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1. Scope
1.1 This practice covers the relative fusion characteristics of
poly(vinyl chloride) compounds.
1.2 The test procedures appear in the following order:
Section
Fusion Test
Thermal Stability Test
Color-Hold Stability Test
Shear Stability Test
9
10
11
12
6. Apparatus
6.1 Microprocessor Torque Rheometer,4 equipped with a
high-shear mixer with roller-style blades, bowl-jacket thermocouple, stock thermocouple, and temperature recorder.
2. Referenced Documents
2.1 ASTM Standards:
D 883 Terminology Relating to Plastics2
D 1600 Terminology for Abbreviated Terms Relating to
Plastics2
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method3
3. Terminology
3.1 DefinitionsDefinitions are in accordance with Terminologies D 883 and D 1600 unless otherwise indicated.
4. Summary of Practice
4.1 A sample of powder-mix compound is added to the
heated roller mixer chamber and is transformed into a fused
mass.
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials.
Current edition approved August 10, 2002. Published October 2002. Originally
published as D 2538 69. Last previous edition D 2538 95(01).
2
Annual Book of ASTM Standards, Vol 08.01.
3
Annual Book of ASTM Standards, Vol 14.02.
4
Suitable equipment may be obtained from C. W. Brabender, 50 E. Wesley St.,
South Hackensack, NJ 07606, and Haake Buchler Instruments, 244 Saddle River
Rd., Saddle Brook, NJ 07662.
Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 2538 02
cleaning the bowl, allow sufficient time to confirm that the
mixing bowl has reached equilibrium at the test temperature
before using again.
7. Materials
7.1 Poly(Vinyl Chloride) Resin.
7.2 Filter.
7.3 Lubricants.
7.4 Plasticizer.
7.5 Process-Aid.
7.6 Impact Modifier.
7.7 Stabilizer.
7.8 Pigments.
8. Hazards
8.1 Do not exceed the power capacity of the instrument, as
damage to the mixer or to the torque rheometer may result.
8.2 Do not attempt to clean or poke objects into the mixer
while it is running.
8.3 Gloves with sufficient insulation to enable the operator
to handle the hot equipment should be worn when conducting
these tests.
9. Fusion Test Method
9.1 Compound Preparation:
9.1.1 The compound may be beaker-mixed, blended in an
intensive mixer or a ribbon blender, or blended and pelletized.
If the compound is beaker-mixed, the total weight of the
compound should equal the amount charged to the roller-head
bowl.
9.2 Equipment Preparation:
9.2.1 Mount the roller head on the torque rheometer.
9.2.2 Select a temperature/rotor speed combination that will
permit the test to be completed within a reasonable time
constraint. Suggested combinations for several types of PVC
compound are found in Appendix X2.
9.2.3 With the mixer empty and running, zero the recording
pen on the chart.
9.3 Procedure:
9.3.1 Determine the sample size to be added to the mixer,
using the following formula:
sample size 5 @~V 2 D! 3 65 %# 3 specific gravity
NOTE 6If the melt torque is not steady, approximate the value and
note whether the torque is increasing or decreasing.
(1)
where:
V = volume of mixer bowl without rotors, and
D = volume displacement or rotors.
NOTE 4The correct sample size for the mixer is when the fusion curve
will duplicate itself. As the mixer wears, it will be necessary to increase
the sample size to reproduce a fusion curve equivalent to previous curves.
D 2538 02
11.5 Alternative Procedure:
11.5.1 Weigh a sample of the test compound in accordance
with 9.3.1. With the mixer running, position the quick-loading
chute on the roller-head mixer and pour in the sample compound. Place the ram into the chute and add the weight. When
the torque curve indicates fusion, remove the loading chute and
the weight.
11.5.2 Using the point of maximum torque (fusion torque)
as zero time, run the mixer until the compound starts to
discolor. Stop the mixer, remove the contents, and press into a
plaque.
11.5.3 Clean the bowl and blades and reassemble the mixer.
11.5.4 Run additional tests, stopping at the same point in
time as 11.5.2.
11.5.5 Measure the color of the plaque in a Hunter Colorimeter (or equivalent).
11.6 ReportReport the following information:
11.6.1 The color number measured on the pressed plaque
and
11.6.2 The temperature of the test, rotor revolutions per
minute, the sample size, and the time as determined in 11.5.2.
10.3 Procedure:
10.3.1 Weigh a sample of the test compound in accordance
with 9.3.1. With the mixer running, position the quick-loading
chute on the roller-head mixer and pour in the sample compound. Place the ram into the chute and add the weight. When
the torque curve indicates fusion, remove the loading chute and
weight.
10.3.2 Continue running until there is a sudden rise in the
torque curve, indicating decomposition of the PVC compound.
10.3.3 Stop the mixer and open the bowl. Clean the compound from the bowl and blades using the brass knife or wool,
or both.
10.3.4 Reassemble the mixing bowl and repeat 10.3.110.3.3 for additional tests. Confirm that the bowl has reached
the test temperature before starting.
10.4 Interpretation of Torque Rheometer Curve (Fig. 1):
10.4.1 Compound Heat StabilityThe time from the point
of maximum torque (fusion torque) to the point of sudden
torque increase.
10.5 ReportReport the following information:
10.5.1 The compound heat stability to the nearest 12 min,
and
10.5.2 The temperature of test, rotor revolutions per minute,
and the sample size used.
NOTE 7Depleting the sample from the bowl can affect the amount of
working the compound receives. Select a time sequence that does not
remove more than half the sample.
12.3 Procedure:
12.3.1 Set the microprocessor for the desired temperature
and program the revolutions per minute as follows:
12.3.1.1 Run at preselected revolutions per minute for ten
min.
12.3.1.2 Return to 0 r/min.
12.3.1.3 Program the speed control to run from 0 to 100
r/min in 1 min and stop.
12.3.2 When the bowl temperature has stabilized, weigh out
a sample of the test compound. Position the quick-loading
chute on the roller-head mixer, turn on the torque rheometer,
and pour in the sample compound. Place the ram into the chute
and add the weight. When the ram bottoms, remove the loading
chute.
12.3.3 When the sample run is finished, use the microprocessor to plot the torque versus revolutions per minute. Use the
plotted curve for analysis.
12.3.4 When the mixer has stopped, open the bowl. Clean
the compound from the bowl and blades, using the brass knife
or wool, or both.
12.3.5 Reassemble the mixing bowl and repeat 12.3.112.3.5 for additional tests.
11.3.5 Stop the mixer and open the bowl. Clean the compound from the bowl and blades, using the brass knife or wool,
or both.
11.3.6 Reassemble the mixing bowl and repeat 11.3.111.3.5 for additional tests. Confirm that the bowl has reached
the test temperature before starting.
11.4 ReportReport the following information:
11.4.1 The time to equivalent color change and
11.4.2 The temperature of test, rotor revolutions per minute,
and the sample size used.
D 2538 02
in accordance with Practice E 691, involving five rigid PVC
dry blend compounds tested by ten laboratories. All laboratories used a computerized torque rheometer and a single zone
electrically heated mixer/measuring head (3:2 gear ratio) to
process the samples. For each material, all the samples were
prepared at one source, but the individual specimens were
prepared at the laboratories that tested them. Each sample was
tested three times on two separate days yielding six points per
data value.
5
Supporting data giving results of the round robin have been filed at ASTM
International Headquarters. Request RR: D20XXXX.
Between Laboratories
Material
Mean Level
Sr
(r)
SR
(R)
Material C
Material B
Material E
Material A
Material D
29.5
30.3
31.4
35.2
39.1
0.58
0.78
0.39
1.15
1.05
1.62
2.18
1.08
3.21
2.94
5.5 %
7.2 %
3.4 %
9.1 %
7.5 %
2.40
2.47
2.00
2.57
3.20
6.72
6.92
5.59
7.19
8.97
22.8 %
22.8 %
17.8 %
20.4 %
23.0 %
Pooled Values
33.1
0.79
2.21
6.6 %
2.53
7.08
21.4 %
Parameter 2 Fusion Torque Temperature, (degrees Celsius), Mean Level in Ascending Order
Within Laboratories
Between Laboratories
Material
Mean Level
Sr
(r)
SR
(R)
Material B
Material D
Material E
Material A
Material C
171.0
174.0
181.6
183.2
188.6
0.97
1.62
1.38
2.09
0.82
2.71
4.53
3.85
5.86
2.30
1.6 %
2.6 %
2.1 %
3.2 %
1.2 %
1.52
3.72
4.97
4.73
2.23
4.25
10.41
13.92
13.24
6.25
2.5 %
6.0 %
7.7 %
7.2 %
3.3 %
Pooled Values
179.7
1.38
3.85
2.1 %
3.43
9.61
5.3 %
Between Laboratories
Material
Mean Level
Sr
(r)
SR
(R)
Material B
Material E
Material C
Material A
Material D
17.9
22.5
23.6
25.5
27.9
0.30
0.26
0.48
0.35
0.64
0.85
0.73
1.33
0.98
1.78
4.8 %
3.3 %
5.6 %
3.8 %
6.4 %
0.79
0.90
0.91
0.95
1.06
2.21
2.53
2.55
2.65
2.98
12.3 %
11.3 %
10.8 %
10.4 %
10.7 %
Pooled Values
23.5
0.41
1.14
4.8 %
0.92
2.58
11.1 %
Parameter 4 Fusion Time (s), Time at Fusion Minus Time at Load Torque, Mean Level in Ascending Order
Within Laboratories
Between Laboratories
Material
Mean Level
Sr
(r)
SR
(R)
Material D
Material B
Material E
Material A
Material C
40.7
47.3
56.8
70.6
85.6
4.78
2.65
3.91
7.61
8.15
13.39
7.41
10.94
21.31
22.83
32.9 %
15.7 %
19.2 %
30.2 %
26.7 %
7.45
9.58
13.21
13.36
20.38
20.86
26.82
36.99
37.40
57.05
51.2 %
56.7 %
65.1 %
52.9 %
66.6 %
Pooled Values
60.2
5.42
15.17
24.9 %
12.79
35.82
58.5 %
D 2538 02
material, obtained by the same operator using the same
equipment on the same day in the same laboratory.
14.2.2 Reproducibility (R)Two results obtained between
two laboratories shall be judged not equivalent if they differ by
more than the R-value, where R = 2.8SR. R is the interval
representing the critical difference between two test results for
the same material, obtained by a different operators using
different equipment on different days.
14.2.3 Any judgment in accordance with 14.2.1 or 14.2.2
would have an approximate 95 % (0.95) probability of being
correct.
15. Keywords
15.1 color stability; fusion of PVC compound; heat stability; PVC compounds; rheometry
APPENDIXES
(Nonmandatory Information)
X1. CALCULATION OF SHEAR SENSITIVITY
D 2538 02
where:
A = area of arc,
B = area of triangle, and
M = torque (mg).
Compound Type
Flexible Compound
Semirigid Compound
Rigid Compound
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