1、Designation: D 4669 07Standard Test Method forPolyurethane Raw Materials: Determination of SpecificGravity of Polyols1This standard is issued under the fixed designation D 4669; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear 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. Scope*1.1 These test methods measure the specific gravity ofpolyols. (See Note 1.)1.2 This standard does not purport to
3、 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.NOTE 1There is no equivalent ISO standard.2. Referen
4、ced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 4052 Test Method for Density and Relative Density ofLiquids by Digital Density MeterE1 Specification for ASTM Liquid-in-Glass ThermometersE 202 Test Methods for Analysis of Ethylene Glycols andPropylene Glycols3. Terminology3.1
5、 DefinitionsFor definitions of terms used in these testmethods see Terminology D 883.3.2 Description of Term Specific to This Standard:3.2.1 specific gravitythe ratio of the weight in air of agiven volume of the material at a stated temperature to theweight in air of an equal volume of water at a st
6、atedtemperature. It shall be expressed as specific gravity, 25/25C,indicating that the sample and reference water were bothmeasured at 25C.4. Significance and Use4.1 These test methods are suitable for quality control, as aspecification test, and for research. It is necessary whenconverting from kin
7、ematic to absolute viscosity.TEST METHOD ASPECIFIC GRAVITY USING APYCNOMETER5. Apparatus5.1 Pycnometer, of 25 or 50-mL capacity, conical shapewith a capillary side arm overflow tube complete with astandard-taper512 ground-glass joint to receive a ground-glassvented cap. A thermometer with a scale gr
8、aduated from 12 to38C in 0.2-degree divisions joins the neck of the flask with astandard-taper1018 ground-glass joint. The thermometer con-tained in the pycnometer shall be calibrated in accordance withSpecification E1.5.2 Water Bath, capable of maintaining a temperature of25.0 6 0.05C during the te
9、st.5.3 Thermometer, an ASTM Low Softening Point Ther-mometer having a range from -2 to +80C and conforming tothe requirements for Thermometer 15C as prescribed inSpecification E1.5.4 Analytical Balance, sensitive to 0.1 mg.6. Reagents6.1 Chromic Acid Cleaning SolutionPrepare a saturatedsolution of c
10、hromic acid (CrO3) in concentrated sulfuric acid(H2SO4, sp gr 1.84).7. Sampling7.1 Polyesters and polyethers usually contain moleculescovering an appreciable range of molecular weights. Thesehave a tendency to fractionate during solidification. Unless thematerial is a finely ground solid it is neces
11、sary to melt (usingno higher temperature than necessary) and mix the resin wellbefore removing a sample for analysis. Since many polyols arehygroscopic, take care to provide minimum exposure toatmospheric moisture during the sampling.1These test methods are under the jurisdiction of ASTM Committee D
12、20 onPlastics and is the direct responsibility of Subcommittee D20.22 on CellularMaterials - Plastics and Elastomers. It was recommended toASTM by the Center forthe Polyurethane Industry of the American Chemistry Council.Current edition approved Nov. 1, 2007. Published November 2007. Originallyappro
13、ved in 1987. Last previous edition approved in 2002 as D 4669 98(2002).2For referenced ASTM standards, 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 AST
14、M website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8. Procedure8.1 Clean the pycnometer by filling it with a chromic acidcleaning solution. Allow it to stand fo
15、r a few hours, empty, andrinse well with distilled water.8.2 Fill the pycnometer with freshly boiled distilled watercooled to 22 to 24C, and set the pycnometer thermometer inplace carefully, avoiding trapping of air. Place the pycnometerin the water bath that has been maintained at 25.0 6 0.05C fora
16、t least 30 min. Wipe the overflow from the side-arm capillaryand cover with the vented cap, remove from the bath, wipe dry,and weigh.8.3 Empty the pycnometer, rinse successively with alcoholand ether, remove the ether vapor, and dry under vacuum for 15min. Weigh the pycnometer and subtract the weigh
17、t of theempty pycnometer from the weight when filled with water inorder to obtain the weight, W, of the contained water at 25Cin air.8.4 The sample for test must be completely liquid. If thesample contains solid polyol, warm the entire sample in theoriginal container until it becomes liquid. Then co
18、ol the sampleto 22 to 24C and quickly fill the pycnometer with it, allowingit minimal exposure to the atmosphere.8.5 Insert the thermometer carefully, avoiding trapping ofair. Cover the side arm with the vented cap, remove from thebath, wipe dry, and weigh. Subtract the weight of the emptypycnometer
19、 from the weight when filled with the sample inorder to obtain the weight, S, of the contained sample at25.0C.9. Calculation9.1 Calculate the specific gravity at 25/25C as follows:S/W 5Specific gravity, 25/25Cwhere:S = sample used, g, andW = water in the pycnometer, g.10. Precision and Bias10.1 Atte
20、mpts to develop a precision and bias statement forthis test method have not been successful. Data on precisionand bias cannot be given for this reason. Anyone wishing toparticipate in the development of precision and bias datashould contact the Chairman, Subcommittee D20.22 (SectionD20.22.01), ASTM
21、100 Barr Harbor Drive, West Consho-hocken, PA 19428-2959.10.2 Test Methods E 202 is similar and does include preci-sion data. Precision statements from Test Methods E 202 arerestated below as an estimate of the precision for this testmethod.10.2.1 RepeatabilityIt has been estimated that duplicateres
22、ults by the same analyst should be considered suspect if theydiffer by 0.0002 units.10.2.2 ReproducibilityIt has been estimated that resultsreported by different laboratories should be considered suspectif they differ by 0.0008 units.10.3 BiasThere are no recognized standards by which toestimate the
23、 bias of this test method.TEST METHOD BSPECIFIC GRAVITY USING ADIGITAL DENSITY METER11. General11.1 A general test method for specific gravity using adigital density meter, which applies to polyols as well as otherliquids is published in Test Method D 4052.12. Keywords12.1 density; polyols; polyuret
24、hane raw materials; specificgravitySUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue(D 4669 98(02) that may impact the use of this standard. (November 1, 2007)(1) Changed the tense of sentences 1.1 and 4.1 to reflectinclusion of a s
25、econd procedure.(2) Added Test Method D 4052 to 2.1 and Section 11.(3) Added a title for “Test Method ASpecific Gravity Usinga Pycnometer.”(4) Added a title for “Test Method BSpecific Gravity Usinga Digital Density Meter.”(5) Updated the reference in Footnote 1.ASTM International takes no position r
26、especting the validity of 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.Thi
27、s standard is subject to 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 Inte
28、rnational Headquarters. 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
29、below.This standard is copyrighted 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 4669 072
