1、Designation: D4669 07 (Reapproved 2013)1Standard Test Method forPolyurethane Raw Materials: Determination of SpecificGravity of Polyols1This standard is issued under the fixed designation D4669; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f 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.1NOTEReapproved with editorial changes in April 2013.1. Scope*1.1 These test methods measure the specific
3、gravity ofpolyols. (See Note 1.)1.2 This standard does not purport 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 limitati
4、ons prior to use.NOTE 1There is no known ISO equivalent to this standard.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD4052 Test Method for Density, Relative Density, and APIGravity of Liquids by Digital Density MeterE2251 Specification for Liquid-in-Glass ASTM The
5、rmom-eters with Low-Hazard Precision LiquidsE202 Test Methods for Analysis of Ethylene Glycols andPropylene Glycols3. Terminology3.1 DefinitionsFor definitions of terms used in these testmethods see Terminology D883.3.2 Definitions of Terms Specific to This Standard:3.2.1 specific gravitythe ratio o
6、f 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 statedtemperature. 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 Th
7、ese test methods are suitable for quality control,specification testing, and research. The specific gravity isnecessary when converting kinematic viscosity to absoluteviscosity.TEST METHOD ASPECIFIC GRAVITY USING APYCNOMETER5. Apparatus5.1 Pycnometer, of 25 or 50-mL capacity, conical shapewith a cap
8、illary side arm overflow tube complete with astandard-taper512 ground-glass joint to receive a ground-glassvented cap. A thermometer with a scale graduated 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
9、 pycnometer shall be calibrated in accordance withSpecification E2251.5.2 Water Bath, capable of maintaining a temperature of25.0 6 0.05C during the test.5.3 Thermometer, an ASTM Low Softening Point Ther-mometer having a range from -2 to +80C and conforming tothe requirements for Thermometer S15C as
10、 prescribed inSpecification E2251.5.4 Analytical Balance, sensitive to 0.1 mg.6. Reagents6.1 Chromic Acid Cleaning Solution Prepare a saturatedsolution 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
11、 polyether polyolscontain molecules covering an appreciable range of molecularweights. These have a tendency to fractionate during solidifi-cation. Unless the material is a finely ground solid it isnecessary to melt (using no higher temperature than necessary)and mix the polyol well before removing
12、a sample for analysis.1These test methods are under the jurisdiction of ASTM Committee D20 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
13、 Council.Current edition approved April 1, 2013. Published April 2013. Originallyapproved in 1987. Last previous edition approved in 2007 as D4669 07. DOI:10.1520/D4669-07R13E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.
14、For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Sinc
15、e many polyols are hygroscopic, take care to provideminimum exposure to atmospheric moisture during the sam-pling.8. Procedure8.1 Clean the pycnometer by filling it with a chromic acidcleaning solution. Allow it to stand for a few hours, empty, andrinse well with distilled water.8.2 Fill the pycnome
16、ter 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 forat least 30 min and allow it to equilibrate to 25.0C. Wipe theoverflow from th
17、e side-arm capillary and cover with the ventedcap, remove from the bath, wipe dry, and weigh.8.3 Empty the pycnometer, rinse well with acetone and dryunder vacuum for 15 min. Weigh the pycnometer and subtractthe weight of the empty pycnometer from the weight whenfilled with water in order to obtain
18、the weight, W, of thecontained water at 25C in 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 cool the sampleto 22 to 24C and quickly fill the pycnometer with it, allowingit mini
19、mal exposure to the atmosphere.8.5 Insert the thermometer carefully, avoiding trapping ofair. Place the pycnometer in the water bath that has beenmaintained at 25.0 6 0.05C for at least 30 min and allow it toequilibrate to 25.0C. Cover the side arm with the vented cap,remove from the bath, wipe dry,
20、 and weigh. Subtract theweight of the empty pycnometer from the weight when filledwith the sample in order to obtain the weight, S, of thecontained sample at 25.0C.9. Calculation9.1 Calculate the specific gravity at 25/25C as follows:S/W 5 Specificgravity, 25/25Cwhere:S = sample used, g, andW = wate
21、r in the pycnometer, g.10. Precision and Bias10.1 Attempts 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 C
22、hairman, Subcommittee D20.22 (SectionD20.22.01), ASTM 100 Barr Harbor Drive, WestConshohocken, PA 19428-2959.10.2 Test Methods E202 is similar and does include preci-sion data. Precision statements from Test Methods E202 arerestated below as an estimate of the precision for this testmethod.10.2.1 Re
23、peatabilityIt has been estimated that duplicateresults by the same analyst on different days should beconsidered suspect if they differ by 0.0002 units based on a 95% confidence interval.10.2.2 ReproducibilityIt has been estimated that resultsreported by different laboratories should be considered s
24、uspectif they differ by 0.0005 units based on a 95 % confidenceinterval.10.3 BiasThere are no recognized standards by which toestimate the bias of this test method.TEST METHOD BSPECIFIC GRAVITY USING ADIGITAL DENSITY METER11. General11.1 A general test method for specific gravity using adigital dens
25、ity meter, which applies to polyols as well as otherliquids is published in Test Method D4052.12. Keywords12.1 density; polyols; polyurethane raw materials; specificgravitySUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue(D4669 07)
26、that may impact the use of this standard. (April 1, 2013)(1) In 2.1, changed reference fromASTM E1 to E2251 to allowfor use of non-mercury thermometers.(2) In 4.1, changed grammar to reflect multiple methods andclarify statement.(3) In 5.1, updated reference to ASTM E2251.(4) In 5.3, updated thermom
27、eter name and reference.(5) In 6.2, added the solvent to the list of reagents.(6) In 7.1, made editorial 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 clarit
28、y.(10) In 10.2.1, expanded statement for clarity.(11) In 10.2.2, corrected a typographical error and expandedstatement for clarity.D4669 07 (2013)12ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
29、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.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every fi
30、ve 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 International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
31、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 below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
32、A 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D4669 07 (2013)13
