Astm D1238 20

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
“Hak cipta ASTM International, 100 Barr Harbour Drive, West Conshohocken, PA 19428, USA. Copy ini dibuat oleh BSN di bawah lisensi ASTM International “
Designation: D1238 − 20
Standard Test Method for

Melt Flow Rates of Thermoplastics by Extrusion
Plastometer1
This standard is issued under the fixed designation D1238; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* E456 Terminology Relating to Quality and Statistics

1.1 This test method covers the determination of the rate of E691 Practice for Conducting an Interlaboratory Study to
extrusion of molten thermoplastic resins using an extrusion Determine the Precision of a Test Method
plastometer. 2.2 ANSI Standard:
B46.1 on Surface Texture3
Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

1.2 The values stated in SI units are to be regarded as
2.3 ISO Standard:
standard.
ISO 1133 Determination of the Melt-Mass Flow Rate (MFR)
1.3 This standard does not purport to address all of the and the Melt Volume-Flow Rate (MVR) of Thermoplas-
safety concerns, if any, associated with its use. It is the tics3
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 3. Terminology
mine the applicability of regulatory limitations prior to use. 3.1 Terms used in this standard are defined in accordance
NOTE 1—This standard and ISO 1133 address the same subject matter, with Terminology D883, unless otherwise specified. For terms
but differ in technical content. relating to precision and bias and associated issues, the terms
1.4 This international standard was developed in accor- used in this standard are defined in accordance with Terminol-
dance with internationally recognized principles on standard- ogy E456.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4. Summary of Test Method
mendations issued by the World Trade Organization Technical 4.1 After a specified preheating time, resin is extruded
Barriers to Trade (TBT) Committee. through a die with a specified length and orifice diameter under
prescribed conditions of temperature, load, and piston position
2. Referenced Documents in the barrel. Four procedures are described. Comparable
2.1 ASTM Standards:2 results have been obtained by these procedures in interlabora-
D618 Practice for Conditioning Plastics for Testing tory round-robin measurements of several materials and are
D883 Terminology Relating to Plastics described in Section 16.
D3364 Test Method for Flow Rates for Poly(Vinyl Chloride) 4.2 Procedure A is used to determine the melt flow rate
with Molecular Structural Implications (MFR) of a thermoplastic material. The units of measure are
D4000 Classification System for Specifying Plastic Materi- grams of material/10 minutes (g/10 min). It is based on the
als measurement of the mass of material that extrudes from the die
D5947 Test Methods for Physical Dimensions of Solid over a given period of time. It is generally used for materials
Plastics Specimens having melt flow rates that fall between 0.15 and 50 g/10 min
(see Note 2).
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
4.3 Procedure B is an automatically timed measurement
and is the direct responsibility of Subcommittee D20.30 on Thermal Properties used to determine the melt flow rate (MFR) as well as the melt
(Section D20.30.08). volume rate (MVR) of thermoplastic materials. MFR measure-
Current edition approved July 1, 2020. Published August 2020. Originally ments made with Procedure B are reported in g/10 minutes.
approved in 1965. Last previous edition approved in 2013 as D1238 - 13. DOI:
10.1520/D1238-20. MVR measurements are reported in cubic centimeters/ten
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
*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 19428-2959. United States
Copyright by ASTM Int'l (all rights reserved); Tue Nov 10 03:27:02 EST 2020
1
Downloaded/printed by
() pursuant to License Agreement. No further reproductions authorized.
D1238 − 20
minutes (cm3/10 min). Procedure B measurements are based method. Table 1 in Classification D4000 lists the ASTM
on the determination of the volume of material extruded from materials standards that currently exist. An alternative test
the die over a given period of time. The volume is converted to method for poly (vinyl chloride) (PVC) compounds is found in
a mass measurement by multiplying the result by the melt Test Method D3364.
density value for the material (see Note 3). Procedure B is 5.5 Additional characterization of a material can be ob-
generally used with materials having melt flow rates from 0.50 tained if more than one condition is used. In the case that two
to 1500 g/10 min. or more conditions are employed, a Flow Rate Ratio (FRR) is
4.4 Procedure C is an automatically timed measurement obtained by dividing the flow rate at one condition by the flow
used to determine the melt flow rate (MFR) of polyolefin rate at another condition. Procedure D provides one method to
materials. It is generally used as an alternative to Procedure B measure more than one condition in a single charge.
on samples having melt flow rates greater than 75 g/10 min. 5.6 Frequently, variations in test technique, apparatus
Procedure C involves the use of a modified die, commonly geometry, or test conditions, which defy all but the most
referred to as a “half-die,” which has half the height and half careful scrutiny, exist, causing discrepancies in flow rate
the internal diameter of the standard die specified for use in determinations. A troubleshooting guide is found in Appendix
Procedures A and B thus maintaining the same length to X2 and it is a resource to be used to identify sources of test
diameter ratio. The test procedure is similar to Procedure B, but error.
the results obtained with Procedure C shall not be assumed to
be half of those results produced with Procedure B. 6. Apparatus

4.5 Procedure D is a multi-weight test commonly referred to 6.1 Extrusion Plastometer (Alternative Names—Melt
as a “Flow Rate Ratio” (FRR) test. Procedure D is designed to Indexer, Melt Flow Indexer):
allow MFR determinations to be made using two or three
different test loads (either increasing or decreasing the load NOTE 4—Older plastometers that were manufactured in accordance
with “design specifications” detailed in previous revisions of this test
during the test) on one charge of material. The FRR is a method (pre D1238 - 04c) are deemed to be acceptable, as long as they
dimensionless number derived by dividing the MFR at the meet the dimensional and performance specifications stated in this section.
higher test load by the MFR at the lower test load. Results NOTE 5—Relatively minor changes in the design and arrangement of
generated from multi-weight tests shall not be directly com- the component parts have been shown to cause differences in results
pared with results derived from Procedure A or Procedure B. among laboratories. For the best interlaboratory agreement, it is important
that the design adhere closely to the description herein; otherwise, it
NOTE 2—Polymers having melt flow rates less than 0.15 or greater than
should be determined that modifications do not influence the results. Refer
900 g/10 min may be tested by the procedures in this test method;
to Fig. 1.
however, precision data have not been developed.
NOTE 3—Melt density is the density of the material in it molten state. 6.1.1 The apparatus shall be a dead-weight piston plastome-
It is not to be confused with the standard density value of the material. See ter consisting of a thermostatically controlled heated steel
Table 4.
cylinder with a bore that contains a die at the lower end, and a
5. Significance and Use weighted piston operating within the cylinder. The essential
features of the plastometer, illustrated in Figs. 1 and 2, are
5.1 This test method is particularly useful for quality control described in 6.2-6.12. The bore of the extrusion plastometer
tests on thermoplastics. shall be properly aligned in the vertical direction (see Appen-
5.2 The data produced by this test method serves to indicate dix X1). All dimensional measurements shall be made when
the uniformity of the flow rate of the polymer as made by an the article being measured is at 23 6 5°C.
individual process. It is not to be used as an indication of 6.2 Cylinder—The cylinder shall be 50 mm 6 10 mm in
uniformity of other properties without valid correlation with diameter, 115 to 180 mm in length with a smooth, straight bore
data from other tests. 9.5504 6 0.0076 mm in diameter. The cylinder bore shall be
5.3 The flow rate obtained with the extrusion plastometer is manufactured in a way that produces a finish approximately 12
not a fundamental polymer property. It is an empirically rms or better in accordance with ANSI B46.1. Means shall be
defined parameter critically influenced by the physical proper- provided to monitor the temperature inside the bore.
ties and molecular structure of the polymer and the conditions 6.3 Die (Orifice):
of measurement. The rheological characteristics of polymer 6.3.1 Standard Die—The outside diameter of the die shall
melts depend on a number of variables. It is possible that the be such that it will fall freely to the bottom of the hole in the
values of these variables occurring in this test will differ cylinder. The orifice of the die shall have a smooth straight bore
substantially from those in large-scale processes, which would 2.095 6 0.005 mm in diameter and shall be 8.000 6 0.025 mm
result in data that does not correlate directly with processing in length (see Fig. 2). The bore of the orifice and its finish are
behavior. critical. It shall have no visible drill or other tool marks and no
5.4 Measure the flow rate of a material using any of the detectable eccentricity. The bore of the orifice shall be manu-
conditions listed for the material in X4.1. For many materials, factured by techniques known to produce finishes approxi-
there are specifications that require the use of this test method, mately 12 rms or better in accordance with ANSI B46.1.
but with some procedural modifications that take precedence 6.3.2 “Half” Die—Used for Procedure C. When testing
when adhering to the specification. Therefore, it is advisable to polyolefins with a MFR of 75 or greater (using the standard
refer to that material specification before using this test die), an alternate die has shown to improve the reproducibility
2
D1238 − 20

FIG. 1 General Arrangement of Extrusion Plastometer (See Sec-
tion 6.)
FIG. 2 Details of Extrusion Plastometer
of results by reducing the flow rate of these materials. The dimensional checks and visual inspections on the die more often.
outside diameter of the die shall be such that it will fall freely 6.4 Piston:
to the bottom of the hole in the cylinder. The orifice shall have
6.4.1 The piston shall be made of steel. There shall be
a smooth straight bore 1.048 6 0.005 mm in diameter and shall
insulation at the top as a barrier to heat transfer from the piston
be 4.000 6 0.025 mm in length (see Fig. 2A). The bore of the
to the weight. The piston shall be prevented from rubbing on
orifice and its finish are critical. It shall have no visible drill or
the bore. Most commercially available instruments use a loose
other tool marks and no detectable eccentricity. The bore of the
fitting metal guide sleeve, but other methods are acceptable.
orifice shall be manufactured by techniques known to produce
The weight of the sleeve shall not be considered as part of the
finishes approximately 12 rms or better in accordance with
test load. The land (foot) of the piston shall be
ANSI B46.1 (Note Note 6). No spacer shall be used with this
9.4742 6 0.0076 mm in diameter and 6.35 6 0.10 mm in
die.
NOTE 6—Recommended die material is tungsten carbide. Also satisfac- length. Above the land, the piston shall be relieved to ≤ 9.0 mm
tory are steel, synthetic sapphire, and cobalt-chromium-tungsten alloy. in diameter (see Fig. 2). The piston land shall be manufactured
When softer materials are used, it will be necessary to conduct critical by techniques known to produce finishes approximately 12 rms
3
D1238 − 20
in accordance with ANSI B46.1. If corrosion is a problem, the piston movement within the specified travel range. The re-
piston or piston land, if removable, shall be made of corrosion quirements of the automatic timing system shall be as follows:
resistant material. 6.6.1 Sense and indicate the piston travel time within
6.4.2 For procedure A, the piston shall be scribed with two 60.01 s.
reference marks 4 mm apart in such fashion that when the 6.6.2 Measure piston travel within 60.4 % of the nominal
lower mark coincides with the top of the cylinder, guide sleeve selected value (see 11.7) for use in the flow rate calculations.
or other suitable reference point, the bottom of the piston is 48 This requires that the measurement be 6.35 6 0.025 mm or
mm above the top of the die (see Fig. 1) and the timed test run 25.4 6 0.102 mm.
shall start within these two reference marks. The targeted 6.6.3 Operate within a fixed portion of the cylinder. This is
starting point shall be 46 6 2mm above the upper face of the defined as the portion of the cylinder between 48 mm and
die. (see Fig. 1). 18.35 mm above the top of the die.
6.4.3 The combined weight of piston and load shall be 6.6.4 Any effects on the applied load caused by the Timing
within a tolerance of 60.5 % of the selected load. Device/System must be included in the allowable tolerance
6.5 Temperature Control System: given in 6.4.3.
6.5.1 The equipment shall have the capability of heating and 6.6.5 The equipment used to calibrate the Timing Device/
maintaining the temperature inside the bore of the cylinder in System shall be traceable to a national standard (for example,
accordance with the requirements specified in Table 1 through- NIST).
out the duration of the test. 6.7 Operating Tools:
6.5.2 The preferred method for calibrating the temperature

6.7.1 Level—Used to verify the vertical alignment of the
is to use a temperature sensor assembly having a sensor with at bore of the extrusion plastometer. This is necessary to mini-
least an accuracy of 60.08°C at 200°C and a 20 6 0.5-mm mize subtractive loads resulting from rubbing or friction
long brass tip press fit on the end of the sensor. The diameter between the piston tip and sidewall. Means of alignment are
of the brass tip shall closely match the diameter of the die and discussed in Appendix X1.
the length of the active measuring length of the temperature 6.7.2 Go/No-Go Gauge:
sensor (see Appendix X3).
6.7.2.1 For the standard die, a go/no-go gauge suitable to
6.5.3 Temperatures shall be verified with the bottom of the
inspect the inner diameter of the hole in the die. The go
temperature sensor at 10 and 75 6 1 mm above the upper face
member of the gauge shall be no smaller than 2.090 mm. The
of the die and at each test temperature, without touching the
no-go member shall be no larger than 2.100 mm. (See Note 7.)
die. Allow at least four minutes for equilibrium of temperature
6.7.2.2 For the “half” die, a go/no-go gauge suitable to
to be reached for each position. Temperature variation shall be
inspect the hole in the die. The go member of the gauge shall
determined over a minimum of 15 minutes. When using the
be no smaller than 1.043 mm. The no-go member shall be no
“half” die, the temperature indicating device shall be calibrated
larger than 1.053 mm. (See Note 7.)
as stated in Table 1 except temperatures are measured at
79 6 1 mm and 14 6 1 mm above the upper surface of the die. NOTE 7—Frequent use of Go/No-Go Gauges subject them to wear. They
6.5.4 An alternative method is to insert the temperature should be verified routinely.
sensor without a brass tip into the melt from the top of the 6.7.3 Funnel—For charging samples to the cylinder
cylinder so that it is 10 and 75 6 1 mm above the upper face 6.7.4 Packing Tool—For charging samples to the cylinder
of the die. 6.7.5 Spatula—Or similar device used to cut extrudate
6.5.5 The temperature sensor and readout equipment used 6.7.6 Balance—Capable of weighing to 0.001 g
for calibration of the extrusion plastometer shall be traceable to
a national standard (for example, NIST). 6.8 Cleaning Equipment:
6.8.1 Cylinder bore cleaning tool
6.6 Timing Device/System—For Procedure A, a timing de-
6.8.2 Die cleaning tool
vice with an accuracy of 0.1 s shall be used. For Procedures B,
6.8.3 Cotton patches
C, and D, an automatic timing system shall measure and time
6.9 Weight Support—Used with high Melt Flow Rate mate-
rial to prevent material from flowing out during the preheat
period.
TABLE 1 Maximum Allowable Variation in Temperature with
Distance and Time Throughout the Test 6.10 Die Plug—Used with high melt flow rate material to
Test temperature Temperature tolerance, °C plug the die when weight support measures are not enough to
set point prevent material from flowing out during the preheat period.
T °C At 75 ± 1 mm At 10 ± 1 mm
above the die above the die 6.11 Automatic Weight Lowering and Lifting Device—
surface (°C)A surface (°C)A Optional for Procedures A, B, and C, but required for Proce-
125 # T < 250 ±2.0 ±0.2
250 # T < 300 ±2.5 ±0.5
dure D. Device for automatically applying test loads to the
300 # T ±3.0 ±1.0 piston. This device is often useful as a weight support.
A
When using the “half” die, the temperature indicating device shall be calibrated as 6.12 Multi-Weight (Flow Rate Ratio) Accessory—For test-
stated in this table except temperatures are measured at nominal 79 ± 1 mm and
14 mm ± 1mm above the upper surface of the die. ing in accordance with Procedure D, it is necessary to have an
accessory that permits Melt Flow Rate determinations to be
4
D1238 − 20
made using two or three different test loads on one charge of 23 6 5°C) to verify that the die is within the tolerances given
material by loading or unloading test loads, or both, at pre-set in 6.3.1. Visually examine the die bore to verify that it is not
heights. scratched or damaged. Also visually inspect the land of the
NOTE 8—Different manufacturers of equipment may offer options that piston foot to verify that it is not scratched or damaged and use
help to automate the test and/or data collection. These are acceptable for a micrometer to verify that the dimensions are within the
use provided they operate in a manner that does not conflict with
descriptions in Section 6 and the procedures listed in Sections 10, 11, 12,
tolerances given in 6.4.1 (see Note 12).
and 13. NOTE 12—Cleaning and usage will eventually cause damage or wear to
6.13 Micrometer—Apparatus for measuring the dimensions the, bore, die and the land of the piston. Data has shown that erroneous
results will be obtained if these components are not within the appropriate
of the piston foot shall comply with the requirements of Test
tolerances.
Method D5947.
10.4 Set the temperature in accordance with the manufac-
7. Test Specimen turer’s instructions.
7.1 The test specimen is permitted to be in any form that 10.5 Insert the die and the piston into the bore. Allow the
allows it to be introduced into the bore of the cylinder, for temperature of the cylinder, with the piston and die in place, to
example, powder, granules, strips of film, or molded slugs. stabilize within 60.2°C of the selected test temperature for at
NOTE 9—It may be desirable to pre-form or pelletize a powder. Trapped least 15 min before starting a test. When equipment is used
air causes the piston to fall faster, hence measurements are affected.
continuously, it is not necessary to heat the piston and die for
8. Conditioning 15 minutes when runs of the same or similar material at the
same test temperature are being measured over a continuous

8.1 Many thermoplastic materials do not require condition-
time frame, provided the piston and die are cleaned and
ing prior to testing. Some materials that contain volatile
re-inserted into the bore within five minutes after removal from
components, are chemically reactive, or have other special
the extrusion plastometer at the end of each test. If the piston,
characteristics will require appropriate conditioning proce-
or die, or both, are removed from the bore for longer than five
dures. Moisture not only affects reproducibility of flow rate
minutes, they shall be considered “cold” and the full 15
measurement but, in some types of materials, degradation is
minutes heating stabilization time shall be required.
accelerated by moisture at the high temperatures used in
testing. Check the applicable material specification for any 10.6 Remove the piston from the bore (see Note 13). Within
conditioning requirements before using this test. See Practice 60 seconds, charge the cylinder with a weighed portion of the
D618 for appropriate conditioning practices. sample in accordance with the expected flow rate (as given in
Table 2), reinsert the piston and add the appropriate weight.
9. Procedural Conditions The charging weights given in Table 2 are merely suggestions,
9.1 A list of possible test conditions for various materials is and the actual charging weight for a specific sample, if not
shown in Table X4.1 found in Appendix X4. Test conditions known, will need to be determined by trial and error. Adjust the
shall be shown as: Condition _ _ _ / _ _ _, where the charge weight so that the piston is in the proper position at the
temperature in degrees Celsius is shown first, followed by the end of the pre-heat period. If necessary, it is acceptable to
weight in kilograms. For example: Condition 190/2.16.
NOTE 10—Some materials may require special materials of construction TABLE 2 Standard Test Conditions, Sample Mass,A and Testing
or handling for performing this test. Please refer to the material specifi- TimeB
cation for appropriate recommendations. Suggested Mass
Factor for
Flow Range, of Time Inter-
Obtaining Flow
10. Procedure A—Manual Operation g/10 min Sample in val, min
Rate in g/10 min
Cylinder, g
10.1 Select conditions of temperature and load from X4.1 or 0.15 to 1.0 2.5 to 3.0 6.00 1.67
in accordance with material specifications. Where multiple test >1.0 to 3.5 3.0 to 5.0 3.00 3.33
conditions exist, test conditions shall be agreed upon by the >3.5 to 10 4.0 to 8.0 1.00 10.00
>10 to 25 4.0 to 8.0 0.50 20.00
cooperating laboratories. If test conditions are not known, >25 4.0 to 8.0 0.25 40.00
select conditions that result in flow rates between 0.15 to 50 A
This is a suggested mass for materials with melt densities of about 0.7 g/cm3.
g/10 min. Correspondingly, greater quantities are suggested for materials of greater melt
densities. Density of the molten resin (without filler) may be obtained using the
10.2 Inspect the extrusion plastometer for cleanliness (see procedure described by Terry, B. W., and Yang, K., “A New Method for Determining
Note 11). All surfaces of the cylinder bore, die and piston shall Melt Density as a Function of Pressure and Temperature,” SPE Journal , SPEJA,
be free of any residue from previous tests. Vol. 20, No. 6, June 1964, p. 540 or the procedure described by Zoller, Paul, “The
Pressure-Volume-Temperature Properties of Polyolefins,” Journal of Applied Poly-
NOTE 11—The degree of cleanliness can significantly influence the flow mer Science, Vol 23, 1979, p. 1051. It may also be obtained from the weight of an
extruded known volume of resin at the desired temperature. For example, 25.4 mm
rate results, therefore a thorough method of cleaning should be estab-
(1 in.) of piston movement extrudes 1.804 cm3 of resin. An estimate of the density
lished. It has been found that swabbing the barrel with a clean cotton patch of the material can be calculated from the following equation:
several times is satisfactory for most materials and that the die, barrel, and
piston are more easily cleaned while hot. For materials that are difficult to resin density at test temperature 5 M/1.804
clean from the metal surfaces, use of a brass brush has been found to be where:
satisfactory. M = mass of extruded resin.
10.3 Check the die bore diameter at frequent intervals with B
See 10.13.
appropriately sized go/no-go gauge (checked with die at
5
D1238 − 20
purge excess material from the cylinder bore so that the piston period. The individual cuts may give an indication of the presence of
is in the proper position at the end of the pre-heat period. bubbles which may be masked due to their size or to opacity of the sample
which will result in test error. This technique is particularly helpful in the
Purging of material done at conditions with greater force than case of highly pigmented materials.
testing conditions shall be completed at least 2 min prior to
making the initial cut-off (see Note 14). 10.12 Purge the remainder of the sample from the bore and
follow the extrusion plastometer manufacturer’s instructions
NOTE 13—Placing the piston on an insulated surface after removing it for removing the die from the bore. Swab out the cylinder with
from the bore will reduce heat loss. cotton patches and the cylinder bore cleaning tool. Thoroughly
NOTE 14—Material is purged by forcing the piston to a position that
will ensure that subsequent travel of the piston during the remainder of the clean the die and the piston to remove all residues (Note Note
pre-heat period will position the piston at the correct start position. The 18).
material should be allowed to soften and melt before manually purging.
NOTE 18—The die may be cleaned by dissolving the residue in a
NOTE 15—Additional care may be necessary to prevent thermal
solvent. A better method is pyrolytic decomposition of the residue in a
degradation in the extrusion plastometer. This is sometimes done by the
nitrogen atmosphere. Place the die in a tubular combustion furnace or
addition of an appropriate antioxidant. For highly unstable materials, it
other device for heating to 550 6 10°C and clean with a small nitrogen
may be necessary to use alternative techniques as an indication of flow
purge through the die. This method is preferable to flame or solvent
characteristics.
cleaning, being faster than solvent cleaning and less detrimental to the die
10.7 Start the test by initiating the timing device that than an open flame. In certain cases where materials of a given class
monitors the pre-heat period, which is a period of time that having similar flow characteristics are being tested consecutively, interim
die cleaning may be unnecessary. In such cases, however, the effect of
allows the material to soften and begin to melt. The pre-heat cleaning upon flow rate determination must be shown to be negligible if
period shall last for 7.0 6 0.5 min from the completion of the this step is avoided.

charge unless otherwise stated in the materials specification.
10.13 In case a specimen has a flow rate at the borderline of
10.8 For materials with flow rates greater than 10 g/10 min, the ranges in Table 2 and slightly different values are obtained
a weight (and if needed, a piston) support must be used to at different time intervals, the referee value shall be obtained at
prevent the piston from travelling during the pre-heat period in the longer time interval.
order to ensure that there is enough material in the bore to
correctly test the material. The support is to be installed in a 11. Procedure B—Automatically Timed Flow Rate
manner that holds the lower scribe mark of the piston approxi- Measurement
mately 25 mm above the top of the guide bushing or other 11.1 Install/enable the automatic timing device on the ex-
suitable reference mark. Alternatively, it is acceptable for the trusion plastometer.
operator to delay applying the weight to the piston. The support
shall be removed or the weight applied to the piston at such a 11.2 Select conditions of temperature and load from Table
time as to allow the operator to make the initial cut-off within X4.1 or in accordance with material specifications. Where
7 6 0.5 min of the completion of the charge. multiple test conditions exist, test conditions shall be agreed
upon by the cooperating laboratories. A melt density value (see
NOTE 16—It has been found that the effect of supporting the weight is Table 2 and Table 3) for the material is required if MFR is to
significant to the flow rate results. The choice of piston support was made be calculated from the results.
to cover all conditions and flow rates 10 to 50 g/10 min. Piston/weight
supports will vary between extrusion plastometer manufacturers. 11.3 Inspect the extrusion plastometer for cleanliness (see
10.9 At the end of the pre-heat period and when the top Note 18). All surfaces of the cylinder bore, die and piston shall
scribe mark on the piston is visible above the cylinder (or top be free of any residue from previous tests.
of the guide sleeve) and the lower scribe mark is in the cylinder 11.4 Check the die bore diameter at frequent intervals with
(or below the top of the guide sleeve) indicating that the piston appropriately sized go/no-go gauge (checked with die at
land is 46 6 2 mm from the top of the die, reset the timer to 23 6 5°C) to verify that the die is within the tolerances given
zero then simultaneously make the initial cut-off. Discard the in 6.3. Visually examine the die bore to verify that it is not
extrudate from the pre-heat period. Make the final cut-off scratched or damaged. Also visually inspect the land of the
exactly when the time interval selected (see Table 2) is reached.
Collect and weigh the extrudate specimen. If the extrudate
specimen contains visible bubbles, discard it and begin the test TABLE 3 Factors for Calculation of Flow Rate
again. If the initial cut-off was initiated outside of the toler- Factor for
ances of the pre-heat period or the piston position Material Tempera- Piston Travel, Calculation of
(Unpigmented) ture, °C L, cm (in.) Flow
requirements, discard the specimen and repeat the test with Rate, FA
readjusted piston position after the initial purge, or change the Polyethylene 190 2.54 (1) 826
weight. Polyethylene 190 0.635 (0.25) 207
Polypropylene 230 2.54 (1) 799
10.10 Once the extrudate is cool, weigh to the nearest 1 mg. Polypropylene 230 0.635 (0.25) 200
A
10.11 Multiply the weight of the extrudate by the appropri- Factors calculated using melt-density values of 0.7636 g/cm3 for polyethylene
and 0.7386 g/cm3 for polypropylene, as expressed in article by Zoller, Paul, “The
ate factor shown in Table 2 to obtain the flow rate in grams per Pressure-Volume-Temperature Properties of Polyolefins,” Journal of Applied Poly-
10 min. mer Science, Vol 23, 1979, P. 1051. The base densities at 23°C for which the melt
densities are reported were 0.917 g/cm3 for annealed low-density polyethylene
NOTE 17—Some labs have found it helpful to take interim cuts of the and polypropylene homopolymer.
extrudate at uniform time intervals during the specified extrusion time
6
D1238 − 20
piston foot to verify that it is not scratched or damaged and use manner that holds the lower scribe mark of the piston approxi-
a micrometer to verify that the dimensions are within the mately 25 mm above the top of the guide bushing or other
tolerances given in 6.4.1 (see Note 12). suitable reference mark. Alternatively, it is acceptable for the
11.5 Set the temperature in accordance with the manufac- operator to delay applying the weight to the piston. The support
turer’s instructions. shall be removed, or the weight applied to the piston at such a
time as to allow the measurement to start within 7 6 0.5 min of
11.6 Insert the die and the piston into the bore. Allow the the completion of the charge. (For automated weight lowering
temperature of the cylinder with the piston and die in place to systems, the bottom of the piston foot is held at approximately
stabilize within 60.2°C of the selected test temperature for at 71 mm above the top of the die.)
least 15 min before starting a test. When equipment is used
11.11 For materials greater than 50 g/10 min, use of a die
plug is an option in addition to the piston/weight support. The
15 minutes when runs of the same or similar material at the
die plug is inserted before charge and is removed prior to
same test temperature are being measured over a continuous
removing the piston/weight support. (Warning—Rapid expul-
time frame, provided the piston and die are cleaned and
sion of material when die plug is removed is hazardous.)
re-inserted into the bore within five minutes after removal from
the extrusion plastometer at the end of each test. If the piston, 11.12 At the end of the pre-heat period and when automatic
or die, or both, are removed from the bore for longer than five timing system senses that the piston has reached the pre-
minutes, they shall be considered “cold” and the full 15 selected starting point (indicating that the piston land is 46 6 2
minutes heating stabilization time shall be required. mm from the top of the die), the automatic timing system shall

begin measuring the time it takes for the piston to travel the
11.7 Adjust the automatic timing system to operate within
pre-selected distance (see 11.7). If the extrudate specimen
the 6.35 6 0.25 mm measuring range for materials with
contains visible bubbles, discard the results and begin the test
expected melt flow rates of up to 10 g/10 min, or 25.40 6 0.25
again (see Note 14). If the initial timed measurement was
mm measuring range for materials with expected melt flow
initiated outside of the tolerances of the pre-heat period or the
rates of 10 g/10 min or higher and set to begin timing when the
piston position requirements, discard the results and repeat the
bottom of the piston foot is 46 6 2 mm above the top of the
test after readjusting the piston position after the initial purge
die.
or changing the charge weight.
NOTE 19—It has been found that for some materials the melt flow rates 11.13 Record the time to the nearest 0.01 s for the piston to
obtained on a material will be different depending on which travel length
is chosen; therefore, it is important to use the same measurement range to complete the selected distance of travel.
compare interlaboratory results. 11.14 Purge the remainder of the sample from the bore and
11.8 Remove the piston from the bore (see Note 13). Within follow the extrusion plastometer manufacturer’s instructions
60 seconds, charge the cylinder with a weighed portion of the for removing the die from the bore. Swab out the cylinder with
sample in accordance with the expected flow rate (as given in cotton patches and the cylinder bore cleaning tool. Thoroughly
Table 2), reinsert the piston and add the appropriate weight. clean the die and the piston to remove all residues (see Note
The charging weights given in Table 2 are merely suggestions, 11).
and the actual charging weight for a specific sample, if not
12. Procedure C—Automatically Timed Flow Rate
known, will need to be determined by trial and error. Adjust the
Measurement for High Flow Rate Polyolefins Using
charge weight so that the piston is in the proper position at the
“Half” Die
end of the pre-heat period. If necessary, it is acceptable to
purge excess material from the cylinder bore so that the piston 12.1 Procedure:
is in the proper position at the end of the pre-heat period. 12.1.1 Install/enable the automatic timing device on the
Purging of material done at conditions with greater force than extrusion plastometer.
testing conditions shall be completed at least 2 min prior to the 12.1.2 Select conditions of temperature and load from X4.1
expiration of the preheat period (see Note 14). or in accordance with material specifications. Where multiple
test conditions exist, test conditions shall be agreed upon by the
11.9 Start the test by initiating the timing device that cooperating laboratories. A melt density value (not bulk den-
monitors the pre-heat period, which is a period of time that sity) for the material is required if MFR is to be calculated from
allows the material to soften and begin to melt. The pre-heat the results.
period shall last for 7.0 6 0.5 min from the completion of the 12.1.3 Use the procedure described in 11.3 – 11.14with the
charge unless otherwise stated in the materials specification. following exceptions:
11.10 For materials with flow rates greater than 10 g/10 12.1.3.1 Use the “half” die as described in 6.3.2.
min, a weight (and if needed, a piston) support must be used to 12.1.3.2 Adjust the timing device to operate within the
prevent the piston from travelling during the pre-heat period in 25.40 6 0.25 mm measuring range and set to begin timing
order to ensure that there is enough material in the bore to when the bottom of the piston foot is 50 6 2 mm above the top
correctly test the material. The support is to be installed in a of the die.
7
D1238 − 20
13. Procedure D—Multi-Weight Using Automatically 13.1.10 Some materials, particularly those with expected
Timed Flow Rate Measurement melt flow rates less than 10g/10 min during the first measure-
13.1 Procedure: ment period require the operator to purge some material to a
13.1.1 Install/enable the automatic timing device, automatic position that insures subsequent travel of the piston will
weight lifting/lowering device and multi-weight (FRR) acces- activate the timing device at the desired starting point for the
sory on the extrusion plastometer. The multi-weight test shall first measurement within 7.0 6 0.5 min after the completion of
be made in either increasing weight or decreasing weight the charge. The lower scribe mark of the piston shall be at least
conditions. Follow the equipment manufacturer’s instructions 25 mm above the top of the cylinder after purging. Any purging
for installation and operation. must be completed at least 2 min prior to start of the test Melt
13.1.2 Configure the multi-weight (FRR) accessory to take Flow Rates.
at least two MFR determinations at each load condition used 13.1.11 Materials with higher expected flow rates will
before changing to the next test load. After switching load require that the weight and piston support be used after
conditions, achieve stable flow by allowing sufficient piston charging the material. For Procedure D, this can be accom-
travel or time to elapse before beginning measurements (see plished with the automatic weight lifting/lowering device. The
Note 20). Piston travel distances shall be chosen so that at least support shall be removed at such a time as to allow the
2 seconds elapse during the measurement and that the distances automatic timing device to activate at the starting point for the
are determined within 60.4 %. first measurement within 7.0 6 0.5 min after the completion of
the charge. Only use the piston support if there is excessive
NOTE 20—Normally, 5 mm of piston travel or 2 min is sufficient to material flow (see Note 16).

obtain stable flow after changing test loads.
13.1.12 If a die plug is used to prevent excessive leakage
13.1.3 Adjust the automatic timing device to make multiple before the test, for materials with a melt flow rate greater than
test measurements as required and set to begin timing the first 50 g/10 min, then the die plug is to be inserted before the
measurement when the bottom of the piston foot is 46 6 2 mm charge and removed prior to removing the piston/weight
above the top of the die. Do not take readings below 18.35 mm support. The initial charge shall be adjusted to ensure appro-
above the top of the die. priate measurement loads based on suggestions in Table 2. If
13.1.4 Inspect the extrusion plastometer for cleanliness (see the timer is not activated within 7 6 0.5 min after the
Note 11). All surfaces of the cylinder bore, die and piston shall completion of the charge the test must be repeated with
be free of any residue from previous tests. readjusted charge weights.
13.1.5 Check the die bore diameter at frequent intervals
13.1.13 Record the time, to the nearest 0.01 s, for the
with appropriately sized go/no-go gauge (checked with die at
individual piston travel determinations measured for each test
23 6 5°C) to verify that the die is within the tolerances given
load.
in 6.3.1. Visually examine the die bore to verify that it is not
13.1.14 Repeat the above for any additional test loads.
scratched or damaged. Also visually inspect the land of the
piston foot to verify that it is not scratched or damaged and use 13.1.15 Purge the remainder of the sample from the bore
a micrometer to verify that the dimensions are within the and follow the extrusion plastometer manufacturer’s instruc-
tolerances given in 6.4.1 (see Note 12). tions for removing the die from the bore. Swab out the cylinder
13.1.6 Set the temperature in accordance with the manufac- with cotton patches and the cylinder bore cleaning tool.
turer’s instructions. Thoroughly clean the die and the piston to remove all residues
13.1.7 A melt density value (see Table 2) for the material is (see Note 11).
required in order to calculate MFR for the individual determi-
nations. 14. Calculation of Flow Rate
13.1.8 Insert the die and the piston into the bore. Allow the 14.1 Calculation for Procedures B and C:
temperature of the cylinder with the piston and die in place to 14.1.1 Calculate the flow rate in grams per 10 min or
stabilize within 60.2°C of the selected test temperature for at volume rate in cm3 per 10 min as follows (see Note 21):
least 15 min before starting a test. When equipment is used
Melt flow rate 5 ~ 426 3 L 3 d ! /t
or
15 minutes when runs of the same or similar material at the
same test temperature are being measured over a continuous Melt volume rate 5 426 3 L/t
time frame, provided the piston and die are cleaned and where:
re-inserted into the bore within five minutes after removal from L = length, cm, of calibrated piston travel,
the extrusion plastometer at the end of each test. If the piston d = melt density of resin, g/cm3, at test temperature, (see
and/or die are removed from the bore for longer than five reference under Table 2 and Table 3),
minutes, they shall be considered “cold” and the full 15 t = time, seconds, of piston travel for length L, and
minutes heating stabilization time shall be required. 426 = mean of areas, cm2, of piston and cylinder × 600.
13.1.9 Remove the piston from the bore (see Note 13). NOTE 21—Factors that may be substituted in the following equation are
Within 60 seconds, charge the cylinder with a weighed portion given for some materials in Table 3.
of the sample in accordance with the expected melt flow rate
Flow rate, g/10min 5 F/t
(as given in Table 2), reinsert the piston and use the weight
lifting and lowering device to add the test load to the piston. where:
8
D1238 − 20
F = factor from Table 3, and 15.1.5 Any unusual behavior of the test specimen such as
t = time, seconds, of piston travel for length L. discoloration, sticking, extrudate surface irregularity or
roughness, etc.
14.1.2 Improved agreement between Procedures A and au-
15.1.6 Details of conditioning, if any.
tomatically timed flow measurements (Procedures B, C, and D)
15.1.7 For multi-weight tests using Procedure D, also re-
is obtained if an average melt density for a particular type of
port:
material is determined with the actual equipment used and that
15.1.7.1 The average flow rate at each test load.
value is substituted into the equation given in 14.1.1.
15.1.7.2 The Flow Rate Ratio (FRR) together with the
14.2 Calculation for Procedure D: temperature and loads used (for example, FRR-190/21.6/2.16).
14.2.1 Calculate the MFR for each capture at each test load 15.1.7.3 Whether the decreasing or increasing load tech-
in accordance with Section 11 (Procedure B). nique was used.
14.2.2 If the differences between the individual melt flow
rates at each test load are no greater than 63 %, calculate the 16. Precision and Bias (Procedures A, B, and C)
average Melt Flow Rate for each test load. If differences are > 16.1 Precision:
63 % repeat the test. 16.1.1 The precision of this test method is based on a series
NOTE 22—To achieve stable flow after applying each test load, it may of interlaboratory studies of this standard conducted over
be necessary to increase the time or the piston travel distance before taking several years.
a measurement. 16.1.2 Tables 4 and 5 are based on a round robin4 conducted
14.2.3 Calculate the Flow Rate Ratio (FRR) as the ratio of in 1986 and 1987, involving polypropylene, polyethylene,

the average flow rate at the higher load to the average flow rate polystyrene, polycarbonate and acrylic materials. Tables 6 and
at the lower load. 7 are based on a round robin5 completed in 1997 involving low
and high density polyethylene, polypropylene, polystyrene,
15. Report polycarbonate, PMMA, and acetal. The number of participat-
15.1 Report the following information: ing laboratories is shown for each material. Data for Tables 4
15.1.1 Statement indicating the nature and physical form of and 5 were generated through each lab testing two specimens
the material charged to the cylinder. for each material on three different days, while data for Tables
15.1.2 Temperature and load at which the test is run shall be 6 and 7 were generated through each lab testing two specimens
reported. The results and test conditions, along with an for each material on two different days. Practice E691 was
indication of which procedure was used (for example, Proce- followed for the design and analysis of the data; the details are
dure C-190/2.16) shall be documented. Reference shall be given in ASTM Research Report No. D20 -1226 for Table 6.
made to this test method. 16.1.3 Table 8 is based on a round robin6 conducted in 1980
using Procedure B. Four polypropylene samples having flow
NOTE 23—It has become customary to refer to the flow rate of rates from 250 to 1500 were tested in nine laboratories.
polyethylene as “melt index” when obtained under Condition 190/2.16.
However, for all other materials the use of melt index or any term other
than “melt flow rate” is discouraged, regardless of the condition used. 4
Supporting data are available from ASTM Headquarters. Request RR:D20-
15.1.3 Melt flow rate reported as the rate of extrusion in 1164.
5
grams per 10 min or volume rate in cm3 per 10 min. Data shall
1226.
be reported to at least three significant figures. 6
15.1.4 Procedure used (A, B, C, or D). 1124.
TABLE 4 Precision, Procedure A (Values in g/10 min)

Ir as % of IR as % of Number of
Material Condition Average SrA SRB IrC IRD
mean mean Laboratories
Polyethylene 190/2.16 0.27 0.008 0.022 0.023 0.063 8.52 23.33 9
Polyethylene 190/2.16 0.4 0.012 0.038 0.035 0.108 8.75 27.00 9
Polyethylene 190/2.16 2.04 0.026 0.079 0.073 0.224 3.58 10.98 9
Polyethylene 190/2.16 44.1 0.919 1.232 2.56 3.486 5.80 7.90 7
Polypropylene 230/2.16 2.23 0.106 0.226 0.299 0.639 13.41 28.65 9
Polypropylene 230/2.16 7.09 0.222 0.471 0.627 1.331 8.84 18.77 9
Polypropylene 230/2.16 32.8 0.581 1.051 1.644 2.974 5.01 9.07 9
Polystyrene 200/5 1.67 0.024 0.122 0.068 0.344 4.07 20.60 6
Polystyrene 200/5 8.82 0.19 0.667 0.538 1.886 6.10 21.38 6
Polystyrene 200/5 13.3 0.305 0.925 0.864 2.617 6.50 19.68 6
Polycarbonate 300/1.2 2.41 0.076 0.115 0.215 0.326 8.92 13.53 4
Polycarbonate 300/1.2 10.5 0.429 0.647 1.215 1.83 11.57 17.43 4
Polycarbonate 300/1.2 16.2 0.155 1.109 0.438 3.14 2.70 19.38 4
Acrylic 230/3.8 2.59 0.051 0.051 0.145 0.145 5.60 5.60 3
A
S r = within-laboratory standard deviation of the average.
B
SR = between-laboratories standard deviation of the average.
C
Ir = 2.83Sr, and
D
IR = 2.83SR.
9
D1238 − 20
TABLE 5 Precision, Procedure B (Values in g/10 min)
mean mean Laboratories
Polyethylene 190/2.16 0.27 0.009 0.014 0.026 0.039 9.63 14.44 8
Polyethylene 190/2.16 0.4 0.016 0.027 0.045 0.076 11.25 19.00 8
Polyethylene 190/2.16 2.04 0.04 0.094 0.112 0.266 5.49 13.04 9
Polyethylene 190/2.16 43.7 0.997 1.924 2.819 5.443 6.45 12.46 8
Polypropylene 230/2.16 2.25 0.052 0.214 0.1466 0.604 6.52 26.84 8
Polypropylene 230/2.16 7.16 0.143 0.589 0.4051 1.666 5.66 23.27 8
Polypropylene 230/2.16 32.6 0.693 0.945 1.959 2.672 6.01 8.20 8
Polystyrene 200/5 1.65 0.037 0.166 0.106 0.47 6.42 28.48 4
Polystyrene 200/5 8.39 0.144 0.423 0.406 1.197 4.84 14.27 4
Polystyrene 200/5 13 0.108 0.387 0.306 1.097 2.35 8.44 4
A
B
C
Ir = 2.83 Sr, and
D
IR = 2.83SR.

Material Condition Average SrA SRB rC RD
mean mean Labs
Acrylic 230/3.8 1.51 0.013 0.086 0.037 0.242 2.45 16.03 7

LDPE 190/2.16 1.74 0.027 0.052 0.075 0.144 4.31 8.28 11
Polystyrene 200/5.0 1.86 0.04 0.085 0.112 0.238 6.02 12.80 9
HDPE 190/2.16 5.35 0.049 0.103 0.137 0.288 2.56 5.38 11
Polypropylene 230/2.16 10.94 0.088 0.473 0.247 1.324 2.26 12.10 10
Polycarbonate 300/1.2 13.59 0.109 0.233 0.305 0.653 2.24 4.81 4E
Acetal 190/2.16 25.3 0.235 0.571 0.658 1.599 2.60 6.32 7
A
B
C
r = 2.83 Sr.
D
R = 2.83SR.
E
Insufficient laboratories to meet Practice E691.

Material Condition Average SrA SRB rC RD
mean mean Labs
Acrylic 230/3.8 1.54 0.026 0.102 0.072 0.286 4.68 18.57 6
LDPE 190/2.16 1.76 0.015 0.053 0.042 0.149 2.39 8.47 11
Polystyrene 200/5.0 1.89 0.042 0.102 0.117 0.285 6.19 15.08 7
HDPE 190/2.16 5.41 0.041 0.113 0.114 0.316 2.11 5.84 10
Polypropylene 230/2.16 10.96 0.357 0.491 0.999 1.376 9.11 12.55 10
Polycarbonate 300/1.2 13.79 0.104 0.477 0.292 1.335 2.12 9.68 3E
Acetal 190/2.16 25.64 0.182 0.822 0.508 2.302 1.98 8.98 6
A
B
C
r = 2.83 Sr.
D
R = 2.83 SR.
E
Insufficient laboratories to meet Practice E691.
Practice E691 was followed for the design and analysis of the and polyethersulfone materials. The number of participating
data; the details are given in ASTM Research Report No. D20 laboratories is shown for each material. Data for Tables 10 and
-1124. 11 were generated through each lab testing three test samples
16.1.4 Table 9 is based on a round robin conducted in 1999 for a given material, that is, reporting in triplicate, using
on Procedure C. Eight laboratories tested four different poly- Procedure A and Procedure B, respectively. The analysis in
ethylene materials with melt flow rates using the standard die Practice E691 is based on a test result being the average of
ranging from approximately 35 to 2350 g/10 min using the three samples. IR is also reported as a % of the Average,
“half-die” die. specifically looking at standard deviations as a percentage of
16.1.5 Tables 10 and 11 are based on a round robin7 the averages.
conducted in 2019, involving polysulfone, polyphenylsulfone
16.1.6 Warning—The data in Tables 4-11 shall not be
7
rigorously applied to acceptance or rejection of material, as
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D20-2000. Contact ASTM Customer those data are specific to the interlaboratory study and are not
Service at service@astm.org. necessarily representative of other lots, conditions, materials,
10
D1238 − 20
Material Condition Average SrA SRB IrC IRD Ir as % of mean IR as % of mean
Polypropylene 230/2.16 245 13.2 16.6 37.4 46.9 15.3 19.1
Polypropylene 230/2.16 482 31.8 40 89.9 113 18.7 23.4
Polypropylene 230/2.16 837 20.9 58.6 59.1 166 7.1 19.8
Polypropylene 230/2.16 1603 129 243 365 688 22.8 42.9
A
Sr = within-laboratory standard deviation of the average.
B
C
Ir= 2.83Sr,and
D
IR= 2.83SR.
TABLE 9 Precision Data for High Melt Flow Polyolefins Procedure C (Values in g/10 min)A
Materials Average Sr SR r R Ir as % of IR as % of
mean mean
PE-A (35) 4.67 0.068 0.119 0.191 0.334 4.09 7.15
PE-B (185) 24.3 0.688 1.168 1.928 3.27 7.93 13.46
PE-C (2350) 315.7 10.81 19.89 30.27 55.69 9.59 17.64
PE-D (122) 16.2 0.188 0.348 0.526 0.975 3.25 6.02
A
This data was generated with dies having a nominal length of 3.985 mm versus the required 4.000 mm.

Average Average Laboratories
Polysulfone 343/2.16 5.335 0.076 0.221 0.216 0.625 4.0 11.7 8
Polysulfone 343/2.16 6.210 0.056 0.317 0.160 0.896 2.6 14.4 8
Polyphenylsulfone 365/5.0 13.131 0.325 1.032 0.920 2.921 7.0 22.2 8
Polyethersulfone 380/2.16 13.228 0.382 1.211 1.082 3.426 8.2 25.9 8
A
S r=within-laboratory standard deviation of the average.
B
SR=between-laboratory standard deviation of the average.
C
Ir= 2.83Sr,and
D
IR= 2.83SR.

Average Average Laboratories
Polysulfone 343/2.16 5.320 0.057 0.308 0.160 0.871 3.0 16.4 8
Polysulfone 343/2.16 6.163 0.070 0.461 0.199 1.304 3.2 21.2 8
A
S r=within-laboratory standard deviation of the average.
B
SR=between-laboratory standard deviation of the average.
C
Ir= 2.83Sr,and
D
IR= 2.83SR.
or laboratories. Users of this test method shall apply the 17.1.2 The degree of precision is quite high for all levels of
principles outlined in Practice E691 to generate data specific to loads on the ram. The highest level of precision was attained
their laboratory and materials, or between specific laboratories. for the 2.16 kg load, the lowest for the 21.6 kg load. It is
16.2 Bias—There are no recognized standards by which to important to note that the 21.6 kg load is not optimum for the
estimate bias of this test method. standard (8.00 mm) die because the speed of testing does not
allow for the flow to reach probably equilibrium rate. Refer to
17. Precision and Bias (Procedure D) Table 12 for 2.16 kg load; Table 13 for 5 kg load; Table 14 for
17.1 Precision 10 kg load and Table 15 for 21.6 kg load.
17.1.1 Procedure D used as many as nine laboratories, five
materials and two determinations in order to come up with the 18. Keywords
following tables of precision supporting the method. This 18.1 melt flow rate; melt index; volume flow rate
meets or exceeds all the standards required for Practice E691.
11
D1238 − 20
TABLE 12 Precision Statement for Procedure D: 2.16 kg
Average Average
PE1 0.7567 0.0079 0.0323 0.022 0.0904 2.91 11.95
PE2 0.4298 0.006 0.0277 0.0168 0.0776 3.91 18.05
PE3 0.5527 0.0096 0.0179 0.0268 0.0502 4.85 9.08
PE4 0.2627 0.0043 0.0182 0.012 0.0511 4.57 19.45
PE5 0.4104 0.0079 0.0119 0.0222 0.0334 5.41 8.14
TABLE 13 Precision Statement for Procedure D: 5 kg

Average Average
PE1 3.0561 0.7715 0.7809 2.1602 2.1865 70.68 71.55
PE2 1.996 0.0483 0.0927 0.1353 0.2595 6.78 13.00
PE3 1.5821 0.026 0.0462 0.0729 0.1293 4.61 8.17
PE4 0.9976 0.2158 0.256 0.6042 0.7168 60.57 71.85
PE5 1.2308 0.017 0.0285 0.0475 0.0798 3.86 6.48
TABLE 14 Precision Statement for Procedure D: 10 kg


Average Average
PE1 11.6841 0.3065 0.4595 0.8581 1.2867 7.34 11.01
PE2 7.5768 0.1266 0.2751 0.3544 0.7704 4.68 10.17
PE3 4.1181 0.0535 0.1036 0.1497 0.2902 3.64 7.05
PE4 3.7693 0.0538 0.1125 0.1507 0.3151 4.00 8.36
PE5 3.3471 0.0228 0.0647 0.0638 0.1812 1.91 5.41
TABLE 15 Precision Statement for Procedure D: 21.6 kg

Average Average
PE1 59.9335 2.1012 2.7667 5.8833 7.7469 9.82 12.93
PE2 36.2367 1.445 1.445 4.0459 4.0459 11.17 11.17
PE3 14.1078 0.1662 0.3352 0.4653 0.9387 3.30 6.65
PE4 17.6132 0.3324 0.4258 0.9308 1.1924 5.28 6.77
PE5 12.2652 0.1104 0.459 0.309 1.2851 2.52 10.48
APPENDIXES
(Nonmandatory Information)
X1. EXTRUSION PLASTOMETER BORE ALIGNMENT
X1.1 A fixture consisting of a circular level mounted on a insertion into the bore may also be satisfactory. A circular level
shaft having two bearing points 9.48 6 0.01 mm in diameter having a sensitivity of 20 min/2.5 mm has been found
that can be inserted into the bore has been found suitable. A satisfactory. Other alignment techniques that give comparable
circular level that can be rigidly mounted on the piston rod for alignment sensitivity would be considered satisfactory.
12
D1238 − 20
X2. TROUBLESHOOTING GUIDE
INTRODUCTION
This appendix is offered in an effort to help a laboratory improve melt flow rate testing and to get
to the root cause of problems which may be caused by equipment, environment, or testing technique.
This guide is not meant to be an all-inclusive trouble-shooting check list, but merely tries to help users
to evaluate testing to some degree.
X2.1 Basic Programs (3) When a problem arises, the following questions should
X2.1.1 The following are basic programs in which all be asked:
laboratories should participate: (a) Did anything unusual happen?
(b) Does the extrudate contain air bubbles?
X2.1.1.1 Certified Reference Materials (CRMs) and Refer-
(c) Were the proper weights applied?
ence Materials (RMs)—If available, CRMs and RMs can be
(d) Is the unit at the proper temperature?
obtained from national metrological institutes or companies.
(e) Was the piston stored in the barrel?
These materials provide accurate information on the melt flow
(f) Is the die damaged, that is, chipped?
rate, but can be expensive and are available for a very limited
(g) Is the die bore worn, that is, the diameter is larger than
number of materials.

the maximum specified?
X2.1.1.2 Internal Controls—An internal control for each (h) Was the proper amount of material used?
type of material should be set up. This involves setting aside (i) Has the balance been properly calibrated?
enough material to last a long time (at least one year). These (j) Was the proper purge time used?
materials will have to be tested many times to establish (k) Was the plug pulled at the proper time?
statistical parameters. Each time an internal standard is run, the (l) Was the correct warm-up time used?
results should be plotted on a SQC chart so that any problems (m) Was the barrel cleaned properly?
or trends can be detected quickly. A SQC chart should be set up (n) Is the piston rod straight?
for each extrusion plastometer in the laboratory. A replacement (o) Is the piston tip diameter OK?
standard should be introduced before the old standard runs out
and should be compared to the old standard to ensure that any
X2.2 Understanding How Melt Flow Rate is Affected
shifts seen in the SQC chart are due to the material and not to
the equipment. X2.2.1 Levelness of the Instrument—The piston must be
X2.1.1.3 Proficiency Tests—Participation in proficiency test free to move in a vertical position. If the instrument is not level,
programs is important for demonstrating how the laboratory’s the piston can be slowed by friction as it touches the side of the
results compare with other laboratories. Over a period of time, barrel. This will not only introduce an error into the results but
laboratory bias can be demonstrated, if bias exists. may also scratch the barrel. The piston must move in an exact
X2.1.1.4 ASTM Round Robins (Interlaboratory Tests)— vertical plane, indicated by a small bubble level that should be
These programs are similar to proficiency test programs but are placed on the top of the barrel or on the top of the piston when
limited to only a few laboratories and a few materials. placed in the barrel. The level should be checked on a regular
However, these programs do provide information on how well schedule.
the laboratory performs the test. X2.2.2 Die Orifice Diameter—An undersized die orifice
X2.1.1.5 Calibration, Verification, and Maintenance—The (which can result from a buildup of residue) will cause low
extrusion plastometer should be calibrated. Proper mainte- results. Conversely, an oversized orifice (which can result from
nance of the instrument will help to ensure proper calibration. wear) will cause high results. It is important that the die orifice
(1) As a first step to obtaining reproducible results, opera- be cleaned after each test and that the die orifice diameter be
tors should be well trained. Using internal standards can verified frequently using a go/no-go gauge. Remember, the pin
demonstrate that repeatable results can be provided. The gauge can also wear and the diameter should be verified
operators should also understand the test and know what can regularly.
affect the results.
X2.2.3 Die Cleanliness—The die should be completely
(2) Before starting the test, the following should be veri-
cleaned after each test. Any residue left in the orifice will
fied:
eventually char and be very difficult, if not impossible, to
(a) The protocol is understood by the operator.
clean. Buildup of material will reduce the diameter of the die
(b) The barrel, piston, and die orifice have been properly
and change the surface smoothness, resulting in erroneous
cleaned.
results.
(c) The extrusion plastometer, including the piston and
die, are at equilibrium at the proper temperature. X2.2.4 Temperature in the Barrel—Melt flow rates are very
(d) The extrusion plastometer is level. dependent on temperature. The temperature within the barrel is
(e) A standard has been run and the results fall within the only important temperature. Temperature indicators must
established parameters. be calibrated to the temperature within the barrel. High flow
13
D1238 − 20
rates will result from high temperatures and low flow rates X2.2.10 Sample Purge Time—Purging material from the
from low temperatures. Defective heaters may be difficult to barrel before the actual test starts serves two primary functions:
detect and can cause variable results. (1) to expel entrapped air or volatiles before applying the full
test load, and (2) to move the lower scribe mark on the piston
X2.2.5 Preheat Time—Proper preheat time is required to
to the reference start position. For flow rate consistency, it is
allow the material in the barrel to fully melt and to come to
important that the extrudate be free of voids and that the test
temperature equilibrium throughout the barrel. If material is
always starts with the piston in the same position in the barrel.
not fully melted, die plugging and low melt flow rates can
Whether in the extrudate for Procedure A or in the barrel for
result. If not at temperature equilibrium, the melt flow rate will
Procedure B, voids will affect test results.
change as the test is conducted.
X2.2.5.1 It is important that the die and piston be at X2.2.11 Load Weight—The actual weight (load) applied to
temperature equilibrium with the rest of the system before any the material during the test will affect the test results. Higher
sample is introduced into the barrel. If the piston and die are weights will produce higher results. The load weight, which
not at temperature, the large mass of metal involved must be includes the piston weight, should be verified at regular
heated to temperature during testing and the energy required intervals.
may not allow the polymer to reach thermal equilibrium. This X2.2.12 Extrudate Cut Technique—It is important that good
can result in erroneous data. extrudate cutting technique be developed. A sharp, clean tool
should always be used for this operation. The timing of the cut
X2.2.6 Barrel Condition—The barrel should be properly
is critical since a shorter than target cut time will produce low
cleaned after each test. Failure to do so can result in contami-
results and a longer than target cut time will give high results.

nation of the next sample, and buildup and degradation of
The timing intervals should be verified with certified timers.
material in the barrel, resulting in a decrease in the diameter of
When cut, the extrudate end should not be ragged or stringy.
the barrel. This can cause friction with the piston tip resulting
These variables, if not controlled, can cause poor reproducibil-
in low melt flow rates.
ity of test results.
X2.2.6.1 Frequently overlooked is the condition of the
barrel itself. In addition to being clean, the barrel wall must be X2.2.13 Purging—Purging the barrel between runs or when
smooth and of the proper diameter. The inside diameter of the changing materials is sometimes necessary. Purging with the
barrel is as important as the diameter of the die orifice. The same material which will be tested after the purge is best.
barrel diameter should be measured regularly, and changed if However, if for some reason another purge material is used, run
so indicated. The melt flow rate is a function of the fourth the test material through the barrel before the actual test run in
power of the barrel diameter. order to ensure that the purge material is no longer in the barrel.
X2.2.13.1 Purging does not replace cleaning. After purging,
X2.2.7 Piston Parameters—The diameter of the piston foot the equipment must be cleaned properly to avoid the effects of
should be checked. If it is worn, material can flow back past the contamination, resin buildup, and so forth, as discussed previ-
tip. This would result in erroneous data. ously.
X2.2.7.1 The piston tip, or foot, is sometimes screwed into X2.2.14 Melt Density—It is important that the correct melt
the end of the piston and can be changed easily. However, density be used, that is, 0.7636 g/cm3 for PE at 190°C and
because it is easily unscrewed, it can work itself loose. The 0.7386 g/cm3 for PP at 230°C. These values may be different
piston tip must be checked frequently and kept tightly screwed for copolymers or when additives are incorporated into the
into the piston. resin. Small errors in these values can affect the end results. If
X2.2.7.2 Care must be taken not to bend a piston. Even a not known, the melt density can be determined as described at
slight, almost non-detectable curvature in the piston can result the end of Footnote A of Table 2.
in the force not being applied directly to the vertical position,
X2.2.15 Piston (Flag) Travel Distance—The setting of the
resulting in excessive pressure on the wall of the barrel. This
proper piston travel distance (6.35 6 0.25 mm for MFRs up to
will cause low results and can also scratch the barrel wall.
10 g/10 min and 25.40 6 0.25 mm for MFRs greater than 10
X2.2.7.3 The piston has two reference marks. The lower g/10 min) is important in Procedure B. The reproducibility of
scribe mark on the piston must be at the reference start position Procedure B is better if these parameters are strictly adhered to.
(top of the guide ring or barrel) at 7.0 6 0.5 min, as stated in A calibrated distance verification device will be required to
10.8 and 11.9. Starting each test at a different position can give maintain the proper piston travel.
variable results.
X2.2.16 Calculation Factors—When trouble shooting, al-
X2.2.8 Sample Mass—Small variations in sample mass can ways check the calculations and the factors used.
cause significant variability in melt flow rates. Any balance
X2.2.17 Power (Electrical) Fluctuation—Constant power
used to weigh the sample should be calibrated and verified on
(voltage) is important to maintain the temperature desired.
a regular schedule.
Periodic changes in voltage will cause changes in the tempera-
X2.2.9 Moisture in Sample—Samples should be dried be- ture of the unit, creating test values that fluctuate because of
fore testing. Some materials may be affected more than others inconsistent sample temperatures. Though this is a rare
by moisture. However, the presence of moisture during the test, situation, this fluctuation has been found to cause erratic test
in general, will affect the melt flow rates of most materials. results.
14
D1238 − 20
X3. EXTRUSION PLASTOMETER TEMPERATURE CALIBRATION DEVICE
X3.1 The RTD shall be inserted into a bronze tip. Tip of the
RTD element shall touch the bronze tip. Minimum insertion
depth is 11.2 mm. Clearance between the RTD and the bronze
tip wall shall be minimized. (See Fig. X3.1.)

FIG. X3.1 Example of a Temperature Calibration Device
X4. SUGGESTED TEST CONDITIONS FOR SELECT MATERIALS
X4.1 Table X4.1 shows a list of common test conditions

used for determining the rate of extrusion for some thermo-
plastic materials.
15
D1238 − 20
TABLE X4.1 Suggested Test Conditions for Select Materials
Material Temperatures Weights
Acetals (copolymer and homopolymer) 190 1.05
190 2.16
Acrylics 230 1.2
230 3.8
Acrylonitrile-butadienestyrene 200 5.0
220 10
230 3.8
Acrylonitrile/butadiene/styrene/polycarbonate blends 230 3.8
250 1.2
265 3.8
265 5.0
Cellulose esters 190 0.325
190 2.16
190 21.6
210 2.16
Ethylenechlorotrifluoroethylene copolymer 271.5 2.16
271.5 5.0
Ethylene-tetrafluoroethylene copolymer 297 5.0
Polyamide 235 1.0
235 2.16
235 5.0
275 0.325
275 5.0

Perfluoro(ethylenepropylene) copolymer 372 2.16
Perfluoroalkoxyalkane 372 5.0
Polycaprolactone 80 2.16
125 2.16
Polychlorotrifluorethylene 265 12.5
Polyetheretherketone (PEEK) 400 2.16
Polyether sulfone (PESU) 360 10
380 2.16
Polyethylene 125 0.325
125 2.16
190 0.325
190 2.16
190 5
190 10
190 21.6
250 1.2
310 12.5
Polycarbonate 300 1.2
Polymonochlorotrifluoroethylene 265 21.6
265 31.6
Polypropylene 230 2.16
Polyphenyl sulfone (PPSU) 365 5.0
380 2.16
Polystyrene 190 5.0
200 5.0
230 1.2
230 3.8
Polysulfone (PSU) 343 2.16
Polyethylene terephthalate (PET) 250 2.16
285 2.16
Poly(vinyl acetal) 150 21.6
Polyvinyl chloride (PVC), rigid compoundA 190 21.6
Poly(vinylidene fluoride) 230 5.0
230 21.6
Poly(phenylene sulfide) 315 5.0
Styrene acrylonitrile 220 10
230 3.8
230 10
Styrenic Thermoplastic Elastomer 190 2.16
200 5.0
Thermoplastic Elastomer-Ether-Ester 190 2.16
220 2.16
230 2.16
240 2.16
250 2.16
Thermoplastic elastomers (TEO) 230 2.16
Vinylidene fluoride copolymersB 120 5.0
120 21.6
230 2.16
230 5.0
A
Data has shown that greater repeatability and reproducibility when testing PVC can be obtained using Test Method D3364.
B
Tm = 100°C
16
D1238 − 20
REFERENCES
(1) “Polyethylene Insulation and Sheathing for Electrical Cables,” Gov- (4) Harban, A. A., and McClamery, R. M., “Limitations on Measuring
ernment Department Electrical Specification No. 27, Great Britain, Melt Flow Rates of Polyethylene and Ethylene Copolymers by
1950. Extrusion Plastometer ,” Materials Research and Standards, Vol 3,
(2) Tordella, J. P., and Jolly, R. E., “Melt Flow of Polyethylene,” Modern No. 11, 1963, p. 906.
Plastics, Vol 31 , No. 2, 1953, p. 146. (5) Rudin, A., and Schreiber, H. P., “Factors in Melt Indexing of
(3) Dexter, F. D., “Plasticity Grading of Fluorothenes,” Modern Plastics, Polyolefins,” SPE Journal, Vol 20, No. 6, 1964, p. 533.
Vol 30 , No. 8, 1953, p. 125.
SUMMARY OF CHANGES
Committee D20 has identified the location of selected changes to this standard since the last issue, D1238 - 13,
that may impact the use of this standard. (July 1, 2020)
(1) Editorial changes were made to comply with Practice (7) Revised 15.1.3.

D4968. (8) Revised 16.1.2.
(2) Revised 6.6.2. (9) Revised 16.1.3.
(3) Revised 6.7.2. (10) Added 16.1.4 (Tables 10 &11).
(4) Added 6.13. (11) Revised X2.1.1.1.
(5) Revised 8.1. (12) Revised X2.2.2.
(6) Revised 10.3.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of 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 five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make 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, PA 19428-2959,
United States. 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), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/
17

Astm D1238 20

Uploaded by

Copyright:

Available Formats

Astm D1238 20

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Astm D1238 20

Uploaded by

Copyright:

Available Formats

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

Standard Test Method for

1. Scope* E456 Terminology Relating to Quality and Statistics

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

*A Summary of Changes section appears at the end of this standard

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

FIG. 2 Details of Extrusion Plastometer

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

TABLE 4 Precision, Procedure A (Values in g/10 min)

TABLE 6 Precision, Procedure A (Values in g/10 min)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

TABLE 7 Precision, Procedure B (Values in g/10 min)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

TABLE 11 Precision, Procedure B (Values in g/10 min)

TABLE 13 Precision Statement for Procedure D: 5 kg

TABLE 14 Precision Statement for Procedure D: 10 kg

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

TABLE 15 Precision Statement for Procedure D: 21.6 kg

X1. EXTRUSION PLASTOMETER BORE ALIGNMENT

X2. TROUBLESHOOTING GUIDE

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

X3. EXTRUSION PLASTOMETER TEMPERATURE CALIBRATION DEVICE

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

X4. SUGGESTED TEST CONDITIONS FOR SELECT MATERIALS

X4.1 Table X4.1 shows a list of common test conditions

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

Untuk Balai Teknologi Polimer - BPPT (LP-106-IDN)

You might also like