1、Designation: D4669 07 (Reapproved 2013)1D4669 18Standard Test Method forPolyurethane Raw Materials: Determination of SpecificGravity of Polyols 1This standard is issued under the fixed designation D4669; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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 NOTEReapproved with editorial changes in April 2013.1. Scope*1.1 These test methods measure the
3、 specific gravity of polyols. (See Test Method A measures the specific gravity of polyolsusing a pycnometer and Test Method B lists a reference for measuring the specific gravity of liquids using a density meter thatis applicable to polyols (see Note 1.).1.2 This standard does not purport to address
4、 all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.NOTE 1There is no known ISO equivalent to this standard.1.2 Th
5、is 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 to establish appropriate safety, health, and environmental practices and determine the applicability ofregulatory limitations prior to use.NOTE 1T
6、here is no known ISO equivalent to this standard.1.3 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the
7、World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density MeterE2251 Specification for Liquid-in-Glass ASTM Thermo
8、meters with Low-Hazard Precision LiquidsE202 Test Methods for Analysis of Ethylene Glycols and Propylene Glycols3. Terminology3.1 DefinitionsFor definitions of terms used in these test methods see Terminology D883.3.2 Definitions of Terms Specific to This Standard:3.2.1 specific gravitythe ratio of
9、the weight in air of a given volume of the material at a stated temperature to the weight inair of an equal volume of water at a stated temperature. It shall be expressed as specific gravity, 25/25C, indicating that the sampleand reference water were both measured at 25C.4. Significance and Use4.1 T
10、hese test methods are suitable for quality control, specification testing, and research. The specific gravity is necessary whenconverting kinematic viscosity to absolute viscosity.1 These test methods are under the jurisdiction ofASTM Committee D20 on Plastics and is the direct responsibility of Sub
11、committee D20.22 on Cellular Materials - Plasticsand Elastomers. It was recommended to ASTM by the Center for the Polyurethane Industry of the American Chemistry Council.Current edition approved April 1, 2013April 1, 2018. Published April 2013April 2018. Originally approved in 1987. Last previous ed
12、ition approved in 20072013 asD4669 07.D4669 07(2013)1. DOI: 10.1520/D4669-07R13E01.10.1520/D4669-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Doc
13、ument 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. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM
14、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 appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Bo
15、x C700, West Conshohocken, PA 19428-2959. United States1TEST METHOD ASPECIFIC GRAVITY USING A PYCNOMETER5. Apparatus5.1 Pycnometer, Pycnometer,of 25 or 50-mL capacity, conical shape with a capillary side arm overflow tube complete with astandard-taper 512 ground-glass joint to receive a ground-glass
16、 vented cap. A thermometer with a scale graduated from 12 to 38Cin 0.2-degree divisions joins the neck of the flask with a standard-taper 1018 ground-glass joint. The thermometer contained in thepycnometer shall be calibrated in accordance with Specification E2251.5.2 Water Bath, Water Bath,capable
17、of maintaining a temperature of 25.0 6 0.05C during the test.5.3 Thermometer, Thermometer,anASTM Low Softening Point Thermometer having a range from -2 to +80C and conformingto the requirements for Thermometer S15C as prescribed in Specification E2251.5.4 Analytical Balance, Analytical Balance,sensi
18、tive to 0.1 mg.6. Reagents6.1 Chromic Acid Cleaning SolutionChromic Acid Cleaning SolutionPrepare Prepare a saturated solution of chromic acid(CrO3) in concentrated sulfuric acid (H2SO4, sp gr 1.84).6.2 Acetone, reagent grade7. Sampling7.1 High molecular weight polyester and polyether polyols contai
19、n molecules covering an appreciable range of molecularweights. These have a tendency to fractionate during solidification. Unless the material is a finely ground solid it is necessary tomelt (using no higher temperature than necessary) and mix the polyol well before removing a sample for analysis. S
20、ince manypolyols are hygroscopic, take care to provide minimum exposure to atmospheric moisture during the sampling.8. Procedure8.1 Clean the pycnometer by filling it with a chromic acid cleaning solution.Allow it to stand for a few hours, empty, and rinsewell with distilled water.8.2 Fill the pycno
21、meter with freshly boiled distilled water cooled to 22 to 24C, 23 6 1C, and set the pycnometer thermometerin place carefully, avoiding trapping of air. Place the pycnometer in the water bath that has been maintained at 25.0 6 0.05C forat least 30 min and allow it to equilibrate to 25.0C. Wipe the ov
22、erflow from the side-arm capillary and cover with the vented cap,remove from the bath, wipe dry, and weigh.8.3 Empty the pycnometer, rinse well with acetone and dry under vacuum for 15 min. Weigh the pycnometer and subtract theweight of the empty pycnometer from the weight when filled with water in
23、order to obtain the weight, W, of the contained waterat 25C in air.8.4 The sample for test must be completely liquid. If the sample contains solid polyol, warm the entire sample in the originalcontainer until it becomes liquid. Then cool the sample to 22 to 24C and quickly fill the pycnometer with i
24、t, allowing it minimalexposure to the atmosphere.8.5 Insert the thermometer carefully, avoiding trapping of air. Place the pycnometer in the water bath that has been maintainedat 25.0 6 0.05C for at least 30 min and allow it to equilibrate to 25.0C. Cover the side arm with the vented cap, remove fro
25、mthe bath, wipe dry, and weigh. Subtract the weight of the empty pycnometer from the weight when filled with the sample in orderto obtain the weight, S, of the contained sample at 25.0C.9. Calculation9.1 Calculate the specific gravity at 25/25C as follows:S/W 5Specificgravity,25/25Cwhere:S = sample
26、used, g, andW = water in the pycnometer, g.10. Precision and Bias10.1 Attempts to develop a precision and bias statement for this test method have not been successful. Data on precision andbias cannot be given for this reason. Anyone Because this test method does not contain a round robin-based nume
27、rical precisionand bias statement, it shall not be used as a referee test method in case of dispute. It is recommended that anyone wishing toD4669 182participate in the development of precision and bias data should contact the Chairman, Subcommittee D20.22 (Section D20.22.01),ASTM 100 Barr Harbor Dr
28、ive, West Conshohocken, PA 19428-2959.10.2 Test Methods E202 is similar and does include precision data. Precision statements from Test Methods E202 are restatedbelow as an estimate of the precision for this test method.10.2.1 RepeatabilityPrecision under repeatability conditions.10.2.2 Reproducibil
29、ityPrecision under reproducibility conditions.10.2.3 Repeatability LimitRepeatabilityTheIt has been estimated that duplicate results value below which the absolutedifference between two individual test results obtained under repeatability conditions may be expected to occur with a probabilityof appr
30、oximately 0.95 (95 %). For E202, the maximum expected difference between two test results for the same material, obtainedby the same analyst on different days should be considered suspect if they differ by 0.0002 units based on a 95 % confidenceinterval.operator using the same equipment on the same
31、day in the same laboratory due solely to the method is 0.0002 units.10.2.4 Reproducibility LimitReproducibilityTheIt has been estimated that results reported value below which the absolutedifference between two individual test results obtained under reproducibility conditions may be expected to occu
32、r with aprobability of approximately 0.95 (95 %). For E202by different laboratories should be considered suspect if they differ by 0.0005units based on a 95 % confidence interval., the maximum expected difference between two test results for the same material,obtained by different operators using di
33、fferent equipment in different laboratories due solely to the method is 0.0005 units.10.3 BiasThere are no recognized standards by which to estimate the bias of this test method.TEST METHOD BSPECIFIC GRAVITY USING A DIGITAL DENSITY METER11. General11.1 A general test method for specific gravity usin
34、g a digital density meter, which applies to polyols as well as other liquidsis published in Test Method D4052.12. Keywords12.1 density; polyols; polyurethane raw materials; specific gravitySUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last
35、 issue(D4669 07(2013)1) that may impact the use of this standard. (April 1, 2013)2018)(1) InSubsection 2.1, changed reference fromASTM E1 to E2251 to allow for use of non-mercury thermometers.1.1:Added fullerdescription of scope.(2) InSubsection 4.1, changed grammar to reflect multiple methods and c
36、larify statement.8.2: Restated tolerance for consistency.(3) InSection 5.1, updated reference to ASTM E2251.10: Changed precision and bias statement to comply with D496817.(4) In 5.3, updated thermometer name and reference.(5) In 6.2, added the solvent to the list of reagents.(6) In 7.1, made editor
37、ial changes for clarity.(7) In 8.2, expanded explanation of procedure for clarity.(8) In 8.3, replaced ether and alcohol solvents with acetone.(9) In 8.4, expanded explanation of procedure for clarity.(10) In 10.2.1, expanded statement for clarity.(11) In 10.2.2, corrected a typographical error and
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