath, maintained at 23 6 0.5C and equippedwith a
8、 stirring device.5.3 Pressure MeterA gage or manometer that is accurateto 0.2 kPa, is required to measure the differential pressurebetween the outside and inside of the system.5.3.1 Alternatively, a device for measuring the absolutepressure inside the system can be used. The range of themeasuring de
9、vice should be at least 100 kPa for differentialpressure meters and at least 10 kPa for absolute pressuremeters.5.4 DesiccatorA glass desiccator constructed with heavywalls to withstand a differential pressure of 100 kPa and withan opening at the side or top. The desiccator should be enclosedin a st
10、urdy box or shield to prevent possible injury to theoperator.5.5 Vacuum PumpAn oil-filled, motor-driven pump, ca-pable of reducing the absolute pressure of the system to 2 kPa.5.6 Thermometer, having a minimum range from 10 to 30Cand graduated in 0.1C divisions. ASTM Solidification PointThermometer
11、having a range from 0 to 30C and conformingto the requirements for Thermometer 90C as prescribed inSpecification E1, may be used.5.7 Weighing BottleA wide-mouth, cylindrical, glassweighing bottle (about 30 mm in height and 70 mm indiameter) provided with a ground-glass stopper.6. Sampling6.1 Select
12、a representative sample of the chemical to betested in accordance with the appropriate section of PracticeE300.6.2 Mesh SizeRubber chemicals are generally in the formof powders that require no further treatment. Grind any lumps,pellets, and so forth, to pass a 149-m sieve prior to thedetermination.6
13、.3 DryingIt is not necessary to dry rubber chemicals,unless it is known that they contain sufficient water to interferewith an accurate density measurement. If necessary, dry toconstant mass at least 10C below the melting pointing but notabove 110C.1This test method is under the jurisdiction of ASTM
14、 Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved June 1, 2016. Published June 2016. Originallyapproved in 1961. Last previous edition approved in 2011 as D1817 05 (2011).DOI: 10.1520/D1817-05R16.2For referenced ASTM standar
15、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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1
16、9428-2959. United States17. Immersion Liquid7.1 An immersion liquid should be chosen in which noportion of the rubber chemical (major component, impurity, oradded component) is soluble and which will not react with anyportion of the rubber chemical. Refined white kerosene ofnarrow boiling range and
17、low evaporation rate may sometimesbe used. Other immersion liquids such as ethylene glycol,tetrahydronaphthalene, and so forth, may be suitable. If animmersion liquid cannot be found that meets these solubilityrequirements, an immersion liquid saturated with the solublecomponents of the sample shall
18、 be used.8. Standardization of Pycnometer8.1 Fill the pycnometer with freshly boiled distilled water at20 to 22C; gradually bring to 23 6 0.5C in the water bath,and then remove, dry, and weigh it as described in 9.1. Emptythe pycnometer, then clean, dry, and reweigh it. Next, fill thepycnometer with
19、 the immersion liquid at 22C or less, andbring to 23 6 0.5C in the water bath. Remove from the bath,dry, and weigh as before. Calculate the density of the immer-sion liquid as follows:Density at 23C, Mg/m35 A/B! 30.997 (1)where:A = mass of immersion liquid, andB = mass of water,0.9976 = density of w
20、ater at 23C, Mg/m3.9. Procedure9.1 WeighingTransfer a sufficient amount of the testspecimen to a clean, dry, weighed pycnometer to form a layerapproximately 19 mm (34 in.) deep and reweigh. Weigh rubberchemicals of a hygroscopic nature from a weighing bottle.9.2 Addition of Immersion LiquidAdd suffi
21、cient immer-sion liquid to the pycnometer to form a thin layer above therubber chemical. When necessary, swirl the contents of thepycnometer by hand, to wet the sample.9.3 Removal of Occluded AirPlace the pycnometer in thedesiccator, close, and attach to the pump for the removal of air.Take care not
22、 to decrease the pressure too quickly, otherwisesome of the sample may be lost due to the sudden removal ofthe entrapped air. A pinch-cock may be used to control the rateof evacuation. The pressure meter is used to indicate whetherthe oil pump is giving the proper vacuum, which is an absolutepressur
23、e of 0.2 kPa. Bubbles of air rise from the sample rapidlyat first, then decrease and finally stop. The time required forcomplete removal of air may vary from 30 min to 24 h. Whenno more bubbles can be seen, it may be assumed that occludedair has been removed and the rubber chemical is thoroughlywet
24、with immersion liquid. Slowly readmit air to the desicca-tor.NOTE 2If an immersion liquid is used whose vapor pressure is greaterthan 0.2 kPa at room temperature, the liquid will evaporate, often with“bumping.” Therefore it is necessary to adjust the vacuum to a higherpressure with some loss in effe
25、ctiveness of air removal. The use of suchimmersion liquids should be limited to those cases in which no low vaporpressure liquid can be used. In no case should a mixed liquid be used inwhich any component has an appreciable vapor pressure.9.4 Final AdjustmentRemove the pycnometer from thedesiccator,
26、 fill with immersion liquid at 22C or less, takingcare to add a sufficient quantity to prevent air bubbles remain-ing in the pycnometer when closed. Insert the stopper, beingcareful not to trap any air bubbles. Place the pycnometer in thewater bath and permit it to come to constant temperature at 23
27、6 0.5C. Remove from the water bath, wipe the end of thecapillary with lint-free toweling or lens paper, making sure notto suck any liquid from the capillary. Cap the capillary. Dip thepycnometer (up to the side arm) in a beaker of alcohol toremove any residual immersion liquid. Thoroughly dry theout
28、side of the pycnometer and weigh.9.5 Number of SpecimensMake duplicate tests on allspecimens.10. Calculation10.1 Calculate the density of the rubber chemical as fol-lows:Density at 23C, Mg/m35 PS/P1K! 2 F# (2)where:P = mass of rubber chemical used,S = density of the immersion liquid,K = mass of the
29、pycnometer filled with immersion liquid,andF = final mass of the pycnometer with rubber chemical andimmersion liquid.11. Report11.1 Report the following information:11.1.1 Sample identification11.1.2 Density at 23C, Mg/m3, and11.1.3 Immersion liquid used.12. Precision and Bias12.1 PrecisionThis test
30、 method has not been tested forreproducibility or repeatability, but duplicate determinations onthe same sample should not differ by more than 0.02 Mg/m3at23C.12.2 BiasNo statement about bias is being made at thistime.13. Keywords13.1 density; rubber chemicalsD1817 05 (2016)2ASTM International takes
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