ASTM D1755-1992(2001) Standard Specification for Poly(Vinyl Chloride) Resins《聚氯乙烯树脂标准规范》.pdf

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1、Designation: D 1755 92 (Reapproved 2001)Standard Specification forPoly(Vinyl Chloride) Resins1This standard is issued under the fixed designation D 1755; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A

2、number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification covers the establishment of require-ments for homopolymers of vinyl chloride in original powderform intended for su

3、bsequent mixing and processing in ther-moplastic compositions. These resins have a nominal specificgravity of 1.4 and a theoretical chlorine content of 56.8 %.1.2 Two types of resin have been recognized: generalpurpose and dispersion. When mixed with the customaryamount of plasticizer, general-purpo

4、se resins yield a dry ormoist powder while dispersion resins yield a liquid slurry.Since many resins are polymerized to meet special require-ments, a system of classification has been provided that permitsa wide choice of grades.21.3 The values stated in SI units are to be regarded as thestandard.NO

5、TE 1This standard is similar in content (but not technicallyequivalent) to ISO 1264 1980.31.4 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practic

6、es and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 281 Test Method for Oil Absorption of Pigments bySpatula Rub-Out4D 495 Test Method for High-Voltage, Low-Current, DryArc Resistance of Solid Electrical Insulation5, 6D 883 Terminolo

7、gy Relating to Plastics6D 1125 Test Methods for Electrical Conductivity and Re-sistivity of Water7D 1243 Test Method for Dilute Solution Viscosity of VinylChloride Polymers6D 1249 Specification for Octyl Ortho-Phthalate Ester Plas-ticizers6D 1600 Terminology for Abbreviated Terms Relating toPlastics

8、6D 1705 Test Method for Particle SizeAnalysis of PowderedPolymers and Copolymers of Vinyl Chloride6D 1755 Specification for Poly(Vinyl Chloride) Resins6D 1823 Test Method for Apparent Viscosity of Plastisolsand Organosols at High Shear Rates by Extrusion Viscom-eter6D 1824 Test Method for Apparent V

9、iscosity of Plastisolsand Organosols at Low Shear Rates by Brookfield Vis-cometer6D 1895 Test Methods for Apparent Density, Bulk Factor,and Pourability of Plastic Materials6D 1898 Practice for Sampling of Plastics6D 1921 Test Method for Particle Size (Sieve Analysis) ofPlastic Materials6D 2132 Test

10、Method for Dust-and-Fog Tracking and Ero-sion Resistance of Electrical Insulating Materials5D 2396 Test Method for Powder-Mix Test of Poly(VinylChloride) (PVC) Resins Using a Torque Rheometer8D 2873 Test Method for Interior Porosity of Poly(VinylChloride) (PVC) Resins by Mercury Intrusion Porosim-et

11、ry8D 3030 Test Method for Volatile Matter (Including Water)of Vinyl Chloride Resins8D 3892 Practice for Packaging/Packing of Plastics8E1 Specifications for ASTM Thermometers93. Terminology3.1 DefinitionsDefinitions are in accordance with Termi-nology D 883 and Terminology D 1600, unless otherwiseind

12、icated.1This specification is under the jurisdiction of ASTM Committee D20 onPlastics and is the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials (Section D20.15.07).Current edition approved June 15, 1992. Published August 1992. Originallypublished as D1755 60 T. Last previous

13、edition D1755 81 (1987).2Hutson, J. L., “Proposed Method for Classifying Poly(Vinyl Chloride) Resins.”ASTM Research Report File No. RR: D-20-1: (May 20, 1959). Available fromASTM Headquarters.3Available from American National Standards Institute, 11 W. 42nd St., 13thFloor, New York, NY 10036.4Annual

14、 Book of ASTM Standards, Vol 06.02.5Annual Book of ASTM Standards, Vol 10.02.6Annual Book of ASTM Standards, Vol 08.01.7Annual Book of ASTM Standards, Vol 11.01.8Annual Book of ASTM Standards, Vol 08.02.9Annual Book of ASTM Standards, Vol 14.03.1Copyright ASTM International, 100 Barr Harbor Drive, P

15、O Box C700, West Conshohocken, PA 19428-2959, United States.4. Classification4.1 TypesThis specification covers two types of resin:4.1.1 Type GPGeneral-purpose resins primarily intendedfor either dry blending, preblending, or thermoplastic process-ing.4.1.2 Type DDispersion resins primarily intended

16、 for usein organosols and plastisols. As a class, these are small inparticle size.4.2 GradesThis specification provides for as many gradesof resin as may be selected from the possible combinations ofrequirements in Table 1 and Table 2. A grade is designated byfirst indicating the type (GP or D), fol

17、lowed by cell numbersfor each property in the order in which they are listed in Table1 and Table 2. Where there is no interest in a property, a “0” isentered in place of a cell number. Should it be desirable, a celllimit may be extended by half the cell range into the nexthigher or lower cell, but n

18、ot both. When this is done, it isindicated by a dash above the cell number ( n) if the extensionis into the higher cell, or a dash below (n) if into the lower cell.Extension of cell limits applies only to cells where ranges ofproperties are allowed and not where maximum or minimumvalues are specifie

19、d. The cell number of the first property(dilute solution viscosity) is separated from those that followby a dash.TABLE 1 Type GP, General-Purpose Resin RequirementsDesig-nationOrderNo.PropertyCell Limits01 2 3 4 5 6 7 8 91 Dilute solution(inherent)viscosityunspec-fied1993 Severs viscosity,poiseunspe

20、cified 0 to 49 50 to 99 100 to 149 150 to 199 200 to 299 300 to 499 500 to 999 1000 to 1499 1499TABLE 3 Requirements of Resin GP6-43054DesignationOrder No.Property UnitRequirementCell Codemin max1 Inherent viscosity 1.10 1.19 62 Sieve analysis percent through No. 200(75-m) sieve30 44(39 + 10/2)43 Ap

21、parent (bulk) density g/1000 cm3(lb/ft3) 233(14.51)328(20.50)34 Plasticizer sorption parts DOP phrAnone 05 Dry flow s/400 cm33.0(4.02.0/2)5.9 56 Conductivity S/cmg . $64Aphr = per 100 parts of resin.D 1755 92 (2001)2NOTE 2Resin GP643054. This is a grade of general-purpose resin(see Table 1) having t

22、he requirements given in Table 3.10Standard valuesdefined by round-robin testing of eight laboratories are listed in Table 4.5. General Requirements5.1 The resin shall be in powder form.5.2 The resin shall conform to the requirements of Table 1or Table 2, as specified by the type and grade designati

23、onagreed upon between the purchaser and the supplier.NOTE 3Properties not covered, such as heat stability, color, andvolatile loss, may also be important for application performance incompounds.6. Sampling6.1 Unless otherwise agreed upon between the purchaserand the supplier, the material shall be s

24、ampled in accordancewith the sampling procedure in Practice D 1898.7. Number of Tests7.1 One set of test specimens as prescribed in the Sectionson General and Specific Sampling Procedures of PracticeD 1898 shall be considered sufficient for testing each batch.8. Retest and Rejection8.1 If any failur

25、e occurs, the materials may be retested toestablish conformity in accordance with an agreement betweenthe purchaser and the supplier.TEST METHODS9. Dilute Solution Viscosity9.1 Test Method D 1243.10. Apparent (Bulk) Density10.1 Test Methods D 1895.11. Sieve Analysis11.1 Test Method D 1921.NOTE 4Test

26、 Method D 1705 may be substituted at the option of thepurchaser and the supplier.NOTE 5Specifications for sieve analysis (Table 1) are primarilyintended to control fines.12. Brookfield Viscosity12.1 Test Method D 1824. Take readings using a BrookfieldRVF viscometer at 20 r/min with a No. 6 spindle.

27、Prepare theplastisol sample as follows:12.1.1 PlasticizerDi (2-ethylhexyl) phthalate (DOP),Type I in Specification D 1249.12.1.2 Apparatus:12.1.2.1 Mixer, planetary-gear type, equipped with flatbeater mixing paddle.1112.1.2.2 Vacuum Desiccator, capable of being evacuated to133 Pa (1 mm Hg).12.1.3 Pr

28、ocedure:12.1.3.1 Condition the mixing bowl and materials to 2361C. Weigh 500 6 0.5 g of resin into the mixing bowl. Weigh300 6 0.5 g of plasticizer and add it directly on top of the resinin the mixing bowl. Hand mix with the flat beater for 1 min.12.1.3.2 Mount the bowl on the mixer and mix for 5 mi

29、n atthe No. 1 speed. Stop the mixer and scrape down the sides ofthe bowl and the beater. Resume mixing at the No. 2 speed foran additional 15 min. Note and record the temperature of theplastisol immediately after mixing. The temperature rise mustnot exceed 5C. Use a cooling bath if necessary.12.1.3.

30、3 Place the mixing bowl in the desiccator, evacuateto 133 Pa (1 mm Hg), and allow it to remain in the desiccatorfor an additional 10 min after the foam collapses. Consider thetime in the desiccator as part of the normal aging period. Takecare to ensure that the plastisol does not overflow the contai

31、nerduring evacuation.13. Severs Viscosity13.1 Test Method D 1823. Determinations shall be madethrough a 3.17 6 0.13-mm (0.125 6 0.005-in.) diameter orificeat a gas pressure of 0.69 MPa (100 psi). The plastisol sampleshall be prepared in accordance with 12.1.1-12.1.3.14. Electrical Conductivity of Wa

32、ter Extract14.1 DefinitionsSee the Definitions Section of Test Meth-ods D 1125.14.2 Summary of Test MethodThis test is intended todistinguish between electrical and nonelectrical grades ofunprocessed resin. In general, the test will not detect relativelysmall differences among different lots of elec

33、trical grade resin.Awater dispersion of the resin is boiled for a short time and theelectrical conductivity of the solution measured. The conduc-tivity of the water extract results from ionic impurities in theresin that adversely affect its use for electrical insulation.12Electrical grade resins gen

34、erally yield conductivity values lessthan 6 S/cmg.14.3 Apparatus:10ASTM General Purpose PVC Reference Standard is available from B. F.Goodrich Chemical Co., Manufacturing Services Laboratory, P.O. Box 134, AvonLake, OH 44012.11A Hobart Model N-50, manufactured by the Hobart Manufacturing Co., Troy,O

35、H, has been found satisfactory for this purpose.12DeCoste, J. B., and Siratelli, B. A., “Characterization of PVC Resins by theConductivity of Solvent Extract,” Rubber Age, Vol 87, pp. 279285.TABLE 4 ASTM PVC Reference Standard No. 1(General Purpose)NOTE 1The cell classification of this standard is G

36、P5-15443.Method Accepted ValueAInherent viscosity D 1243 1.0186 0.012Percent through No. 200 sieve D 1921 1.3 6 0.4Apparent density, g/1000 cm3D 1895 503 6 5Plasticizer sorption, phr D 1755 101 6 6Dry flow, s/400 cm3D 1755 2.6 6 0.2Conductivity, S/cmg D 1755 1.0 6 0.3Porosity, cm3/g D 2873 0.268 6 0

37、.022Powder mix time, s D 2396 163 6 17AExpected range for mean of two replicates (within a probability of 99.5 %).D 1755 92 (2001)314.3.1 A-C Wheatstone Bridge, having a range up to250 000V , a 100 6 50-Hz oscillator and a sensitive null pointindicator with minimum accuracy of 6 2%.14.3.2 Dip Cell,1

38、3having platinum electrodes and a cellconstant of about 0.1 cm1, similar to the one shown in Fig. 1.The cell shall be prepared and calibrated in accordance withTest Method D 495.14.3.3 Thermometer, equivalent to or better than ASTMPartial Immersion Thermometer, having a range from 20to +150C and con

39、forming to the requirements for Thermom-eter 1C in accordance with Specifications E1.14.3.4 Electric Hot Plate.14.4 Reagents:14.4.1 High-Purity WaterWater having a conductivity notgreater than 1.0 S/cm, prepared in accordance with TestMethod D 2132.NOTE 6Ahigh-purity water may also be obtained by pa

40、ssing ordinarydistilled water through a dual-bed ion exchange column packed with anappropriate resin.1414.4.2 Isopropyl Alcohol, ACS reagent grade.14.5 Procedure:14.5.1 Place a resin sample weighing 2.00 6 0.01gina250-mLErlenmeyer flask that has previously been rinsed twicewith boiling, high-purity

41、water.Add 5.0 6 0.5 mL of isopropylalcohol to the sample, and swirl the mixture until the resin isuniformly wet. Add 1006 1 mL of boiling, high-purity water,set a watch glass on top of the flask, and boil gently for 5 min.Cool rapidly to 23 6 1C. Allow the resin to settle, and thenplace the dip cell

42、 in the flask so that the electrodes arecompletely immersed, as shown in Fig. 2. Measure the resis-tance on the most sensitive scale of the bridge after 30-simmersion. Perform determinations in duplicate.14.5.2 Between measurements, rinse the cell thoroughly inhigh-purity water and gently shake off

43、any water clinging to thesurface.14.5.3 BlankMake duplicate parallel determinations us-ing 5 mLof isopropyl alcohol and 100 mLof high-purity water.14.5.4 CalculationCalculate the electrical conductivity ofthe extract solution as follows:Electrical conductivity, S/cmg 5 L/R22 L/R3!/m 3 106where:13The

44、 cell illustrated is a Leeds and Northrup Conductivity Cell No. 4920. Othercells are available from Beckman Instruments, Inc., Cedar Grove, NJ 07009, andRutherford Research Products Co., Rutherford, NJ 07070.14Amberlite MB-1, available from the Rohm and Haas Co., Philadelphia, PA, issatisfactory for

45、 this purpose.FIG. 1 Dip Cell for Electrical Conductivity TestFIG. 2 Dip Cell Immersed in FlaskD 1755 92 (2001)4L = cell constant,R2= resistance, V, of extract solution,R3= resistance, V, of blank, andm = sample weight, g.14.6 ReportReport the average of duplicate determina-tions of electrical condu

46、ctivity in S/cmg of sample.14.7 Precision and BiasThe precision of the test method,calculated by analysis of the round-robin data from fourlaboratories, is as follows:14.7.1 RepeatabilityCoefficient of variation (average ofreplicates) within a laboratory of 14.7 %.14.7.2 ReproducibilityCoefficient o

47、f variation (average ofreplicates) between laboratories of 17.2 %.15. Plasticizer Sorption15.1 ScopeThis test method covers the measurement ofthe amount of plasticizer that a resin can absorb at the standardlaboratory temperature. Plasticizer sorption is one of theparameters for judging the dry blen

48、ding properties of a resin.This test method is similar in many respects to that employedin Test Method D 281.15.2 Apparatus:15.2.1 Platform Scales or Balance, 0.01-g accuracy.15.2.2 Glass or Glazed Porcelain Plate, 254 by 254 by 6.4mm (10 by 10 by 0.25 in.), minimum.15.2.3 Spatula, with width and sh

49、ape to fit mold cavity (seeFig. 3).15.2.4 Dropping Bottle, 60-mL capacity.15.2.5 Mold, aluminum or brass, as shown in Fig. 3.15.3 PlasticizerDi(2-ethylhexyl)-phthalate (DOP), Type Iin Specification D 1249.15.4 ConditioningDetermine plasticizer sorption at theStandard Laboratory Temperature of 23 6 1C.15.5 ProcedureWeigh 5 6 0.01 g of resin and transfer itto the plate. Obtain the gross weight, to the nearest 0.01 g ofthe dropping bottle about half full of DOP. Begin adding theDOP to the resin in 1-mL increments, using the spatu