ASTM D1755-2009 Standard Specification for Poly(Vinyl Chloride) Resins《聚氯乙烯树脂标准规范》.pdf

1、Designation: D 1755 09Standard 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 number in parenthe

2、ses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This specification covers the establishment of require-ments for homopolymers of vinyl chloride in original powderform intended for subsequent mixing an

3、d 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-purpose resins yield a

4、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.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard doe

5、s 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 practices and determine the applica-bility of regulatory limitations prior to use.NOTE 1This standard and ISO 1264 198

6、0 address the same subjectmatter, but differ in technical content (and results cannot be directlycompared between the two test methods.2. Referenced Documents2.1 ASTM Standards:2D 281 Test Method for Oil Absorption of Pigments bySpatula Rub-outD 495 Test Method for High-Voltage, Low-Current, DryArc

7、Resistance of Solid Electrical InsulationD 883 Terminology Relating to PlasticsD 1125 Test Methods for Electrical Conductivity and Re-sistivity of WaterD 1243 Test Method for Dilute Solution Viscosity of VinylChloride PolymersD 1600 Terminology for Abbreviated Terms Relating toPlasticsD 1823 Test Me

8、thod for Apparent Viscosity of Plastisolsand Organosols at High Shear Rates by Extrusion Viscom-eterD 1824 Test Method for Apparent Viscosity of Plastisolsand Organosols at Low Shear RatesD 1895 Test Methods for Apparent Density, Bulk Factor,and Pourability of Plastic MaterialsD 1921 Test Methods fo

9、r Particle Size (Sieve Analysis) ofPlastic MaterialsD 2132 Test Method for Dust-and-Fog Tracking and Ero-sion Resistance of Electrical Insulating MaterialsD 2396 Test Methods for Powder-Mix Time of Poly(VinylChloride) (PVC) Resins Using a Torque RheometerD 3030 Test Method for Volatile Matter (Inclu

10、ding Water)of Vinyl Chloride ResinsD 3892 Practice for Packaging/Packing of PlasticsE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 DefinitionsDefinitions are in accordance with Termi-nology D 883 and Terminology D 1600, unless otherwiseindicated.4. Classification4.1 TypesThi

11、s 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 for usein organosols and plastisols. As a class, these are small inparticle size.4.2 Gra

12、desThis specification provides for as many gradesof resin as it is feasible to be selected from the possiblecombinations of requirements in Table 1 and Table 2. A gradeis designated by first indicating the type (GPor D), followed bycell numbers for each property in the order in which they arelisted

13、in Table 1 and Table 2. Where there is no interest in aproperty, a “0” is entered in place of a cell number. If it weredesirable, it is acceptable to extend a cell limit by half the cell1This specification is under the jurisdiction of ASTM Committee D20 onPlastics and is the direct responsibility of

14、 Subcommittee D20.15 on ThermoplasticMaterials.Current edition approved Feb. 1, 2009. Published February 2009. Originallyapproved in 1960. Last previous edition approved in 2001 as D 1755 - 92(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service

15、 at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM 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 19428-2

16、959, United States.range into the next higher or lower cell, but not both. When thisis done, it is indicated by a dash above the cell number ( n)ifthe extension is into the higher cell, or a dash below (n) if intothe lower cell. Extension of cell limits applies only to cellswhere ranges of propertie

17、s are allowed and not where maxi-mum or minimum values are specified. The cell number of thefirst property (dilute solution viscosity) is separated from thosethat follow by a dash.4.3 Inherent Viscosity Cell NumberWhen selecting theinherent viscosity cell number, the number shall cover the fullinher

18、ent viscosity production range for the specific product. Aresin with an inherent viscosity of 1.07 to 1.11 productionrange would have a 5 cell number. A resin with an inherentviscosity of 1.10 to 1.14 production range would have a 6 cellnumber5. General Requirements5.1 The resin shall be in powder f

19、orm.5.2 The resin shall conform to the requirements of Table 1or Table 2, as specified by the type and grade designationagreed upon between the purchaser and the supplier.NOTE 2It is possible that properties not covered, such as heatstability, color, and volatile loss, are also important for applica

20、tionperformance in compounds.6. Sampling6.1 Sample using a statistically acceptable procedure.7. Number of Tests7.1 One set of test specimens shall be considered sufficientfor testing each batch.8. Retest and Rejection8.1 If any failure occurs, the materials shall be permitted tobe retested to estab

21、lish conformity in accordance with anagreement between the 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 3Specifications for sieve analysis (Table 1) are pri

22、marilyintended 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. Prepare theplastisol sample as follows:12.1.1 PlasticizerDi (2-ethylhexyl) phthalate (DOP).TABLE 1 Type GP, General-Purpose Resin Requirem

23、entsDesig-nationOrderNo.PropertyCell Limits01 2 3 4 5 6 7 8 91 Dilute solution(inherent) viscosityunspecfied 0.39 0.70 0.75 0.87 0.99 1.09 1.19 1.29 1.382 Sieve analysis,percent throughNo. 200 (75-m)sieveunspecified 0 to 9 10 to 19 20 to 29 30 to 39 40 to 49 50 to 59 60 to 79 80 to 99 1003 Apparent

24、(bulk)density:g/1000 cm3unspecified 1993 Severs viscosity,poiseunspecified 0 to 49 50 to 99 100 to 149 150 to 199 200 to 299 300 to 499 500 to 999 1000 to 1499 1499D175509212.1.2 Apparatus:12.1.2.1 Mixer, planetary-gear type, equipped with flatbeater mixing paddle.12.1.2.2 Vacuum Desiccator, capable

25、 of being evacuated to133 Pa (1 mm Hg).12.1.3 Procedure: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.

26、3.2 Mount the bowl on the mixer and mix for 5 min 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 ex

27、ceed 5C. Use a cooling bath if necessary.12.1.3.3 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

28、 that the plastisol does not overflow the containerduring 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

29、 12.1.1-12.1.3.14. Electrical Conductivity of Water 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 relative

30、lysmall differences among different lots of electrical 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 ele

31、ctrical insulation.Electrical grade resins generally yield conductivity values lessthan 6 S/cmg.14.3 Apparatus:14.3.1 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, having platinum elec

32、trodes 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 conforming to the requir

33、ements 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 4It is also possible to obtain a high-purity water by passingordina

34、ry distilled water through a dual-bed ion exchange column packedwith an appropriate resin.14.4.2 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 water.Add 5.0

35、 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 in the flask

36、 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.FIG. 1 Dip Cell for Electrical Conductivity TestD175509314.5.2 Between measurements, rinse the cell thoroughl

37、y inhigh-purity water and gently shake off 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 conductiv

38、ity, S/cmg 5 L/R22 L/R3!/m 3 106where:L = 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 conductivity in S/cmg of sample.14.7 Precision and BiasThe precision of the tes

39、t 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 of variation (average ofreplicates) between laboratories of 17.2 %.15. Plas

40、ticizer 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 blending properties of a resin.This test method is similar in many respects to

41、 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 shape to fit mold cavity (seeFig. 3).15.2.4 Dropping Bottle, 60-mL capacity.

42、15.2.5 Mold, aluminum or brass, as shown in Fig. 3.15.3 PlasticizerDi(2-ethylhexyl)-phthalate (DOP).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 ne

43、arest 0.01 g ofthe dropping bottle about half full of DOP. Begin adding theDOP to the resin in 1-mL increments, using the spatula formixing after each. When 4 mL have been added, change therate to two drops at a time, making consistency determinationsuntil the end point is reached. This is done by f

44、illing the mold,as it rests on the plate, with the mixture and then sliding thespatula under the charge. Lift the charge above the mold cavitywith the spatula horizontal, and then rotate the blade to aFIG. 2 Dip Cell Immersed in FlaskFIG. 3 Mold for Plasticizer Sorption TestD1755094vertical position

45、. The end point is reached when the mixturefirst slides off the blade. At this point, reweigh the droppingbottle and its contents. Make duplicate determinations.NOTE 5Return the mix portions used for consistency determinationsto the main mix for each subsequent addition of plasticizer until the endp

46、oint is reached.15.6 CalculationCalculate the plasticizer sorption as fol-lows:Plasticizer sorption, parts of DOP per 100parts of resin by weight 5W02 W1!320where:W0= original weight of dropping bottle and DOP, andW1= final weight of dropping bottle and DOP.15.7 ReportReport the parts of DOPper 100

47、parts of resinby weight for the average of duplicate determinations.15.8 Precision and BiasThe precision of the test method,calculated by analysis of round-robin data from six laborato-ries, is as follows:15.8.1 RepeatabilityCoefficient of variation (average ofreplicates) within a laboratory of 2.1

48、%.15.8.2 ReproducibilityCoefficient of variation (average ofreplicates) between laboratories of 5.0 %.16. Dry Flow16.1 Summary of Test MethodThe dry flow characteristicsof powdered resins bear a complex relationship to particleshape, structure, and size distribution. One way of measuringthe flow is

49、by measuring the time for a prescribed volume ofresin to flow through a standard funnel. The funnel orifice mustbe large enough to permit continuous flow of dry resins withoutbridging. The volatile content of the resin shall be within 650 % of the average specified by the manufacturer (see TestMethod D 3030).NOTE 6Resins of abnormally high or abnormally low moisturecontent will exhibit reduced nonuniform flow. It is possible that extremelydry resins will develop static changes that will impede flow; damp resinwill coalesce.16.2 Si