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Designation: D2538 − 02 (Reapproved 2010

)

Standard Practice for
Fusion of Poly(Vinyl Chloride) (PVC) Compounds Using a
Torque Rheometer1
This standard is issued under the fixed designation D2538; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 4. Summary of Practice
1.1 This practice covers the relative fusion characteristics of 4.1 A sample of powder-mix compound is added to the
poly(vinyl chloride) compounds. heated roller mixer chamber and is transformed into a fused
1.2 The test procedures appear in the following order: mass.
Section 4.2 The resulting torque curve can be used to determine the
relative fusion time and fusion characteristics.
Fusion Test 9
Thermal Stability Test 10 5. Significance and Use
Color-Hold Stability Test 11
Shear Stability Test 12 5.1 When PVC compounds are mixed under appropriate
1.3 The values stated in SI units are to be regarded as the conditions of heat and shear, a fused mass is produced. This
standard. mass has certain melt characteristics which can be defined with
1.4 This standard does not purport to address all of the a torque rheometer operated under fixed conditions of shear
safety concerns, if any, associated with its use. It is the and temperature. The fusion characteristics of a PVC com-
responsibility of the user of this standard to establish appro- pound are manifest as fusion time, fusion torque, melt torque,
priate safety and health practices and determine the applica- melt viscosity, and heat and color stability.
bility of regulatory limitations prior to use. Specific hazards 5.2 A control lot is to be used as a standard against which
statements are given in Section 8. other test results are to be compared. Test data are to be
evaluated relative to the control lot.
NOTE 1—There are no ISO standards covering the primary subject
matter of this ASTM standard.
6. Apparatus
2. Referenced Documents 6.1 Microprocessor Torque Rheometer,3equipped with a
high-shear mixer with roller-style blades, bowl-jacket
2.1 ASTM Standards:2
thermocouple, stock thermocouple, and temperature recorder.
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plas- NOTE 2—A torque rheometer without microprocessor capability can be
tics used to perform the fusion, thermal stability, and color hold tests.
E691 Practice for Conducting an Interlaboratory Study to 6.1.1 For flexible and rigid compounds, use a Type 6 roller
Determine the Precision of a Test Method head with a rotor ratio of 3 Drive: 2 Driven.
NOTE 3—A Type 5 roller head can also be used, but the data generated
3. Terminology cannot be compared with the Type 6 data.
3.1 Definitions—Definitions are in accordance with Termi- 6.2 Quick-Loading Powder Chute or equivalent.
nologies D883 and D1600 unless otherwise indicated. 6.3 Brass Knife.
6.4 Brass Wool or Brush.
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and 6.5 Insulated Gloves.
is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials. 6.6 Balance, 500-g minimum capacity, with a 0.1-g sensi-
Current edition approved Nov. 1, 2010. Published March 2011. Originally
approved in 1969. Last previous edition approved in 2002 as D2538 – 02. tivity.
DOI:10.1520/D2538-02R10.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Suitable equipment may be obtained from C. W. Brabender, 50 E. Wesley St.,
Standards volume information, refer to the standard’s Document Summary page on South Hackensack, NJ 07606, and Haake Buchler Instruments, 244 Saddle River
the ASTM website. Rd., Saddle Brook, NJ 07662.

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Copyright by ASTM Int'l (all rights reserved); 1

6. steady state.4. 7. 9. relatively flat.3.1 The fusion torque to the nearest 100 m·g.9 Aluminum Foil. blended in an pound.3.2 Fusion Time—The time from the point of loading to where: the point of maximum torque.6 Impact Modifier.4 constraint.1 The compound may be beaker-mixed. Since some cooling takes place when compound are found in Appendix X2.2-9. Fusion Test Method 9.7 Stabilizer. allow sufficient time to confirm that the 9.5 Report—Report the following information: the sample size to reproduce a fusion curve equivalent to previous curves. the torque curve indicates maximum torque has been reached. before using again.1.10 Timer. 6. 1): sample size 5 @ ~ V 2 D ! 3 65 % # 3 specific gravity (1) 9.4 Interpretation of Torque Rheometer Curve (Fig. as damage to the mixer or to the torque rheometer may result.1 Compound Preparation: chute on the roller-head mixer and pour in the sample com- 9. 7. Hazards 8.3. the start of each test.4. 7. 7. 6. 9. 8. 9. it will be necessary to increase 9. 1 Torque Rheometer Curve to handle the hot equipment should be worn when conducting these tests. 7. With the mixer running.3 Continue mixing until the melt torque achieves a bowl. pound from the bowl and blades using the brass knife or wool.1 Determine the sample size to be added to the mixer. cleaning the bowl.2. Suggested combinations for several types of PVC for additional tests. 8.1.3.3.12 Hand-Press Mold.2 Weigh a sample of the test compound in accordance with 9.1 Mount the roller head on the torque rheometer. the total weight of the remove the loading chute and weight.2 Do not attempt to clean or poke objects into the mixer while it is running. NOTE 4—The correct sample size for the mixer is when the fusion curve will duplicate itself.8 Pigments. 9.2 Filter. 7.3 Gloves with sufficient insulation to enable the operator FIG. 8.5 Process-Aid. Clean the com- 9. stainless steel.3 With the mixer empty and running.3 Melt Torque—The fusion where the torque curve is D = volume displacement or rotors. and 9. compound should equal the amount charged to the roller-head 9.3. Copyright by ASTM Int'l (all rights reserved).8 Oven.5. D2538 − 02 (2010) 6.3.1 Fusion Torque—The point of maximum torque. zero the recording mixing bowl has reached equilibrium at the test temperature pen on the chart. 7. Materials 7.1 Poly(Vinyl Chloride) Resin. When intensive mixer or a ribbon blender.2 Equipment Preparation: 9. 9.3 Procedure: NOTE 5—The quick-loading chute should be at the same temperature at 9. 2 .1 Do not exceed the power capacity of the instrument. Heat or cool as required.7 Beaker. 9.2.2. 6. position the quick-loading 9. using the following formula: 9. If the compound is beaker-mixed.4 Stop the mixer and open the bowl.3. 400 mL.4 Plasticizer. As the mixer wears. 6.5 Reassemble the mixing bowl and repeat 9.4. 7. Place the ram into the chute and add the weight.3 Lubricants. or blended and pelletized. V = volume of mixer bowl without rotors.11 Long-Nose Pliers. permit the test to be completed within a reasonable time 9.2 Select a temperature/rotor speed combination that will or both.

12. 11.1.5. 10. 10.3. When 10. and or both.3. 11.3.3.1. the weight. 11.4 Report—Report the following information: 10. Place the ram into the chute and add the weight.5. 11.1 Set the microprocessor for the desired temperature with 9.5. the weight.5.3. Color-Hold Stability Test Method 12.3 for additional tests.3. 11. stopping at the same point in time as 11. With the mixer running.5.1 Weigh a sample of the test compound in accordance with 9. Place the ram into the chute and add the weight.3. 10.3 Procedure: 11. Place the ram into the chute and add the weight.3 Procedure: and the sample size used. rotor revolutions per and minute.2 Return to 0 r/min. rotor revolutions per minute. 10. Copyright by ASTM Int'l (all rights reserved).1.3 Program the speed control to run from 0 to 100 11. NOTE 7—Depleting the sample from the bowl can affect the amount of 9. 10.2 Using the point of maximum torque (fusion torque) r/min in 1 min and stop. rotor revolutions per minute.4 Reassemble the mixing bowl and repeat plaque.1.5 Report—Report the following information: and 10. 1): 11. remove the loading bowl. Position the quick-loading long-nose pliers to remove a sample from the bowl.5 Stop the mixer and open the bowl. position the quick-loading and program the revolutions per minute as follows: chute on the roller-head mixer and pour in the sample com.3 Stop the mixer and open the bowl. 11.2.1. remove the contents. 3. 12.2 The fusion time to the nearest 1⁄2 min. NOTE 6—If the melt torque is not steady.1 Prepare the test compound in accordance with 9. D2538 − 02 (2010) 9. When with 9. indicating decomposition of the PVC compound.5.5.4 Run additional tests. pound.2.5. the sample size.3.2.2 The temperature of test. 11.6 Report—Report the following information: 11. Restart the chute on the roller-head mixer. and the sample size used.1. With the mixer running.3.3. When min. remove the loading chute and 12. chute.6.5 Alternative Procedure: chute on the roller-head mixer and pour in the sample com.4.1 Prepare the test compound in accordance with 9.3. as zero time. as zero time. turn on the torque rheometer. 3 . of maximum torque (fusion torque) to the point of sudden torque increase.6.2 Prepare the test equipment in accordance with 9. 10. approximate the value and 11.3. discolor.1 Compound Heat Stability—The time from the point rimeter (or equivalent).5 Measure the color of the plaque in a Hunter Colo- 10. the torque curve indicates fusion.5.1. rotors.2 Using the point of maximum torque (fusion torque) pound from the bowl and blades using the brass knife or wool. scale.3 Clean the bowl and blades and reassemble the mixer.3 The melt torque to the nearest 100 m·g. Stop the rotors and use a pair of a sample of the test compound. position the quick-loading the torque curve indicates fusion.5. pound from the bowl and blades. remove more than half the sample. 12.3.6 Reassemble the mixing bowl and repeat 11. using the brass knife or wool. Clean the com.5.2 Prepare the test equipment in accordance with 9.3.1 Prepare the test compound in accordance with 9.1 The compound heat stability to the nearest 1⁄2 min.2 When the bowl temperature has stabilized.1.1 Report to the nearest 25 m·g when using a 0 to 1000 11.3. run the mixer until the compound starts to or both.3.2.4 Continue sampling until the desired color change has 9.2 Continue running until there is a sudden rise in the the torque curve indicates fusion. and press into a 10.1. 11.5. weigh out intervals of 2.1-11.4 Interpretation of Torque Rheometer Curve (Fig. 11. When the ram bottoms. 12. remove the loading chute and torque curve.3.2 The temperature of the test. Clean the com- note whether the torque is increasing or decreasing.2 Prepare the test equipment in accordance with 9.4. Place the compound into a hand press to shape the and pour in the sample compound. remove a sample of the compound at regular time 12.5 for additional tests. Select a time sequence that does not scale.1-10. Shear Stability Test Method 11. With the mixer running.1 Weigh a sample of the test compound in accordance 12.1 Weigh a sample of the test compound in accordance pound. sample size used. Place the ram into the chute sample.5. Thermal Stability Test Method reached the test temperature before starting. Confirm that the bowl has 10. 9. reached the test temperature before starting.3.1.3.1 The time to equivalent color change and 11. and the time as determined in 11. been observed. or 5 min. Trim the sample and return the excess to the mixing and add the weight.4. rotor revolutions per minute.2 The temperature of test. position the quick-loading 11. 11.5.3 Procedure: 12.3.3.3.1 The color number measured on the pressed plaque 10.3. Confirm that the bowl has 11. 11. 11.4 Temperature of test. NOTE 8—Use the microprocessor torque rheometer for this test.2. Stop the mixer. 9.1 Run at preselected revolutions per minute for ten pound. 10.1 Report to the nearest 25 m·g when using a 0 to 1000 working the compound receives. remove the loading chute and chute on the roller-head mixer and pour in the sample com- weight.3 Mount the samples in a sequential time order.

52 4. prepared at the laboratories that tested them.9 % Material C 85. 4 .5 for additional tests.2 2. Request RR:D20-1237.1. Copyright by ASTM Int'l (all rights reserved).91 10.94 7.7 % Material E 56. Point E (Newton-meters).33 5.21 12.08 3.97 2.97 13. using the brass knife or wool.8 % Material A 25.72 22.65 10.38 57.2 The calculation programmed into the software is 12.62 4.55 10.72 10.2 Technical Analysis: 13.2 % Material C 188.6 % 2. A higher index cessor to plot the torque versus revolutions per minute.85 4.1 0.91 2.30 1.3. Mean Level in Ascending Order Within Laboratories Between Laboratories Material Mean Level Sr r (r) SR R (R) Material B 17. Mean Level in Ascending Order Within Laboratories Between Laboratories Material Mean Level Sr r (r) SR R (R) Material B 171.4 When the mixer has stopped.62 5.40 6. materials.2 5.3 % Pooled Values 179.26 0.18 7.1.1 % 2.85 2.98 3. formulations. Time at Fusion Minus Time at Load Torque.2 The torque versus revolutions per minute plot can be tested three times on two separate days yielding six points per used as a relative comparison of shear sensitivity.1 1.17 24.45 20. A large arc or loop denotes more precision of this test method.7 % 9.8 3.92 7.65 7.53 2. D2538 − 02 (2010) TABLE 1 Round Robin Test Results Parameter 1– Fusion Torque.31 30. or labo- ratories.6 7. A acceptance or rejection of materials. the shear sensitivity can be intended to present a meaningful way of considering the approximate estimated by the degree of arc.1 Table 1 is based on a round robin4 conducted in 2001 12.9 0. The data in Table 1 should not be applied to shear-sensitive material than does a smaller arc or loop.2 % 2.3 % Material E 22.6 8.83 26.59 17.73 13. as these data apply only to the visual observation can be made to determine the relative shear materials tested in the round robin and are unlikely to be rigorously sensitivity between sample materials.09 5.6 1.2.21 9.3.92 2.3 Bearing in mind that a straight inclined line would NOTE 9—Caution: The explanation of r and R (14.7 % 20.3 0.95 2. Interpretation of Torque Rheometer Results used a computerized torque rheometer and a single zone 13.7 % Material A 183.53 7.05 66.58 11.2.25 2. representative of other lots.5 % 2.3.2.73 3.3 2.6 % 3.5 % Material D 174.78 13.5 % 3. or stabilized torque. software is programmed to give such a number.97 23.15 22.1 Visual Analysis: electrically heated mixer/measuring head (3:2 gear ratio) to 13.3.6 % 0.58 1. Each sample was 13.61 5.7 4.36 37.78 2.1 % Material A 70.0 % Pooled Values 33.6 0.53 11.82 56.43 9.8 % Material B 30. Use the number denotes a more shear-sensitive material.39 1.2 % 4.78 6. Point X (Newton-meters).9 0. Mean Level in Ascending Order Within Laboratories Between Laboratories Material Mean Level Sr r (r) SR R (R) Material C 29.5 % 12.06 2.9 % 12.35 0.7 1.58 26.79 35.21 6. all the samples were fusion curve which can be used to determine the fusion time. Mean Level in Ascending Order Within Laboratories Between Laboratories Material Mean Level Sr r (r) SR R (R) Material D 40. 14. (degrees Celsius).79 2.23 6.1 % 3.8 % Material E 31.1 % 4.6 % Pooled Values 60.14 4. or both.2-14.8 % 0.7 % Pooled Values 23.71 1.61 21. conditions.1 The torque versus revolutions per minute plotted graph can be used in conjunction with the microprocessor 4 Supporting data giving results of the round robin have been filed at ASTM software to provide a shear-sensitivity index number.3 % Material C 23.5 0.3 When the sample run is finished.85 2.86 51.2 % Material B 47.86 3.24 7.8 % 0.41 15.47 6.00 5. data value. open the bowl.99 65.20 8.98 10.5 0. in accordance with Practice E691.2 1.3 % 0. use the micropro.39 32.1.82 58.6 0.4 % 1.41 1.92 22.3 % Parameter 3– End Torque.4 % Material D 27.19 20.1 The first 10 min of the graph represents a standard process the samples.40 52.0 0. For each material. The International Headquarters.90 2.21 36. prepared at one source. Precision and Bias 12.2 % 2.4 0.15 3.4 % 2.4 % Parameter 2– Fusion Torque Temperature.05 2.9 % 7.5 0.79 2.5 0.2 % 13. but the individual specimens were fusion torque and melt. 13.38 3.3.25 3. plotted curve for analysis.1 % Parameter 4– Fusion Time (s).3) is only denote a Newtonian material.38 3.8 % 0.0 1.41 6. 13.6 % 1. Clean shown in the Appendix X1.2 % 13.48 1.4 % Material D 39.8 % Material A 35.1-12.08 21.57 7.94 19.64 1.0 % Material E 181.82 2.42 15. All laboratories 13.30 0. Users of this method should apply the principles outlined in 13.5 Reassemble the mixing bowl and repeat 14. involving five rigid PVC dry blend compounds tested by ten laboratories. the compound from the bowl and blades.

then: 14. where R = 2. X1. rheometry APPENDIXES (Nonmandatory Information) X1. measurement units the same material. % different equipment on different days.4.2 If the shear-sensitivity approaches zero (n ap- curve at 50 r/min as shown in Fig.3 Any judgment in accordance with 14. and for test results would have an approximate 95 % (0.2.1 Repeatability (r)—Two results obtained within one 15.3 Calculation—Calculate the shear sensitivity of temperature can be obtained by using speed programming. fusion of PVC compound.2 Reference Curve X1. D2538 − 02 (2010) Practice E691 to generate data specific to their materials and laboratory (or the critical difference between two test results for the same between specific laboratories). measurement units two laboratories shall be judged not equivalent if they differ by (r) = within laboratory repeatability.2.2. NOTE 10—Symbols are defined as follows: Sr = within laboratory standard deviation 14. between the reference revolutions per minute and the torque X1. where r = 2. 5 .2 Concept of r and R in Table 1—If Sr and SR have been 14.1 or 14.1 The torque versus revolutions per minute curve at test X1. Use pseudoplastics. X1. correct.4 Data Interpretation (see Fig.1 Torque Versus Revolutions Per Minute Curve FIG.2 Reproducibility (R)—Two results obtained between r = within laboratory repeatability. X1. Copyright by ASTM Int'l (all rights reserved). S.2 calculated from a large enough body of data.2 Draw a reference line from the origin to the intercept erlaw index n approaches zero). X1. X1. r is the interval representing ity. it is more shear sensitive. The principles of 14.8SR.1 If the shear-sensitivity index approaches one (pow- X1. heat stabil- than the r-value.3 would then material. PVC compounds. it is less shear sensitive. Keywords laboratory shall be judged not equivalent if they differ by more 15. % more than the R-value.2. obtained by a different operators using (R) = between laboratory reproducibility. equipment on the same day in the same laboratory.8Sr. CALCULATION OF SHEAR SENSITIVITY FIG. X1.3.2. X1.2-14.95) probability of being that were averages from testing one point for each test result. proaches one). obtained by the same operator using the same be valid for such data. the first half of the torque versus revolutions per minute curve (0 to 50 r/min) in order to avoid melt temperature rise due to X1.1).3): frictional heat (Fig. 14.2.2. as shown in Fig.1 color stability.4. R is the interval SR = between laboratory standard deviation representing the critical difference between two test results for R = between laboratory reproducibility.

and M = torque (m·g). X1.org (e-mail). Users of this standard are expressly advised that determination of the validity of any such patent rights. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. FIG. 6 .astm.1 Suggested temperature/rotor speed combinations for PVC compounds are as follows: Compound Type Suggested Set Temperature/Rotor Speed Flexible Compound 140°C (284°F) @ 31 r/min Semirigid Compound 180°C (356°F) @ 50 r/min Rigid Compound 197°C (387°F) @ 60 r/min ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. either reapproved or withdrawn. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone). This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised. West Conshohocken. PA 19428-2959. SUGGESTED TEMPERATURE/ROTOR SPEED COMBINATIONS FOR PVC COMPOUNDS X2. which you may attend. Copyright by ASTM Int'l (all rights reserved). PO Box C700. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. Permission rights to photocopy the standard may also be secured from the ASTM website (www. 100 Barr Harbor Drive. and the risk of infringement of such rights. 610-832-9555 (fax). This standard is copyrighted by ASTM International. United States. Your comments will receive careful consideration at a meeting of the responsible technical committee.astm. B = area of triangle. or service@astm. D2538 − 02 (2010) where: A = area of arc. are entirely their own responsibility. or through the ASTM website (www. at the address shown below.org/ COPYRIGHT/).org).3 Shear Sensitivity of Pseudoplastic Materials X2.