ASTM D1817 – 96

Designation: D 1817 – 96 Standard Test Method for Rubber Chemicals—Density1 This standard is issued under the fixed designation D 1817; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the density of solid chemicals used as rubber additives during processing and manufacture. It is intended for determining the density of the rubber chemical itself and not for the determination of the effective density of the chemical in a rubber. 1.2 The values stated in SI units shall be regarded as standard. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility 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 Documents 2.1 ASTM Standards: E 1 Specification for ASTM Thermometers2 E 300 Practice for Sampling Industrial Chemicals3 3. Summary of Test Method 3.1 The density of the test specimen is obtained via wet pycnometry. 4. Significance and Use 4.1 The density of a rubber chemical is used for calculating the rubber compound volume, which is used to determine the cost of a rubber product. The density may also be used as a raw material control tool. 5. Apparatus 5.1 Pycnometer, 50-cm3 capacity. NOTE 1—The weld type with the cap seal on the outside of the neck of the bottle is preferred because there is less danger of trapping air just under the capillary tube than with types having the ground seal on the inside of the neck. The stopper may contain a thermometer. However, the control of the temperature is through the adjustment of the water bath rather than by this thermometer. 5.2 Water Bath, maintained at 25 6 0.5°C and equipped with a stirring device. 5.3 Pressure Meter—A gage or manometer that is accurate to 0.2 kPa, is required to measure the differential pressure between the outside and inside of the system. 5.3.1 Alternatively, a device for measuring the absolute pressure inside the system can be used. The range of the measuring device should be at least 100 kPa for differential pressure meters and at least 10 kPa for absolute pressure meters. 5.4 Desiccator—A glass desiccator constructed with heavy walls to withstand a differential pressure of 100 kPa and with an opening at the side or top. The desiccator should be enclosed in a sturdy box or shield to prevent possible injury to the operator. 5.5 Vacuum Pump—An 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 30°C and graduated in 0.1°C divisions. ASTM Solidification Point Thermometer having a range from 0 to 30°C and conforming to the requirements for Thermometer 90C as prescribed in Specification E 1, may be used. 5.7 Weighing Bottle—A wide-mouth, cylindrical, glass weighing bottle (about 30 mm in height and 70 mm in diameter) provided with a ground-glass stopper. 6. Sampling 6.1 Select a representative sample of the chemical to be tested in accordance with the appropriate section of Practice E 300. 6.2 Mesh Size—Rubber chemicals are generally in the form of powders that require no further treatment. Grind any lumps, pellets, etc., to pass a 149-µm sieve prior to the determination. 6.3 Drying—It is not necessary to dry rubber chemicals, unless it is known that they contain sufficient water to interfere with an accurate density measurement. If necessary, dry to constant mass at least 10°C below the melting pointing but not above 110°C. 7. Immersion Liquid 7.1 An immersion liquid should be chosen in which no portion of the rubber chemical (major component, impurity, or added component) is soluble and which will not react with any portion of the rubber chemical. Refined white kerosene of narrow boiling range and low evaporation rate may sometimes be used. Other immersion liquids such as ethylene glycol, tetrahydronaphthalene, etc., may be suitable. If an immersion liquid cannot be found that meets these solubility requirements, 1 This test method is under the jurisdiction of ASTM Committee D-11 on Rubber and is the direct responsibility of Subcommittee D11.11 on Chemical Analysis. Current edition approved Jan. 10, 1996. Published February 1996. Originally published as D 1817 – 61 T. Last previous edition D 1817 – 90 (1995)e1. 2 Annual Book of ASTM Standards, Vol 14.03. 3 Annual Book of ASTM Standards, Vol 15.05. 1 AMERICAN SOCIETY FOR TESTING AND MATERIALS 100 Barr Harbor Dr., West Conshohocken, PA 19428 Reprinted from the Annual Book of ASTM Standards. Copyright ASTM NOTICE:¬This¬standard¬has¬either¬been¬superseded¬and¬replaced¬by¬a¬new¬version¬or discontinued.¬Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information. an immersion liquid saturated with the soluble components of the sample shall be used. 8. Standardization of Pycnometer 8.1 Fill the pycnometer with freshly boiled distilled water at 23 to 24°C; gradually bring to 25 6 0.5°C in the water bath, and then remove, dry, and weigh it as described in 9.1. Empty the pycnometer, then clean, dry, and reweigh it. Next, fill the pycnometer with the immersion liquid at 24°C or less, and bring to 25 6 0.5°C in the water bath. Remove from the bath, dry, and weigh as before. Calculate the density of the immersion liquid as follows: Density at 25°C, Mg/m3 5 ~A/B! 3 0.997 (1) where: A 5 mass of immersion liquid, and B 5 mass of water, 0.997 5 density of water at 25°C, Mg/m3. 9. Procedure 9.1 Weighing—Transfer a sufficient amount of the test specimen to a clean, dry, weighed pycnometer to form a layer approximately 19 mm (3⁄4in.) deep and reweigh. Weigh rubber chemicals of a hygroscopic nature from a weighing bottle. 9.2 Addition of Immersion Liquid—Add sufficient immersion liquid to the pycnometer to form a thin layer above the rubber chemical. When necessary, swirl the contents of the pycnometer by hand, to wet the sample. 9.3 Removal of Occluded Air—Place the pycnometer in the desiccator, close, and attach to the pump for the removal of air. Take care not to decrease the pressure too quickly, otherwise some of the sample may be lost due to the sudden removal of the entrapped air. A pinch-cock may be used to control the rate of evacuation. The pressure meter is used to indicate whether the oil pump is giving the proper vacuum, which is an absolute pressure of 0.2 kPa. Bubbles of air rise from the sample rapidly at first, then decrease and finally stop. The time required for complete removal of air may vary from 30 min to 24 h. When no more bubbles can be seen, it may be assumed that occluded air has been removed and the rubber chemical is thoroughly wet with immersion liquid. Slowly readmit air to the desiccator. NOTE 2—If an immersion liquid is used whose vapor pressure is greater than 0.2 kPa at room temperature, the liquid will evaporate, often with“ bumping.” Therefore it is necessary to adjust the vacuum to a higher pressure with some loss in effectiveness of air removal. The use of such immersion liquids should be limited to those cases in which no low vapor pressure liquid can be used. In no case should a mixed liquid be used in which any component has an appreciable vapor pressure. 9.4 Final Adjustment—Remove the pycnometer from the desiccator, fill with immersion liquid at 24°C or less, taking care to add a sufficient quantity to prevent air bubbles remaining in the pycnometer when closed. Insert the stopper, being careful not to trap any air bubbles. Place the pycnometer in the water bath and permit it to come to constant temperature at 25 6 0.5°C. Remove from the water bath, wipe the end of the capillary with lint-free toweling or lens paper, making sure not to suck any liquid from the capillary. Cap the capillary. Dip the pycnometer (up to the side arm) in a beaker of alcohol to remove any residual immersion liquid. Thoroughly dry the outside of the pycnometer and weigh. 9.5 Number of Specimens—Make duplicate tests on all specimens. 10. Calculation 10.1 Calculate the density of the rubber chemical as follows: Density at 25°C, Mg/m3 5 PS/@~P 1 K! 2 F# (2) where: P 5 mass of rubber chemical used, S 5 density of the immersion liquid, K 5 mass of the pycnometer filled with immersion liquid, and F 5 final mass of the pycnometer with rubber chemical and immersion liquid. 11. Report 11.1 Report the following information: 11.1.1 Name of the rubber chemical, 11.1.2 Density at 25°C, Mg/m3, and 11.1.3 Immersion liquid used. 12. Precision and Bias 12.1 Precision—This test method has not been tested for reproducibility or repeatability, but duplicate determinations on the same sample should not differ by more than 0.02 Mg/m3 at 25°C. 12.2 Bias—No statement about bias is being made at this time. 13. Keywords 13.1 density; rubber chemicals The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of 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 and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428. 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